Monografie.pdf

KP IX 1003Monographs, Part II 1004 Monographs, Part II KP VIII 1005 1) Crude drugs and Crude drug preparations Acanthopanax Root Bark Acanthopanacis Cortex Acanthopanax Root Bark is the bark of the root and stem of the Acanthopanax sessilifolium Seeman or other species of the same genus (Araliaceae). Description Acanthopanax Root Bark is usually the tubular or semi-tubular bark of the root and stem, 5 to 10 cm in length, 5 to 8 mm in diameter and 1 mm in thickness. Outer surface is yellowish brown to dark gray and flat. Thorns or their marks are on the surface of stem, sporadically. Inner surface of the bark is yellowish white. The texture is fibroid and difficult to be cut. Acanthopanax Root Bark has characteristic odor and slightly bitter taste. Purity (1) Xylem tissue and twigs⎯Not more than 2.0%. (2) Foreign matter⎯Acanthopanax Root Bark contains not more than 1.0% of the foreign matter other than xylem tissue and twigs. Extract Content than 8.0%. Water-soluble extract⎯Not less Acid-insoluble Ash Not more than 1.0%. Achyranthes Root Achyranthis Radix Achyranthes Root is the root of Achyranthes japonica Nakai or Achyranthes bidentata Blume (Amaranthaceae). Description (1) Achyranthes japonica—Achyranthes Root from Achyranthes japonica is a cylindrical main root with numerous lateral roots, 5 cm to 20 cm in length, 3 mm to 5 mm in diameter, with short remains of rhizome at the top. External surface is grayish yellow to pale yellow. Achyranthes Root is hard and brittle and the fractured surface is horn-like, yellowish white to yellowish brown. Achyranthes Root has slightly characteristic odor, slightly sweet taste and viscosity. (2) Achyranthes bidentata—Achyranthes Root from Achyranthes bidentata is a main root or a main root with some lateral roots, with or without short remains of rhizome at the top. Main root is cylindrical and sometimes somewhat tortuous, 15 cm to 90 cm in length and 3 mm to 7 mm in diameter. External surface is grayish yellow to yellow-brown, with numerous longitudinal wrinkles, with scattering scars of lateral roots and with longitudinal lenticel-like protrusion. Achyranthes Root is hard and brittle, or flexible when wet. Fractured surface is flat, grayish white to pale brown on the circumference and with yellowish white horn-like, oily xylem in the center. Under a microscope, a transverse section reveals a rather distinct cambium separating the cortex from the xylem. Small protoxylem is located at the center of the xylem and surrounded by numerous vascular bundles arranged on several concentric circles. Sporadically, abnormal vascular bundles are found. Parenchyma cells contain fine crystals of calcium oxalate. Starch grains are not observed. Achyranthes Root is odorless, sweet and mucilaginous. Identification (1) Weigh 0.5 g of pulverized Achyranthes Root, add 10 mL of water and shake vigorously: a lasting fine foam is produced. (2) Weigh 2 g of pulverized Achyranthes Root, add 10 mL of methanol, sonicate for 1 hour, filter and use the filtrate as the test solution. Seperately, weigh 1 mg of 20-Hydroxyecdison RS, dissolve in 1 mL of methanol and use this solution as the standard solution. Perform the test with the test solution and the standard solution as directed under the Thin-layer Chromatography. Spot 5 μL each of the test solution and the standard solution on a plate of silica gel with a fluorescent indicator for thin-layer chromatography. Develop the plate with a mixture of cholroform, methanol and water (8 : 2 : 0.5) to a distance of about 10 cm and air-dry the plate. Examine under ultraviolet light (main wavelength: 254 nm) or spray evenly sulfuric acid TS for spray, and heat at 105 o C for 10 minutes: the spot from the test solution and the spot from the standard solution show the same color and the same Rf value. Purity (1) Stem⎯Not more than 5.0%. (2) Foreign matter⎯The amount of foreign matter other than stems is not more than 1.0%. Loss on Drying Not more than 17.0% (6 hours). Ash Not more than 10.0%. Acid-insoluble Ash Not more than 1.5%. Akebia Stem Akebiae Caulis Akebia Stem is the stem of Akebia quinata Decaisne 1006 Monographs, Part II (Lardizabalaceae), from which the periderm has been removed. Alpina Katsumadai Seed Description Akebia Stem is the stem without the periderm and cut pieces in circular or ellipsoidal shape, 2 mm to 3 mm in thickness and 1 cm to 3 cm in diameter. Outer cork layer is grayish brown and with circular or transversely elongated elliptical lenticels. Cortex is dark grayish brown. Xylem reveals pale brown vessels and grayish white medullary rays lined alternately and radially. Pith is pale grayish yellow and distinct. Under a microscope, a transverse section reveals ring layers mainly consisting of fiber bundles with crystal cells and stone cell groups and surrounding the outside of the phloem in arc shape. Medullary rays of the phloems are consisted of sclerenchymatous cells containing solitary crystals. Cambium is distinct. Cells around the pith are remarkably thick-walled. Medullary rays of xylem and parenchymatous cells around the pith contain solitary crystals of calcium oxalate and starch grains less than 8 μm in diameter. Akebia Stem is nearly odorless and has slight acrid taste. Alpiniae Katsumadaii Semen Identification Weigh 0.5 g of pulverized Akebia Stem, add 10 mL of water, boil, allow to cool and shake vigorously: a lasting fine foam is produced. Loss on Drying Not more than 12.0% Ash Not more than 7.0%. Alpina Katsumadai Seed is the seed of Alpinia katsumadai Hayata, removed from pericarp. Description Alpina Katsumadai Seed is the mass of seeds, subspheroidal, 15 mm to 27 mm in diameter. External surface is grayish brown, with yellowish white septa in central part dividing the masses into three groups, each having numerous sticky seeds, agglutinated closely. Seed is ovoid-polyhedral, 3 mm to 5 mm in length, about 3 mm in diameter, covered with pale brown membranous aril, with raphe occurring as a longitudinal furrow and with hilum present at one end. Texture is hard. On cutting in half longitudinallay along the raphe, the seed shows oblique-cordate in shape. Testa extending inward along the raphe occupies about 1/2 of the surface area. Endosperm is grayish white. Alpina Katsumadai Seed has characteristic odor and pungent, slightly bitter tastes. Alpinia Rhizome Alpiniae Officinari Rhizoma Alisma Rhizome Alpinia Rhizome is the rhizome of Alpinia officinarum Hance (Zingiberaceae). Alismatis Rhizoma Alisma Rhizome is the tuber of Alisma orientale Juzepzuk (Alismataceae), from which periderm has been usually removed. Description Alisma Rhizome is a spherical or conical tuber, 3 cm to 8 cm in length, 3 cm to 5 cm in diameter, and is sometimes a 2- to 4-branched irregular tuber. External surface is pale yellowish brown to pale grayish brown, and slightly annulated with rarely remains of root in upper part and scars of rootlets in lower part. Under a microscope, a transverse section is nearly dense, the outer part is grayish brown, and the inner part is white to pale yellowish brown. Texture is rather light and difficult to break. Alisma Rhizome has slight odor and taste. Ash Not more than 5.0%. Acid-insoluble Ash Not more than 0.5%. Description Alpinia Rhizome is the rhizome, which is cylindrical, usually curved, and branched, 5 cm to 9 cm in length and 10 mm to 15 mm in diameter. External surface is reddish brown to dark brown with fine striped lines, grayish white nodes with 2 mm to 10 mm in length, and several scars of rootlet in one side. The texture is hard, tough and difficult to break. The fracture surface is grayish brown to reddish brown and fibrous, in which the stele occupies one third. Alpinia Rhizome has characteristic order and extremely pungent taste. Identification Weigh 1 g of pulverized Alpinia Rhizome, add 10 mL of ether, shake for 10 minites, and filter. To the residue obtained from evaporation of the filtrate, add 2 mL of phosphate TS, heat and dissolve: yellow color develops. Add 2 mL of water, shake and keep; the solution become cloudy. Loss on Drying Not more than 12.0% (6 hours). Ash Not more than 6.0%. Acid-insoluble Ash Not more than 1.5% indistinctly 3-ridged. filter and to the filtrate. Anemarrhena Rhizome has slightly characteristic odor and slightly sweet and mucous taste. Under a magnifying glass.5 g of pulverized Anemarrhena Rhizome with 2 mL of acetic anhydride on a water-bath for 2 minutes while shaking. Ash Not more than 9.Wu et Senjen and Amomum villosum Lourerio (Zingiberaceae). heat on a water bath for 1 hour under a reflux condenser and filter again. scars of root appear as numerous round spot-like hollow. Seeds are conical polyhedral. Identification 1) Weigh 0.0% Amomum Fruit Essential Oil Content Not less than 0. and base often bearing a fruit stalk. Description Ammomum Fruit is the fruit. Dissolve the residue to 2 mL of toluene and use the solutions as the test solution and the . add 1 drop of ferric chloride TS: a dark green precipitate is produced. and with grayish white membranous aril.6 mL (30. 15 mm to 20 mm in length and 10 mm to 15 mm in diameter. add 20 mL of ethanol. 10 mm to 25 mm in diameter.5 g of pulverized Anemarrhena Rhizome. Pericarp is thin and soft. with three prominent. apix with remains of perianth. transverse section reveals a few of lateral vascular bundles in cortex. slightly bitter tastes. Pericarp is hard. and fatty oil droplets and mucilage cells containing fine needles of calcium oxalate in parenchyma.0% Extract Content Dilute ethanol-soluble extract— Not less than 15. The seed mass is divided into 3 loculi by white septa and each loculus contains 5 to 26 seeds.KP VIII 1007 Essential Oil Content Not less than 0. Anemarrhena Rhizome Anemarrhenae Rhizoma Anemarrhena Rhizome is the rhizome of Anemarrhena asphodeloides Bunge (Liliaceae). Fractured surface is pale yellowish brown. heat on a water bath for 40 minutes under a reflux condenser and filter. about 5 mm in diameter. Description Anemarrhena Rhizome is rather flat and cord-like rhizome.0%.0% Acid-insoluble Ash Not more than 2. about 3 mm in diameter. 3 cm to 15 cm in length. add carefully 1 mL of sulfuric acid to make two layer: a red-brown color develops at the zone of contact. External surface is yellowish brown to brown. There are loculi divided into three groups by yellowish brown septa. seed). densely covered with spiny protrudings. On the lower surface. Anemarrhena Rhizome is light and easily broken. cool and slight bitter. dull ridges. xanthioides T. External surface is reddish brown. followed by bitterness.3 mL (100 g) Amomi Fructus Amomum Fruit is the ripe fruit of Amomum villosum Lourerio var. 5 mm to 15 mm in diameter. add 10 mL of water and 20 mL of toluene to the concentrated solution. ellipsoidal or ovoid. Texture is hard and endosperm is grayish white. Add 1 mL of hydrochoric acid to 10 mL of the filtrate. a longitudinal furrow and hair-like remains or scars of leaf sheath forming fine ring-nodes are present. The texture is hard and endosperms are grayish white. with round remains of stigma in apex and with a fruit stalk and its remains in base. Under a microscope.0% (seed).L. add 10 mL of water: a lasting fine foam is produced.0% (seed). Acid-insoluble Ash Not more than 3. Identification Amomum Tsao-ko Fruit is the long ellipsoidal fruit. transverse section reveals an extremely narrow cortex and stele porous. Amomum Tsao-ko Fruit Amomi Tsao-ko Fructus Amomum Tsao-ko Fruit is the well ripe fruit of Amomum tsao-ko Crevost et Lemaire (Zingiberaceae). 3) Weigh 2 g each of pulverized Anemarrhena Rhizome and Anemarrhena Rhizome RMPM. extract and evaporate the toluene layer to dryness. slightly bent and sometimes branched. Essential Oil Content Not less than 0. with a long longitudinal furrow in lateral side and concaved hilum in apex. On the upper surface. Concentrate to about 5 mL of the filtrate in vaccum. respectively. and external surface is reddish brown or dark brown. lasting and easily split longitudinally.2 mL (50 g). External surface is grayish brown to reddish brown with longitudinal furrow and ridge. 2 cm to 4 cm in length. Loss on Drying Not more than 12. Amomum Tsao-ko Fruit has characteristic odor and pungent. Filter the mixture and to 2 mL of the filtrate. Seed is irregularly polyhedral. Amomum Fruit has characteristic odor and taste is pungent. each containing 8 to 11 seeds agglutinated into a mass. 2) Weigh 0. External surface is pale brown.0 g. Ash Not more than 4. with many irregularly scattered vascular bundles. Main root is about 3 cm to 7 cm in length and 2 cm to 5 cm in diameter.5%. heat the plate at 105 o C for 10 minutes. much starch grains. Branched root is 15 cm to 20 cm in length. External surface is grayish brown to dark brown. add 10 mL of ethanol. the outer region is grayish white and the central region is sometimes dark brown. the standard solution of Anemarrhena Rhizome RMPM and the standard solution on a plate of silica gel for thin-layer chromatography. formosana Shan et Yuan (Umbelliferae).0%. Description Angelica Dahurica Root is a main root from which many long roots are branched out and nearly fusiform.36)]. dissolve with 1 mL each of ethanol and use these solution as the standard solution (1) and (2). Perform the test with the test solution and the standard solutions as directed under the Thin-layer Chromatography. Spot 5 μL each of the test solution and the standard solutions on a plate of silica gel with fluorescent indicator for thin-layer chromatography. Angelica Dahurica Root Angelicae Dahuricae Radix Angelica Dahurica Root is the root of Angelica dahurica Bentham et Hooker f. Ash Not more than 7. Separately.0%.0% of the sum of nodakenin (C20H24O9: 408.0%. dissolve 1 mg each of Decursin RS and Decursinol RS.0%. One spots among those spots from the test solution and a reddish purple spot from the standard solution show the same color and the same Rf value. Spray the vanillin sulfuric acid TS to the plate. Under a microscope. with dark yellow color around the cambium. Xylem and cortex are distinguished clearly by cambium ring. add 5 mL of ethanol. Ash Not more than 7. Under a microscope. weigh 5 mg of Sarsasapogenin RS. Spot 10 μL each of the test solution. the transverse section reveals cork consisting of 5 to 6 layers of cells.1008 Monographs. Acid-insoluble Ash Not more than 2. Purity Foreign matter—The amount of fiber. The spots from the test solution and the spots from the standard solution of Anemarrhena Rhizome RMPM show the same color and the same Rf value.0%. filter and use the fitrate as the test solution. Part II standard solution of Anemarrhena Rhizome RMPM. Acid-insoluble Ash Not more than 2. var. parenchymas from primary cortex to xylem aligned systematically in rectangular shape. Identification Weigh 1 g of pulverized Angelica Gigas Root. Deve1op the plate with a mixture of toluene and acetone (9 : 1) to a distance of about 10 cm and air-dry the plate. In a transverse section. and white in the remaining part. Identification Weigh 0.40) and total decursin [decursin (C19H20O5: 328. and bitter and sweet taste. secretary canal with yellowish brown ingredient and substitute fiber is sparsely scattered. allow to stand for 5 minutes with shaking and filter. External surface is pale yellowish brown to dark brown with longitudinal wrinkles. Extract Content Dilute ethanol-soluble extract— Not less than 25. and the clusters of calcium oxalate in parenchyma cells. boil in the water bath for 10 minutes. Numerous starch grains are observed in parenchyma cells. Scalariform or spiral vessel is observed. Angelica Gigas Root is the root of Angelica gigas Nakai (Umbelliferae). or Angelica dahurica Bentham et Hooker f. the standard solution of Anemarrhena Rhizome RMPM and the standard solution as directed under the Thinlayer Chromatography. Angelica Gigas Root contains not less than 6. dissolve in 1 mL of toluene and use this solution as the standard solution. with longitudinal wrinkles and with numerous scars of rootlets laterally elongated and protruded. cool.0%.0%. Develop the plate with a mixture of hexane and ethyl . The cortex has schizogenous intercellular space. Separately.2 g of pulverized Angelica Dahurica Root. Examine the filtrate Purity (1) Leaf sheath—Not more than 3. Angelica Dahurica Root has characteristic odor and slightly bitter taste. Perform the test with the test solution. 10 cm to 25 cm in length and 15 mm to 25 mm in diameter. under ultraviolet light (main wavelength: 365 nm): a blue to bluish purple fluorescence develops. A few remains of leaf sheath at the crown and ring-nodes closely protruded near the crown. transverse section reveal vessels and medullary rays developed radially from the center. Fractured surface is flat. cells aligned transversely. Angelica Gigas Root Angelicae Gigantis Radix Description Angelica Gigas Root is thick and short root with the remains of stems and leaf sheaths. main root sometimes has transverse wrinkles. (2) Foreign matter—The amount of foreign matter other than leaf sheath contained in Angelica Dahurica Root dose not exceed than 1.36) and decursenol angelate (C19H20O5: 328. Angelica Gigas Root has characteristic odor. originating from the dead leaves and other foreign matter is not more than 3. 8 mm to 13 mm in width and 4 mm to 7 mm in thickness. Apricot Kernel Armeniacae Semen Apricot Kernel is the well ripe seed of Prunus armeniaca Linné var. contains not less than 3. decursin and decursinol angelate are eluted in this order. and perform the test as directed under the Liquid Chromatography according to the following operating conditions. extract under a reflux condensor for 1 hours. Column temperature: An ordinary temperature. Cotyledons are two. forming angular circle to ellipse and approximately uniform in shape. 10 mm to 18 mm in length. the standard solution. and filter. weigh accurately about 10 mg of Nodakenin RS.5 g of pulverized Angelica Gigas Root. Assay Weigh accurately about 0. Under a microscope. the test solution and ASN and ASD. Numerous vascular bundles run from chalaza throughout the seed coat.0%.0 g). Seed coat and thin semi-transparent white albumen easily separate from cotyledon when soaked in boiling water. brown and its surface is powdery with rubbing easily detachable stone cells of epidermis. somewhat asymmetric ovoid seed.02). with uniformly thickened walls and 60 μm to 90 μm in diameter. Apricot Kernel. decursin and decursinol angelate (the relative retention time to decursin is about 1. ATN. when dried. milky white and oily. To the residue. surface of epidermis reveals stone cells on veins protruded by vascular bundles. Determine the peak areas. ansu Maximowicz. dissolve acucurately about 10 mg of Decursin RS. 4. Seed coat is thin.0 mL/min System suitability System performance: When the procedure is run with 10 μL of this solution under the above operating conditions. add 20 mL of methanol. respectively. Mobile phase A – acetonitrile Mobile phase B – water 50 90 10 Flow rate: 1. packed with octadecylsilyl silica gel for liquid chromatography (5 μm in particle diameter).KP VIII 1009 acetate (2 : 1) to a distance of about 10 cm and air-dry the plate.5%.0% of amygdalin (C20H27NO11: 457. stone cell appears obtusely triangular and its wall is extremely thickened at the apex. clearly dividing each peak. dissolve in methanol to make 20 mL. Apricot Kernel is sharp at one end and rounded at the other end where chalaza situated.0% of foreign matter other than stems and woody root. Time (min) Mobile phase A Mobile phase B (%) (%) 0 20 80 3 20 80 Purity (1) Stem and woody root—Angelica Gigas Root contains less than 5. Separately. and use this solution as the standard solutions. Mobile phase: Control gradually or concentrationgradiently with mobile phase A and B as follows. decursin and decursinol angelate is not more than 1.6 mm in inside diameter and 25 cm in length. nodakenin. add methanol to make exactly 50 mL. take exactly 5 mL of this solution. Pipet 10 μL each of the test solution and the standard solutions. Amount (mg) of nodakenin (C 20 H 24 O 9 ) = amount (mg) of Nodakenin RS × A TN 1 × A SN 4 Amount (mg) of total decursin [decursin (C 19 H 20 O 5 ) and decursinol angelate (C 19 H 20 O 5 )] = amount (mg) of Decursin RS × A TD + A TDA A SD Operating conditions Detector: An ultraviolet absorption photometer (wavelength: 330 nm).1 mL (50. Combine all the filtrates. glabra Nakai. 41 90 10 Essential Oil Content Not less than 0. Description Apricot Kernel is flattened. of nodakenin and decursin. add methanol to make exactly 50 mL and use this solution as the test solution. respectively. add 20 mL of methanol . System repeatability: When the test is repeated 6 times with 10 μL of the standard solution under the above operating conditions. and proceed in the same manner. Prunus mandshurica Koehne var. Apricot Kernel is almost odorless and has bitter and . appearing as thin vertical furrows. ATD and ATDA. of nodakenin. Prunus sibirica Linné or Prunus armeniaca Linné (Rosaceae).43). 8 30 70 18 30 70 19 50 50 40 50 50 Ash Not more than 6. Examine under ultraviolet light (main wavelength: 365 nm: two spots among the spots from the test solution and spots from the standard solution (1) and (2) show the same color and the same Rf value. (2) Foreign matter—Angelica Gigas Root contains less than 1. In lateral view.0 % of stem and woody root. the relative standard deviation of each peak area of nodakenin. Column: A stainless steel column. with longitudinal wrinkles and sparse rootlet scars.8 to 1. Arctium Fruit is hollow about 1 mm in diameter at one broad end. Acid-insoluble Ash Not more than 2. Assay Weigh accurately about 0. Part II oily taste.0 to 1. medullary rays consisting of 3 to 5 rows. long cylindrical to rod shaped. add 10 mL of methanol. heat for 10 minutes on a water bath with a reflux condenser. Amount (mg) of amygdalin (C20H27NO11) A = amount (mg) of Amygdalin RS × T AS Operating conditions Detector: An ultraviolet absorption photometer (wavelength: 214 nm). vortex and add carefully 0.2 mm in width. 0. Fractured surface is fibrous with pale yellow pith and texture is light and loose. dissolve 2 mg of Amygdalin RS in 1 mL of methanol and use this solution as the standard solution. Arctium Fruit Arctium Fructus Arctium Fruit is the fruit of Arctium lappa Linné (Compositae). transverse section reveals small resin canal with secretary cells in collenchyma. Add 70 mL of water and 70 mL of hexane to the residue. Flow rate: 1.1010 Monographs. Separately. long obovate achene. is clearly. 10 cm to 30 cm in length and 5 mm to 20 mm in diameter. Mobile phase: A mixture of methanol and water (20 : 80). Description Arctium Fruit is slightly curved. About 100 fruits of Arctium Fruit weigh 1.5 mL of anhydrous acetic anhydride. Spot 10 μL each of the test solution and the standard solution on a plate of silica gel for thin-layer chromatography. Combine the whole filtrates and evaporate to dryness under reduced pressure. The clear cambium consists of 3 to 5 rows.5 mm in thickness. Take 1. Column temperature: A room temperature. Filter after cooling and use this as the test solution. extract for 1 hr with agitating.0%. External surface is grayish-white to grayish-brown. longitudinal ridge at the other narrow end. methanol and water (7 : 3 : l) to a distance of about 10 cm and air-dry the plate. shake and discard the ether layer. (2) Foreign matter—Apricot Kernel does not contain fragments of endocarp and other foreign matter. Description Aralia Continentalis Root is the root.0 mL/minute. extract with a reflux condenser for 2 hours and filter. The remaining water layer is filtered. add 0. Perform the test with the test solution and the standard solution as directed under the Thin-layer Chromatography.0%. add 10 mL of chloroform. adjust the total volume to make exactly 100 mL and use this solution as the test solution. dissolve in 100 mL of water and use this solution as the standard solution. Under a microscope.5 g of pulverized Aralia Continentalis Root. a transverse section reveals an ex- .5 g. dry the Amygdalin RS for 24 hours in the desiccator (silica gel) and weigh accurately about 10 mg. Identification Weigh 1 g of pulverized Apricot Kernel. AT and AS. are connected from the pith to the phloem. Add 70 mL of ether to the water layer. Column: A stainless steel column. Ash Not more than 9. xylem fibers is developed around vessles in xylem. Develop the plate with a mixture of ethyl acetate. Purity (1) Rancidity—Grind Apricot Kernel with hot water: no unpleasant odor of rancid oil is perceptible. of amygdalin for the test solution and the standard solution. packed with octadecylsilyl silica gel (5 μm to 10 μm in particle diameter). 5 to 7 mm in length. 2.0 to 3.5 g of pulverized Apricot Kernel. Aralia Continentalis Root Araliae Continentalis Radix Aralia Continentalis Root is the root of Aralia continentalis Kitakawa (Araliaceae). Repeat the above procedure with the residue using 50 mL of methanol. add 50 mL of methanol. with black spots. Perform the test with l0 μL each of the test solution and the standard solution as directed under the Liquid Chromatography according to the following operating conditions and determine the peak areas.0%. Spray evenly sulfuric acid TS for spray and heat for 10 minutes at 105 o C : one spot among the spots from the test solution and a brown to dark brown spot from the standard solution show the same color and the same Rf value.0 mL of the filtrate. (6 hours). Aralia Continentalis Root has characteristic odor and tastes unpleasant and slightly bitter. stand for 15 minutes and filter. respectively. 4 mm to 6 mm in inside diameter and 15 cm to 25 cm in length. and is flat. Identification Weigh 0. shake well and discard the hexane layer. Separately. indistinct.5 mL of sulfuric acid to make two layers: a red to dark red color develops at the zone of contact and the upper layer produces yellowish-red to dark yellowish red. Loss on Drying Not more than 12. Under a microscope. External surface is grayish brown to brown. stalk scars at apex. Areca Peel has slight characteristic odor and slightly astringent taste. weigh 5 mg of Arecoline Bromide RS. Endocarp is dented.0% of foreign matter other than the pericarp.0 % Areca Arecae Semen Areca is the ripe seed of Areca catechu Linné (Palmae). rounded-conical or flattened nearly spherica1. Purity Foreign matter—Areca Peel contains less . Endocarp is hard shell-shaped. dissolve it in 1 mL of methanol and use this as the standard solution.0% of pericarp. dissolve the residue in 1. Cross section is dense in texture. filter. Perform the test with the test solution and the standard solution as directed under the Thin-layer Chromatography. Purity (1) Pericarp—Areca contains less than 2. and use filtrate as the sample solution. 4 cm to 7 cm in length. l5 mm to 35 mm in height and 15 mm to 30 mm in diameter. Spot 5 μL of the sample solution on a plate of silica gel for thin-layer chromatography. Identification Weigh 3 g of pulverized Areca in stoppered centrifuge tube. Ash Not more than 2. Epicarp is deep brown to black.5 g of pulverized Areca Peel. Spray evenly iodine TS on the plate: one spot among the spots from the test solution and a reddish brown spot from the standard solution show the same color and the same Rf value. External surface is grayish reddish brown to grayish yellowish brown. boiled in water and removed from pericarp. remains of fruit stalk and calyx at the base. yellowish white or pale brown. water and acetic anhydride (10 : 6 : l) to a distance of about 10 cm and air-dry the plate. and airdry the plate. and sometimes broken in longitudinal.KP VIII 1011 ocarp of single-layered epidermal tissue. methanol and use this solution as the test solution. and minute crystals of calcium oxalate. Identification Weigh 0. smooth and hard shell-shaped. Extract Content Dilute ethanol-soluble extract— not less than 15.4. usually elliptical or long ovoid gourd-shaped. (2) Daebokmo – Areca Peel is the pericarp. yellowish brown to deep brown. ethyl acetate and water (15:10:1) to a distance of about 10 cm. Mesocarp is fibrous. Spray evenly diluted sulfuric acid TS on the plate.0% (6 hours). and seed coat composed of parenchyma several cells thick. shake for 2 minutes to 3 minutes and filter. smooth. endocarp of a single layer of stone cells containing solitary. and the one from the ripe fruit is known as Daebokmo.5 mL of Description (1) Daebokpi – Areca Peel is the pericarp. and cotyledons with starch grains. add 5 mL of water. exhibiting a marble appearance of grayish brown seed coat alternating with white albumen. raised transverse lines on the surfaces. Spot 5 μL each of the test solution and the standard solution on a plate of silica gel for thin-layer chromatography. Hilum is present at the center of its base and usually forms a dent. brown to deep brown.5 g of pulverized Arctium Fruit. Inner surface is lustrous. mesocarp of slightly sclerified parenchyma containing parenchymatous cells with a brown substance. (2) Foreign matter—Areca contains less than 1. discrete crystals of calcium oxalate. Separately. Arctium Fruit has odorless. shake for 5 minutes. oil drops.0%. add 1 mL of lead subacetate TS: the filtrate turns pale yellow with turbidity and yellow precipitation are slowly occurred. and heat at 105 o C for 10 minutes: a red purple spot appears at around Rf value 0. Loss on Drying Not more than 12. from which the fruit is unripe after boiled. Areca has slightly characteristic odor and astringent and slightly bitter taste. Identification Weigh 0. develop the plate with a mixture of acetone. lustrous. Texture is light and hard and mesocarp fibers visible torn longitudinally. Develop the plate with a mixture of acetone. stoppered. with irregular longitudinal wrinkles. The pericarp from unripe fruit is known as Daebokpi. with a network of pale lines and texture is hard. bitter taste and oily. add 20 mL of methanol. Areca Peel Ash Not more than 7.0%. Areca Peel has slight characteristic odor and weak taste. Epicarp is mostly lost or remained. Evaporate ether in water-bath. Arecae Pericarpium Acid-insoluble Ash Not more than 1. which is collected. The interior of the seed is often hollow. aleurone grains. Acera Peel is the pericarp of Areca catechu Linné (Palmae). shake for 10 minutes. Perform the test with the sample solution as directed under thin-layer chromatography.5%. To 2 mL of the filtrate. Description Areca is the seed. 20 cm to 35 cm in width and 2 mm to 5 mm in thickness. sparce and soft. centrifuge and pipet the supernatant. usually elliptical or gourd-shaped. add 30 mL of ether and 5 ml of sodium hydroxide TS. 0%.1012 Monographs. Purity (1) Terrestrial part—Asiasarum Root and Rhizome contains less than 10. Arisaema erubescens Schott or Arisaema heterophyllum Blume (Araceae).0% of its terrestrial part such as leaves and petioles. The texture is mostly soft or hard.0% (6 hours). peduncles or buds.0% of foreign matter other than terrestrial part. add 10 mL of water. ricum F. (3) On a section of Arisaema Rhizome. Description Asiasarum Root and Rhizome is the root and rhizome. A fractured surface is milky white and starchy. add dilute iodine TS drop-wise: a dark bluish purple color is produced on the surface. Asparagi Tuber Asparagus Tuber is the tuber of Asparagus cochinchinensis Merill (Liliaceae).0%. Asiasari Radix et Rhizoma Description Asparagus Tuber is a fusiform to globular tuber. Asparagus Tuber Ash Not more than 10.5 mL of sulfuric acid to the filtrate: a pale brown color develops at the zone of contact.5 g of pulverized Arisaema Rhizome. like irregularly curved string in shape. from which the cork layer has been removed. filter and add carefully 0.2 g of pulverized Arisaema Rhizome. warm for 2 to 3 minutes Loss on Drying Not more than 15. External surface is pale yellowish brown to pale brown and slightly smooth. add 10 mL of water. Acid-insoluble Ash Not more than 1. Under a microscope. Some tubers are surrounded by small oblate lateral buds. encircled with numerous pitted fibrous root scars. sleek and horny. Arisaema Rhizome Arisaematis Rhizoma Arisaema Rhizome is the tuber of Arisaema amurense Maximowicz. easy to be fractured. 5 cm to 15 cm in length and 5 mm to 20 mm in diameter. the transverse section shows parenchymatous cells filled with starch grains and mucilage cells filled with mucilage duct and fine needles of calcium oxalate. Essential Oil Content Not less than 0. (2) Foreign matter— Asiasarum Root and Rhizome contains less than 1. The upper end of rhizome is sometimes with petioles.5 g of pulverized Asparagus Tuber. and internode has several thin and long roots. (2) Weigh 0.The texture is easy to be broken and the fractured surface is yellowish white and not flat. External surface is pale yellowish white to pale brown. Asiasarum Root and Rhizome is the root and rhizome of Asiasarum heteropoides F. sometimes with longitudinal wrinkles.0%. Asiasarum Root and Rhizome has characteristic odor and pungent taste with a slight numbness on the tongue. macerate and shake vigorously: a lasting fine foam is produced. warm for 2 minutes on a water-bath. Arisaema Rhizome has slight pungent odor and taste. External surface is pale brown to dark brown with extremely thin longitudinal wrinkles on the surface.0% (6 hours). transverse section reveals parenchyma cells and oil drops in endoderm. Identification (1) Weigh 0.0%. mandshu- Identification 1) Weigh 0. Description Arisaema Rhizome is irregular oblate rhizome. Mucilage cells filled with fine needles of calcium oxalate are observed in the parenchymatous cells of cortex and the central cylinder. Loss on Drying Not more than 12. Starch grains don’t exist.6 mL (30.0% of Areca and foreign matters. Asiasarum Root and Rhizome . Maekawa or Asiasarum sieboldi Miquel var. add 2 mL of acetic anhydride. The cork layer has been removed and dried after boiling or steaming by hot water. semi-translucent. The top is with dented stem scars and the bottom is crumpled. Asparagus Tuber has a slight characteristic odor and tastes sweet followed by bitter taste. Acid-insoluble Ash Not more than 3. Under a microscope. seoulense Nakai (Aristolochiaceae). The rhizome is 2 cm to 4 cm in length and 2 mm to 3 mm in diameter with yellowish brown nodes and numerous root about 15 cm in length and about 1 mm in diameter. Under a microscope. Extract Content Dilute ethanol-soluble extract— Not less than 5. somewhat curved. Ash Not more than 7. 15 mm to 65 mm in diameter and 1 cm to 2 cm in height.0%. Texture is hard and uneasily broken. Each node has several scars of petiole and peduncle.0 g). Ash Not more than 5.0%. the transverse section shows stone cells or clusters of stone cells are scattered outside of cortex. Maekawa var. Part II than 10. the fractured surface is grayish yellow. 0% of stem and other foreign material. Aster Root has characteristic odor. water and acetic anhydride (10 : 6 : 3) to a distance of about 10 cm and air-dry the plate.0% (6 hours). Loss on Drying Not more than 13. Ash Not more than 15. External surface is dark grayish-brown to dark yellow-brown. Add 1 to 2 drops of ferric chloride TS to 2 mL of the filtrate. External surface is pale brown to reddish brown. heat the plate at 105 o C for 2 minutes. Extract Content Dilute ethanol-soluble extract⎯ Not less than 25.5 mL of sulfuric acid to make two layers: a reddish brown color develops at the zone of contact Purity Foreign matter—Less than 5. mongholicus Hsiao (Leguminosae) Description Astragalus Root is nearly cylindrical root. The fractured surface is fibrous. Usually pith is unobservable. Description Atractylodes Rhizome is irregularly curved. with longitudinal wrinkles. External surface is pale grayish yellow to pale yellow-brown and covered with irregular. Often white cottonlike crystals are produced on its surface if Atractylodes . 2) Add 10 mL of water to 0. a lasting fine foam is produced. Texture is dense and difficult to break and fractured surface is fibrous. Spot 10 μL the test solution on a plate of silica gel for thin-layer chromatography. 2) Weigh 1 g of pulverized Asparagus Tuber. filter.0%. Identification 1) Weigh 0.5 g of pulverized Aster Root. a purple color develops. Atractylodes Rhizome Atractylodis Rhizoma Atractylodes Rhizome is the rhizome of Atractylodes lancea De Candlle or of Atractylodes chinensis Koidzumi (Compositae). White medullary ray runs from xylem to cortex in thin root. and easily curved. and acrid taste.0%. and filter. Purity Root of Hedysarum species and others— Under a microscope. add 10 mL of water.0%.2 g of pulverized Aster Root. The spot develops at about 0. with pale brown to red-brown secretes as fine points.0% (6 hours). Thickness of the cortex is from about one-third to one-half of the diameter of xylem. Deve1op the plate with a mixture of butanol. A transverse section reveals nearly orbicular. but often appears as radiating cracks in thick root. Shake vigorously. Add slowly 0. 30 cm to 100 cm in length and 7 mm to 20 mm in diameter. twisted near the crown. Under a magnifying glass. Acid-insoluble Ash Not more than 1. a transverse section reveals an outer layer composed of periderm. Astragalus Root Astragali Radix Astragalus Root is the root or the root removed the periderm of Astragalus membranaceus Bunge or Astragalus membranaceus Bunge var. 1 mm to 2 mm in diameter.4 of Rf value. with small bases of lateral root dispersed on the surface. heat on a water bath and cool. Loss on Drying Not more than 15.KP VIII 1013 on a water-bath. shake vigorously to mix. xylem is pale yellow and zone near the cambium somewhat brown.0%. (Compositae) Description Aster Root is the root. Astragalus Root has slightly odor and sweet taste. 3 cm to 10 cm in length and 10 mm to 25 mm in diameter. a reddish brown color followed by a brown color Loss on Drying Not more than 18. cortex is pale yellowish white. 3) Weigh 0. Ash Not more than 3. Extract Content Dilute ethanol-soluble extract— Not less than 30. water (40 : 7).0%.0%. Ash Not more than 5. Perform the test with the test solution as directed under Thin-layer Chromatography. Aster Root Asteris Radix Aster Root is the root of Aster tataricus Linné fil.2 g of pulverized Aster Root.0% (6 hours). Heat for 2 minutes and filter.0% Acid-insoluble Ash Not more than 8. add 1 mL of Fehling solution TS to 3 mL of the filtrate and warm on a water-bath: reddish brown precipitate is produced. a vertical section of Astragalus Root reveals no crystal fiber containing solitary crystals of calcium oxalate outside the fiber bundle. dispersed longitudinal wrinkles and horizontal lenticel-like patterns. 5 cm to 15 cm in length. shake for 30 minutes and filter. Spray diluted sulfuric acid TS to the plate. add 2 mL of acetate anhydride. cylindrical rhizome. shake the solution on a water bath and mix. Use the filtrate as the test solution. soft. add 5 mL of a mixture of butanol. 0 g).5 mL of vanillin-hydrochloric acid TS and shake immediately: no red to red-purple color develops within l minute. Press the mixture. Spray evenly pdimethylaminobenzaldehyde TS for spraying on the plate and heat at 100 °C for 5 minutes: no green to grayish green spot appears between Rf 0. add 0. Belladonna Extract Belladonna Extract contains not less than 0. The pith and medullary rays contain oil sacs similar to those in cortex.6.85% and not more than 1. add 4 L of 35% Ethanol and digest for 3 days. Spot 10 μL of the test solution on a plate of silica gel for thin-layer chromatography. Description (1) Atractylodes japonica—Atractylodes Rhizome White from Atractylodes japonica is rhizome.5%. (2) Atractylodes macrocephala—Atractylodes Rhizome White from Atractylodes macrocephala is the rhizome. and scatterd with yellowish brown oil sacs. Method of preparation Weigh 1000 g of a coarse powder of Belladonna Root. sometimes in a protruding knot-shape. Ash Not more than 7. filter and use this filtrate as the test solution. having sporadic. Texture is hard and difficult to be broken. The fractured surface of dried materials by baking is hornlike shape. macerate with 5 mL of ethanol by warming on a water-bath for 2 minutes and filter. Xylem exhibits vessels surrounded by fiber bundles and arranged radially on the region adjoining the cambium. The parenchyma tissues contain small crystals of inulin and needle crystals of calcium oxalate. and viscosity on chewing. Under a microscope.0 mL of hexane. Texture is difficult to break and the fractured surface is fibrous. and distinct fiber bundle surrounding these vessels. often fiber bundles at the outside of the phloem in the parenchyma of the cortex. Identification Weigh 0. To 2 mL of the filtrate.0 g). Purity Atractylodes rhizome white—Weigh 0. and scars of fibrous rootlets. To 2 mL of the filtrate. 3 cm to 13 cm in length and 15 mm to 70 mm in diameter. add 0. Parenchyma cells contain spherocrystals of inulin and fine needles of calcium oxalate. with or without periderm. Purity Atractylodes lancea rhizome—Weigh 2 g of pulverized Atractylodes Rhizome White. Atractylodes Rhizome has characteristic odor and slightly bitter taste. Filter and prepare the viscous extract as directed . Combine all the extract and allow to stand for 2 days.1014 Monographs. Pith and medullary rays exhibit the same oil sacs as in the cortex. and the end region of medullary rays reveals oil sacs containing pale brown to yellow-brown substances. shake for 5 minutes. add 5. sweet taste. Acid-insoluble Ash Not more than 1. external surface is balckish brown. interrupted longitudinal wrinkles and grooves.3 and 0. External surface is grayish yellow or dark brown. The xylem reveals small and radially lined vessels surrounding pith. Essential Oil Content Not less than 0. Under a microscope. knob-like small protrusions. Atractylodes Rhizome White from Atractylodes macrocephala has characteristic odor. Perform the test with this solution as directed under the Thin-layer Chromatography. Under a microscope. Ash Not more than 7.5 g of pulverized Atractylodes Rhizome White.7 mL (50. Part II Rhizome is stored long time.0%. 3 cm to 8 cm in length and 2 cm to 3 cm in diameter. and oil sacs containing pale brown to brown substances at the end of medullary rays. The fractured surface is not flat and yellowish white to pale brown. add 5 mL of ethanol by warming on a water-bath for 2 minutes and filter.05% of total alkaloids [as hyoscyamine (C17H23NO3: 289. in a shape of irregularly enlarged mass. transverse section reveals interrupted band of needle crystals of calcium oxalate between cork cells and the cortex. Essential oil Not less than 0. When periderm is remained. Atractylodes Rhizome White from Atractylodes japonica has characteristic odor and somewhat bitter taste. Acid-insoluble Ash Not more than 1.0%. of Atractylodes japonica Koidzumi or Atractylodes macrocephala Koidzumi (Compositae). Atractylodes Rhizome White Atractylodis Rhizoma Alba Atractylodes Rhizome White is the rhizome.37)].0%. a transverse section usually reveals no fiber in parenchyma of cortex. a transverse section reveals periderm with stone cell layers.5 mL of vanillin-hydrochloric acid TS and shake immediately: a red to reddish purple color develops and persists. or from which the periderm has been removed. in a irregular mass or irregularly curved cylinder.5 g of pulverized Atractylodes Rhizome. Oil sacs containing brown substances are scattered in the cortex and medullary rays.7 mL (50. relatively deep colored or cracked. Develop the plate with a mixture of hexane and acetone (7 : 1) to a distance of about 10 cm and air-dry the plate. The parenchyma cells sometimes contain needle crystals of calcium oxalate and inulin. Remains of stems and bud scars are attached to the apex. from which periderm is removed. add 2000 mL of 35% Ethanol to the residue and digest again for 2 days. with coarse wrinkles. repeat this operation twice with 25 mL of ether. Develop the plate with a mixture of acetone.0%.0 mL of the standard stock solution. stopper. add mobile phase to make exactly 25 mL and use this solution as the standard solution. sonicate for 5 minutes and centrifuge. Evaporate ethyl acetate in vaccum. weigh 2 mg of Atropine Sulfate RS. add 40 mL of ethyl acetate. shake. . add 3 g of anhydrous sodium sulfate.0%. discard 2 mL of first filtrate and use the subsequent filtrate as the test solution. Belladonna Root Belladonnae Radix Belladonna Root is the root of Atropa belladonna Linné (Solanaceae). Dissolve the residue in 5 mL of the mobile phase.7 g of pulverized Belladonna Root. Perform the test with the test solution and the standard soltuion as directed under the Thin-layer Chromatography. Separately. Identification Weigh 2 g of pulverized Belladonna Root in a glass-stoppered centrifuge tube. add 30 mL of ammonia TS. dissolve the residue in 1 mL of ethanol and use this solution as the test solution. Dissolve the residue in 5 mL of mobile phase.8 　m in diameter). Assay Weigh accurately about 0. when dried. contains not less than 0. stopper tightly. Description Belladonna Root is the root. To the residue. add 15 mL of ammonia TS and shake. separate the ethyl acetate layer. Store in a cold place. centrifuge and separate the ether layer. weigh accurately about 0. Identification Mix 0. weigh accurately about 25 mg of Atropine Sulfate RS. Spray evenly Dragendorff’s TS for spraying: one spot among the spots from the test solution and a yellowish red spot from the standard solution show the same color and the same Rf value. Q 1 calculated on the dried basis × T × × 0. Perform the test with l0 μL each of the test solution and the standard solution as directed under the Liquid Chromatography according to the following operating conditions. dissolve the residue in 1 mL of ethanol and use this solution as the test solution.37)]. shake and filter after the solution is clear.4% of total alkaloids [as hyoscyamine (C17-H23NO3: 289. Purity (1) Stem and crown—Less than 10.0%.4 g of Belladonna Extract. External surface is grayish brown to grayish yellow-brown. respectively. shake for 15 minutes.0 mL of the internal standard solution and add the mobile phase to make exactly 25 mL. Belladonna Root is often cut crosswise or lengthwise. Description Belladonna Extract is a dark brown. transfer the mixture to a separatory funnel. Amount (mg) of hyoscyamine (C17 H 23 NO 3 ) Belladonna Root is almost odorless and has bitter taste. Repeat this procedure twice with the water layer. Periderm of Belladonna Root is often removed. = amount (mg) of Atropine Sulfate RS. Proceed as directed in the Identification under Belladonna Root. Fractured surface is pale yellow to pale yellow-brown and much powdery. water and ammonia water (90 : 7 : 3) to a distance of about 10 cm and dry the plate at 80 °C for 10 minutes. Pipet the supernatant in separatory funnel. Proceed as directed in the Assay under Belladonna Root. tight containers.KP VIII 1015 under Extract. Assay Dry the pulverized Belladonna Root at 60 °C for 8 hours.5 g of Belladonna Extract with 30 mL of ammonia TS in a flask. add 3 g of anhydrous sodium sulfate to the ethyl acetate. add 3. Belladonna Root. Filter this solution with filter paper (not more than 0. Combine all extracts and evaporate the ether layer on a water-bath. QT and QS. dissolve in mobile phase to make 25 mL and use this solution as the standard stock solution.0%. Ash Not more than 6. Add 25 mL of ether.8551 QS 5 Acid-insoluble Ash Not more than 4. with longitudinal wrinkles.0 mL of the internal standard solution and add mobile phase to make exactly 25 mL. Combine the extracts and evaporate the ether on a waterbath. Drain off the ethyl acetate layer. Determine the peak areas.0 mL of the internal standard solution. add 3. place in a sotppered centrifuge tube and moisten with 15 mL of ammonia TS. centrifuge and take the ether layer. cylindrical. (2) Foreign matter—The amount of foreign matter other than stems and crowns contained in Belladonna Root is not more than 2. of hyoscyamine (atropine) for the test solution and the standard solution. Internal standard solution—A solution of brucine dihyrate in the mobile phase (1 in 2500) Packaging and Storage Preserve in light-resistant. Add 25 mL of ether. previously determine loss on drying. add 3. place in a glass-stopperd centrifuge tube. 10 cm to 30 cm in length and 5 mm to 40 mm in diameter. using 25 mL each of ether. Evaporate the filtrate to dryness in vaccum. Separately. dissolve in 1 mL of ethanol and use this solution as the standard solution. has characteristic odor and bitter taste. Pipet 5. Spot 5 μL each of the test solution and the standard solution on a plate of silica gel for thin-layer chromatography. shake and filter after the ethyl acetate become clear. then add 40 mL of ethyl acetate and shake the mixture. shake for 15 minutes. A appropriate quantity of Ethanol and Purified Water may be used in place of 35% Ethanol. 0%. vessels are lined radially or step-wise and fiber groups are scattered. Bitter Cardamon has characteristic odor and slightly bitter taste.3 to 0. Part II Amount (mg) of hyoscyamine (C17 H 23 NO 3 ) = amount (mg) of Atropine Sulfate RS. add 10 mL of ether.8 g of potassium dihyrogenphosphate in 900 mL of water. and texture is hard. about 4 mm in inside diameter and about 15 cm in length.5 mm in diameter. Ash Not more than 10. Ash Not more than 2. Texture is easily broken and the fractured surface is somewhat fibrous. brown to dark brown. single or branched. packed with octadecylsilyl silica ge1 (5 μm in particle diameter). Inside of the Bitter Cardamon is divided vertically into three loculi by thin membranes. in long cone or column-shape. about 3. Flow rate: Adjust the flow rate so that the retention time of atropine is about 14 minutes.0%. Mobile phase: Dissolve 6.3% of saikosaponin a (C42H68O13: 780. Essential Oil Content Not less than 0. Purity Ethanol-insoluble substances—Weigh gently 1 g of Benzoin. 10 cm to 15 cm in length and 5 mm to 15 mm in diameter. The fractured surface exhibits white to pale yellow-red grains in the matrix.5 with phosphoric acid and add water to make 1000 mL.5 mm in thickness. with both ends somewhat pointed. Seeds are irregularly polygonal. Bupleurum Root Bupleuri Radix Buplerum Root is the root of Bupleurum falcatum Linné or its varieties (Umbelliferae).5 g of Benzoin. Benzoin has characteristic odor and slightly pungent and acrid taste. Use a mixture of this solution and acetonitrile (9 : 1). Selection of column: When the procedure is run with 10 μL of the standard solution under the above operating conditions.97). Acid-insoluble Ash Not more than 1. Description Bitter Cardamon is spherical to fusiform fruit. take 1 mL of the solution on a porcelain dish and add 2 to 3 drops of sulfuric acid: a deep red-brown to deep red-purple color develops. Buplerum Root. (2) Weigh 0. when dried. Benzoin is hard and tender at ordinary temperature but softened by heat.0 g). The pith at the crown reveals the same oil canals. lumes of ethanol. grayish brown to dark red-brown block varying in size. External surface is brown to dark brown. In xylem. Column temperature: A Room temperature. each loculus containing 5 to 8 seeds adhering by aril. External surface is pale brown to brown with deep wrinkles. Operating conditions Detector: An ultraviolet absorption photometer (wavelength: 210 nm). atropine and the internal standard are eluted in this order with a resolution between their peaks being not less than 4. After cooling. collect the insoluble substances through a tared glass filter (G3) and wash three times with 5 mL vo- Acid-insoluble Ash Not more than 2. Under a microscope. a transverse section reveals the thickness of cortex reaching 1/3 to 1/2 of the radius. add 10 mL of triethylamine. Apex has numerous hairy fibres from withered leaves. boil with 30 mL of ethanol on a waterbath for 15 minutes under a reflux condenser. Bitter Cardamon Alpiniae Oxyphyllae Fructus Bitter Cardamon is the fruit of Alpinia oxyphylla Miquel (Zingiberaceae).8551 QS 5 Internal standard solution⎯A solution of brucine in mobile phase (1 in 2500). Cortex is scattered with a good many intercellular schizogenous oil canals 15 μm to 35 μm in diameter. Pericarp is 0. calculated on the dried basis × QT 1 × × 0. knob-like protruding lines. (Styracaceae) Description Benzoin is the resin.0%.1016 Monographs. tangentially extended clefts in cortex. 1 to 2 cm in length. Identification (1) Heat a fragment of Benzoin in a test tube: it evolves an irritating vapor and a crystalline sublimate is produced. Upper part is thick and lower part thin. . contains not less than 0. Column: A stainless steel column.0. adjust pH to 3. with numerous longitudinal. Description Bupleurum Root is the root. and 7 to 10 mm in width.5%.4 mL (50. Benzoin Benzoinum Benzoin is the resin obtained from Styax benzoin Dryander or Styrax tonkinensis Craib ex Hart.3 g. Dry the residue at 105 o C for 4 hours: the residue is not more than 0. filter and use the filtrate as the test solution and Bupleurum Root RMPM standard solution. about 3 cm to 10 cm in length and about 0. add methanol to make exactly 50 mL. Identification Proceed as directed in the Identification under Capsicum. add 10 mL of water and shake vigorously: the lasting fine foam is produced. add 50 mL of a mixture of ammonium hydroxide and methanol (1 in 20). Flow rate: 0. for the test solution and the standard solution. Bupleurum Root RMPM standard solution and the standard solutions (1) and (2) as directed under the Thin-layer Chromatography. Capsicum Tincture Method of preparation Capsicum in medium cutting 100 g Ethanol a sufficient quantity ⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯ To make 1000 mL Prepare as direction under Tinctures. Perform the test with 5 μL each of the test solution and the standard solution as directed under the Liquid Chromatography according to the following operating conditions and determine the peak areas. Amount (mg) of saikosapon in a (C 42 H 68 O 13 ) = amount (mg) of Saikosapon in a RS × AT 5 × A S 12 Operating conditions Detector: An ultraviolet absorption photometer (wavelength: 203 nm).8 mL/minute. Bupleurum Root RMPM standard solution and the standard solutions (1) and (2) on a plate of silica gel for thin-layer chromatography. Preserve in light-resistant. Capsicum has characteristic odor and extremely pun- . respectively. Spot 10 μL each of the test solution. add 10 mL each of methanol. To the filtrate. with the above ingredients. Purity (1) Stem and leaf—Less than 10.0 g of pulverized Bupleurum Root or Bupleurum Root RMPM. Spot 20 μL each of the solution and the standard solution. Identification (1) Weigh 0. Alcohol Number Not less than 9. Bupleurum Root has characteristic order and slightly bitter taste. Column temperature: A room temperature.5 g of pulverized Bupleurum Root. Take 30. (2) Foreign matter—The amount of foreign matter other than sterns and leaves is not more than 1. about 5 mm in diameter. Description Capsicum Tincture is yellowish red liquid and has extreamly pungent taste. packed with octadecylsilyl silica ge1 for liquid chromatography (5 μm to l0 μm in particle diameter). Separately. cool. Description Capsicum is elongated conical to fusiform fruit.8 cm in width. Interior of pericarp is hollow and usually divided into two loculi. Spray evenly diluted sulfuric acid TS on the plate and warm at 105 o C for 10 minutes: the spots from the test solution and the spots from Bupleurum Root RMPM standard solution show the color and the same Rf value and 2 spots among these spots from the test solution and the purple spots from the standard solutions (1) and (2) show the color and the same Rf value. methanol and water (30 : 10 : l) to a distance of about 10 cm and air-dry the plate. Capsicum usually has remains of calyx and peduncle. Develop the plate with a mixture of dichloromethane. External surface of pericarp is lustrous and dark red to dark yellow-red.5%. add methanol to make exactly 20 mL and use this solution as standard solution.0%. Add methanol to the residue to make exactly 5 mL and use this solution as the test solution. AT and AS. weigh accurately about 10 mg of Saikosaponin a RS (previously dried in a desiccator of silica gel for 24 hours). Capsicum. Chilly Pepper Capsici Fructus Capsicum is the fruit of Capsicum annuum Linné or its varieties (Solanaceae). dissolve each in l mL of methanol and use these solutions as the standard solutions (1) and (2). Parenchyma cells contain fully starch grains and oil droplets. Perform the test with the test solution. (2) Weigh 2. Packaging and Storage tight containers. weigh l mg of Saikosaponin a RS and Saikosaponin d RS. Ash Not more than 6. containing numerous pale yellow-red seeds nearly circular and compressed.KP VIII 1017 as in the cortex.82.0%. Column: A stainless steel column. boil gently under a reflux condenser on a water-bath for 15 minutes. often bent. sonicate to extract for 2 hours and filter.0%. 20 Specific gravity⎯ d 20 : About 0. 4 mm to 6 mm in inside diameter and 15 cm to 25 cm in length.0 mL of this solution and evaporate.7 (Method 2) Acid-insoluble Ash Not more than 2. Assay Weigh accurately about 0.5 g of pulverized Bupleurum Root. Mobile phase: A mixture of acetonitrile and water (35 : 65). Separately. 0%. A ridgeline is prominent at the back and belly. and lustrous. Pericarp is odorless and tasteless. on a slide glass. The capsules are removed from the seeds before use. Bovis Calculus Acid-insoluble Ash Not more than 4.4-benzoquinonemonoimine TS on the plate and allow to stand in ammonia gas: a spot from the test solution and a blue spot from the standard solution show the same color and the same Rf value. Part II gent taste. hard and difficult to break. 3 mm to 7 mm in length and 2 mm to 4 mm in width. Acid-insoluble Ash Not more than 1. 10 mm to 20 mm in length and 5 mm to 10 mm in diameter.66). add 5 mL of ethanol. Ash Not more than 6. an albumen reveals a bent.Cassia Seed from Cassia tora is short cylindrical seed. Cassia Seed Cassiae Semen Cassia Seed is the ripe seed of Cassia tora Linné or Cassia obtusifolia Linné (Leguminosae). fanwisely dented. dissolve l mg of Capsaicin RS in l mL of ethanol and use this solution as the standard solution. light and fibrous. flat. On both sides. The dorsal side is convex. Cattle Gallstone Ash Not more than 6. . slippery. dark brown to blackish brown.0%. long ellipsoidal. each loculus containing 3 to 7 seeds joining by aril. Cardamon Cardamomi Fructus Cardamon is the ripe fruit of Elettaria cardamomum Maton (Zingiberaceae). The texture is hard and a transverse section is round or obtuse polygona1. Interior is longitudinally divided into three loculi by thin membranes. (2) Cassia obtusifolia . The seed coat is thin. Description (1) Cassia tora . Spot 10 μL each of the test solution and the standard solution on a plate of silica gel for thin-layer chromatography.0%. Ether-soluble extract—Not less Extract Content than 9. Cattle Gallstone contains not less than 20. Both end slopes. Essential Oil Content Not less than 1.1 g of pulverized Cassia Seed. Identification Weigh 0. Pericarp is thin. One end is relatively flat and the other is oblique and acuminate. 1 mm to 2 mm of small protrusion is present. then cover with moistened filter paper and heat gently the slide glass over a small flame. At one end.0%. Purity Foreign matter—Less than 1. dark-colored cotyledon. Packaging and Storage Preserve in tight containers.0% (seed). Spray evenly 2.0 mL (30. put a glass ring.0 g of pulverized Capsicum. the ventral side is longitudinally grooved and coarsely tuberculated. Seed is ovoid to long ovoid or irregularly angular. yellow-brown longitudinal lines or bands are present. 10 mm in both internal diameter and height on it.0%. cool. Take the filter paper when a yellow color has developed on the upper surface of it and place l drop of potassium hydroxide TS on the surface of the filter paper where a sublimate is present: a red color develops. centrifuge and use the supernatant liquid as the test solution. Cassia Seed has slightly characteristic odor and a little bitter taste. Cassia Seed has a acuminate shape at one end and flat at the other. Develop the plate with a mixture of ether and methano1 (19 : 1) to a distance of about 12 cm and air-dry the plate. and two yellow cotyledons are curved as S shape or overlapped. domesticus Gmelin (Bovidae). Identification Weigh 2.0% (seed).0% of conjugated bilirubin (C33H36N4O6: 584. External surface is pale yellow. previously dried in a desiccator (silica gel) for 48 hours. Separately.2%. 3 mm to 4 mm in length. External surface is greenish brown or dark brown. Cattle Gallstone is a stone formed in the gall sac of Bos taurus Linné var. Cassia Seed has characteristic odor and taste. Cardamon has characteristic odor and tastes pungent and slightly bitter. symmetrically slippery in both sides.1018 Monographs. Ash Not more than 5. 3 mm to 6 mm in length and 2 mm to 4 mm in diameter.0 g.Cassia Seed from Cassia obtusifolia is rectangular or short cylindrical seed. Under a magnifying glass. warm on a water-bath for 5 minutes. with three blunt ridges and many longitudinal lines. seed). Purity Foreign matter—Less than 1. Description Cardamon is the fruit. Perform the test with the test solution and the standard solution as directed under the Thinlayer Chromatography. The texture is tough.6dibromo-N-chloro-1. mix well. (4) Sucrose— Weigh 20 mg of pulverized Cattle Gallstone. dissolve in 200 mL of chloroform. add 10 mL of diluted hydrochloric acid (1 in 5) and 200 mL of chloroform. filter and use this filtrate as test solution for free bilirubin. ethyl acetate. water and stone. of bilirubin for the test solution and the standard solution. add 5 g of anhydrous sodium sulfate. add 2 mL of water. time of bilirubin is about 10 minutes. Determine the peak areas. Combine all of the chloroform layer. The remaining water layer is back extracted with chloroform. shake well and discard extracted chloroform. Shake well the residue with 1 mL of hydrochloric acid and 10 mL of chloroform. not show a yellowish fluorescent spot at the same Rf packed with octadecylsilyl silica gel for liquid chromavalue of the standard solution.KP VIII 1019 Description Cattle Gallstone is spherical or massive stone. Chuling is the sclerotium of Polyporus umbellatus Fries (Polyporaceae). Purity (1) Curcuma Root. Assay Proceed under the dark place as fast as possi- . concentrate A by evaporating the filtrate to 1 mL and use this as the = amount (mg) of Bilirubin RS × T × 2 AS test solution.1 g of pulverized Cattle Gallstone. Perform the test with the test solution Amount (mg) of conjugated bilirubin (C33H36N4O6) and the standard solution as directed under the Thinlayer Chromatography.= amount (mg) of total bilirubin . anhydrous acetic acid and water (100 : Operating conditions 30 : 2 : 3) to a distance of about 10 cm and air-dry the Detector: A visible absorption photometer (waveplate. bath. followed by slight sweetness taste. Filter after cooling. disslve in methanol to make 5 mL and use this as the standard solution.5 hours in a water-bath at 61 ± 2 o C and allow to stand.0%. To 1 mL of the filtrate. Cattle Gallstone has slight odor and slightly bitter. Fractured surface shows yellow-brown to red-brown annular rings. (2) Weigh 10 mg of Cattle Gallstone. about 4 mm to 6 mm in inside diameter and 15 cm to 30 cm in length. Polyporus Ash Not more than 10. tography (5 μm to 10 μm in particle diameter). Separately. Transfer the chloroform extract into a separatory funnel. Allow to stand for 10 minutes and take the chloroform layer. Pipet 5 μL each of the test solution and the standard solution and perform the test as directed under the Liquid Chromatography according to the following operating conditions. respectively. about 25 o C .5 mL of acetic anhydride and 2 drops of sulfuric acid and shake: a yellow-red to deep red color develops and changes through dark red-purple to dark red-brown. filter and wash the residue with 10 mL of petroleum ether. add 50 mL of methanol and heat for 30 minutes in a water-bath Amount (mg) of total bilirubin or free bilirubin with reflux condensor. Identification (1) Weigh 0. Examine under ultraviolet light (main wavelength: 436 nm). separate the chloroform layer when it acquires a yellow-brown color and shake with 5 mL of barium hydroxide TS: a yellowbrown precipitate is produced. often containing white granular substances or thin layers in these annular rings. length: 365 nm): the spot from the test solution dose Column: A stainless steel column. dissolve in chloroform to make 100 mL. Weigh accurately about 20 mg of Bilirubin RS. add 10 mL of chloroform. ble. (3) Starch— Weigh 5 mg of pulverized Cattle GallMobile phase: A mixture of methanol. Develop the plate with a mixture of chloroform. The flask is washed with a small volume of chloroform and place the chloroform layer into the separatory funnel. heat for 1. add 2 mL of water. Shake 10 mg of the residue with 3 mL of acetic anhydride for 1 to 2 minutes. heat for 5 minutes in a wateracetic acid (900 : 98 : 2). add 2 mL of anthrone TS Chuling and shake: the solution does not show deep bluish green to dark green color. Spot 10 μL each of the test so. add 10 mL of petroleum ether.1 g of pulverized Cattle Gallstone. Separately. shake for 15 minutes and filter. Curcuma Longa Rhizome —Weigh 0. add 2 to 3 drops of iodine TS: the Flow rate: Adjust the flow rate so that the retention solution does not show bluish purple color. Add chloroform to the filtrate to make 200 mL and use this solution as test solution for total bilirubin. and yellow-brown to red-brown. Seperately weigh 1 mg of Curcumin RS. shake for 30 minutes. mix well and filter. After cooling. Texture is light. (2) Synthesized pigments—Weigh 2 mg of pulveColumn temperature: A constant temperature of rized Cattle Gallstone and add 1 mL of dilute hydrochloric acid: the solution does not show purple color. add a mixture of 0. weigh accurately about 0. Weigh accurately about 0.amount (mg) of free lution and the standard solution on a plate of silica gel bilirubin with fluorescent indicator for thin-layer chromatography. use this solution as standard solution. 1 cm to 4 cm in diameter.1 g of the fine powder of Cattle Gallstone to a Erlenmeyer flask. fragile and brittle.1 g of pulverized Cattle Gallstone. AT and AS. add 10 mL of methanol. Drop the filtrate on the filter paper and examine under a ultraviolet light (365 nm): fluorescence of bluish white color develp. calculated on the dried basis. irregularly long mass-shaped. 1 mm to 5 mm in thickness. Loss on Drying Not more than 11. Cimicifuga dahurica Maximowicz or Cimicifuge foetida Linné (Ranunculaceae).0% . Fractured surface is cork-like and almost white to pale brown and a white speckled pattern on the inner region. Cibot Rhizome is the rhizome of Cibotium barometz J. knotted. The upper part is exhibiting several reddish brown woody petioles and the lower part is showing remains of black fibrous roots. Chuling is odorless and tasteless. Part II Description Chuling is the sclerotium. add 10 mL of water. Chuling is breakable. thin layer. 2) Weigh 1 g of pulverized Cibot Rhizome. add 5 mL of acetone and heat on a water-bath for 2 minutes. Identification Weigh 0. boil in the water bath for 15 minutes and filter. or such bark from which a part of the periderm has been removed.0%. Dissolve the residue in 5 drops of acetic anhydride and add 1 drop of sulfuric acid: a red-purple color develops and immediately changes to dark green. exhibiting a pale brown. Cibot Rhizome is odorless and the taste is weak and slightly astringent. Cimicifuga simplex Wormskjord. Drop the 1% ferric chloride solution to 2 mL of the filtrate:: the filtrate turn to dark green.5%. 10 cm to 30 cm in length and 2 cm to 10 cm in diameter. External surface is dark brown to grayish black.0%. Extract Content Dilute ethanol-soluble extract— Not less than 22.0%. 5 cm to 50 cm in length and 15 cm to 50 cm in diameter. Cinnamon Bark is brittle and the fractured surface is slightly fibrous. Acid-insoluble Ash Not more than 4. Smith (Dicksoniaceae).5%. Acid-insoluble Ash Not more than 1. powdered Cimicifuga Rhizome does not contain crystal druses in the parenchyma. Cinnamon Bark is the bark of the trunk of Cinnamomum cassia Presl or other species of the same genus (Lauraceae). with many remains of roots. Cinnamon Bark Cinnamomi Cortex Description Cinnamon Bark is usually semi-tubular or tubularly rolled pieces of bark. with remains of golden hairs.5 g of pulverized Chuling. red-brown. sometimes with scars of terrestrial stems. and irregularly shaped mass.03% of cinnamic acid (C9H8O2: 148. The center of the scar is dented and the circumference of the scar is pale and shows a radial pattern.1020 Monographs. Texture is hard and uneasily broken.0%. Ash Not more than 16. Cibot Rhizome Cimicifuga Rhizome Cimicifugae Rhizoma Cimicifuga Rhizome is the rhizome of Cimicifuga heracleifolia Komarov. a transverse section reveals a primary cortex and a secondary cortex divided by an almost continuous ring consisting of stone cells. Ash Not more than 2. External surface is deep brown. 6 cm to 18 cm in length and 10 mm to 25 mm in diameter. with numerous dents and coarse wrinkles. Secondary cortex of Cinnamon Bark lacks stone cells and .0%. boil in the water bath for 15 minutes and filter. Under a microscope. Cibotii Rhizoma Ash Not more than 9. irregularly shaped. Extract Content Dilute ethanol-soluble extract— Not less than 18. Description Cimicifuga Rhizome is the rhizome. Description Cibot Rhizome is the rhizome.16). usually 5 cm to 10 cm in length. Cinnamon Bark contains not less than 0. Texture is light and hard and the fractured surface is fibrous. Identification 1) Weigh 1 g of pulverized Cibot Rhizome. Nearly round bundles of fibers are in the outer region of the ring and wall of each stone cell is often thickened in a U-shape. Texture is light. External surface is dark red-brown and the inner surface is red-brown and smooth. Purity Rhizome of Astilbe species—Under a microscope. Cimicifuga Rhizome is odorless and has bitter and slightly astringent taste. filter and evaporate the filtrate to dryness. Pith is dark brown and often hollow. External surface is grayish brown to blackish brown. AT and AS. add 10 mL of methanol. To the residue. Parenchyma tissue is scattered with oil cells. Identification Weigh 2 g of pulverized Cinnamon Bark. Ash Not more than 5. with sharp pedurcle scars in apex. Amount (mg) of cinnamic acid (C9H8O2) A 1 = amount (mg) of Cinnamic Acid RS × T × AS 10 Operating conditions Detector: An ultraviolet absorption photometer (wavelength: 280 nm). add 1 mL of methanol. Combine all the extracts. 4 mm to 6 mm in inside diameter and 15 cm to 25 cm in length. sweet and pungent taste at first. Perform the test with the test solution and the standard solution as directed under Thin-layer Chromatography. yellowish white to pale yellowish brown.0%. Examine under ultraviolet light (main wavelength: 254 nm): the two spots among several spots of the test solution and the spots of the standard solution (1) and the standard solution (2) show the same color and the same Rf value. Mobile phase: A mixture of methanol. use the saturated solution of Hesperidin RS in methanol as the standard solution. Determine the peak areas. a transverse section reveals secretive parenchymatous cells are lined. add 60 mL of ether. Develop the plate with a mixture of toluene. formic acid and water (20 : 10 : 1 : 1) to a distance of about 10 cm and air-dry the plate.0% Ash Not more than 5. Under a microscope. add 60 mL of ether and proceed in the same manner. mucilage cells and cells containing fine needles of calcium oxalate and parenchyma cell contains starch grains. weigh accurately about 10 mg of Cinnamic Acid RS. External surface is grayish green to bluish green. Develop the plate with a mixture of hexane and ethyl acetate (2 : 1) to a distance of about 10 cm and air-dry the plate. 2) Evaporate 5 mL of the filtrate of 1) to about 1 mL. later rather mucilaginous and slightly astringent. respectively. Spot 10 μL of the test solution on a plate of silica gel with fluorescent indicator for thinlayer chromatography. Identification 1) Weigh 0. Perform the test with 10 μL each of the test solution and the standard solution as directed under the Liquid Chromatography according to the following operating conditions. water and anhydrous acetic acid (12 : 88 : 1). Separatlely weigh 1 mg each of Cinnamic Acid RS and 1 mg of Cinnamaldehyde RS.0% . Perform the test with this solution as directed under the Thin-layer Chromatography. ethyl acetate. Description Citrii Unshiu Immature Peel is the globular pericarp. packed with octadecylsilyl silica gel for liquid chromatography (5 μm to 10 μm in particle diameter). and use each of these solutions as the standard solution (1) and the standard solution (2). Loss on Drying Not more than 15. To the residue. filter and use the filtrate as the test solution.5% (6 hours). 5 mm to 20 mm in diameter. Spray 5% solution of the aluminium chloride TS to a plate and examine under ultraviolet light (main wavelength: 365 nm): a fluorescent spot among the several spots form the test solution and a spot from the standard solution show the same color and the some Rf value. Citrii Unshiu Immature Peel has characteristic odor. wash with water and dehydrated with anhydrous sodium sulfate. Separately. Citrii Unshiu Immature Peel Citri Unshius Pericarpium Immaturus Citrii Unshiu Immature Peel is the unripe pericarp of Citrus unshiu Markovich or Citrus reticulata Blanco (Rutaceae). bitter and slightly pungent tastes. Add small amount of magnesium powder to 1 ml of the filtrate and add 3 to 5 droplets of hydrochloric acid: a scarlet color slowly appears. previously dried more than 12 hours in the desiccator. Column temperature: A ordinary temperature. Separately. add methanol to make exactly 100 mL and use this solution as the standard solution. rough and wrinkled. Loss on Drying Not more than 12. use this solution as the test solution. add methanol to make exactly 10 mL and use this solution as the test solution. Repeatedly. add 10 mL of ether. Spot 5 μL each of the test solution and the standard solution on a plate of silica gel with fluorescent indicator for thin-layer chromatography. Column: A stainlees steel column. respectively. extract for 2 hours and the extract is put into a separatory funnel.KP VIII 1021 is with a small number of sclerenchymatous fibers coarsely scattered. Assay Weigh accurately about 2 g of pulverized Cinnamon Bark in a Soxhlet extractor. Cinnamon Bark has characteristic aroma. Flow rate: 2. develop the plate with a upper layer of a mixture of toluene. ethyl acetate. formic acid and water (20 : 10 : 1 : 1) to a distance of about 8 cm and air-dry the plate. with globular fruit stalk scars. of cinnamic acid of the test solution and the standard solution. 15 mm to 40 mm in thickness. The ether is evaporated in vacuum. extract for 20 minutes under a reflux condenser and filter.0 mL/minute. shake for 3 minutes.3 g of pulverized Citrii Unshiu Immature Peel. Description Clove is paddle-shaped. with numerous small dents associated with oil sacs. Perform the test with l0 μL each of the test solution and the standard solution as directed under the Liquid Chromatography according to the following operating conditions. To 5 mL of the filtrate. Column temperature: A ordinary temperature. extract under a reflux condenser for 2 hours and filter. Column: A stainless steel column. enclosing numerous stamens and a single style.5 g of pulverized Citrus Unshiu Peel. packed with octadecylsilyl silica ge1 (5 μm to l0 μm in particle diameter). Determine the peak areas. a transverse section reveals irregular. To the residue. Purity (1) Stem—Less than 5. 2) Weigh 0. Weigh accurately about 20 mg of Hesperidin RS. Clove has strong. bast fiber in phloem.0% Citrus Unshiu Peel Combine all filtrates.1 g of magnesium and 1 mL of hydrochloric acid and allow to stand: a red-purple color develops.0% Essential Oil Content Not less than 0. Separately.1 mL of the mixture of xylene and essential oi1.0 mL/minute. Spot 10 μL each of the test solution and the standard solution on a plate of silica gel with a fluorescent indicator for thin-layer chromatography. Assay Weigh accurately about 0. Parenchyma cell surrounded by vascular bundles contains aggregate crystals of calcium oxalates and oil droplets of essential oil. dissolve in methanol to make 100 mL and use this solution as the standard solution. about 2 mm in thickness.2 mL (50 g) Extract Content Dilute ethanol-soluble extract— Not less than 12.0%. . add 60 mL of methanol. add 30 mL of methanol and proceed in same manner. imbricated petals. AT and AS. warm on a waterbath for 2 minutes and filter. External surface is yellow-red to dark yellow-red to dark yellow-brown. Part II Acid-insoluble Ash Not more than 1.5 g of pulverized Citrus Unshiu Peel. Under a microscope. plateshaped pieces of pericarp. Perform the test with the test solution and the standard solution as directed under the Thin-layer Chromatography. crowned by 4 thick sepals and 4 nearly spherical. Deve1op the plate with a mixture of ethyl acetate. Clove Syzygii Flos Clove is the flowering bud of Syzygium aromaticum Merrill et Perry (Myrtaceae). of hesperidin for the test solution and the standard solution. Citrus Unshiius Pericarpium Amount (mg) of hesperidin (C 28H34O15) Citrus Unshiu Peel is the ripe pericarp of Citrus unshiu Markovich or Citrus reticulate Blanco (Rutaceae). respectively. Loss on Drying Not more than 13.0% of hesperidin (C28H34O15: 610. Flow rate: 1.1022 Monographs. obtained in the Essential oil content. weigh 1 mg of Hesperidin RS. add 0. Texture is light and brittle.0% (6 hours).5 : 3) to a distance of about 10 cm and air-dry the plate.0%. followed by a slight numbness of the tongue. consists of slightly compressed and four-sided receptacle. 4 mm to 6 mm in inside diameter and 15 cm to 25 cm in length. dark brown to dark red buds. membranous. two layered vascular bundles surrounded by collenchyma in the inner surface. methanol and water (100 : 17. Interior is white to pale grayish yellowbrown. Use the filterate as the test solution. Mobile phase: A mixture of methanol and water (40 : 60). Identification 1) Weigh 0. Ash Not more than 4. long ovoid oil sacs in the outer surrounding surface.0%. Citrus Unshiu Peel has characteristic aroma odor and bitter and slightly pungent taste. calculated on the dried basis. add 2 mL of ethanol and add l to 2 drops of ferric chloride TS: a green to blue color develops. add 10 mL of methanol. add 10 mL of methanol. 10 mm to 18 mm in length.5 g of pulverized Citrus Unshiu Peel. Citrus Unshiu Peel contains not less than 4. sonicate for 20 minutes and filter. add methanol to make exactly 100 mL and use this solution as the test solution. AT AS Operating conditions Detector: An ultraviolet absorption photometer (wavelength: 280 nm).56).. Identification Take 0. characteristic odor and pungent taste. Spray the aluminium chloride TS to the plate and examine under ultraviolet light (main wavelength: 365 nm): One spot among several spots from the test solution and the bluish white spot from the standard solution of the standard solution show the same color and the same Rf value. (2) Foreign matter—The amount of foreign matter other than the stem is not more than 1. dissolve in 1 mL of methanol and use this solution as the standard solution. and spongy tissue in vascular bundles. = amount (mg) of Hesperidin RS × Description Citrus Unshiu Peel is irregular. 10 cm to 35 cm in length and 4 mm to 20 mm in diameter. and the apex of each stem scar is sunkenly dotted. Margin of the vertical section irregularly branched. ma-yuen Stapf (Gramineae). (2) Root of Codonopsis pilosula var. semi-translucent and occasionally with hollows. Essential Oil Content Not less than 1. Codonopsis pilosula Nannfeldt var. Interior is grayish white to grayish brown. Under a micro- . and the bark is yellowish white.0%. Dense transverse annulations are occurring below the root stock. Shen or Codonopsis tangshen Oliver (Campanulaceae). Ash Not more than 6. about 6 mm in length and about 5 mm in width with a slightly hollowed apex and base. modesta consists of the root. a transverse section reveals white endosperm in the dorsal side and pale yellow scutellum in the hollow of the ventral side. Cnidium Rhizome has characteristic odor and slightly bitter taste. add 10 mL of water. Packaging and Storage Preserve in tight containers. Pour this solution to test tube and shake vigorously: the fine persistent foam is rising. brown and membranous pericarp and seed coat are attached. relatively cleft or radial. Texture is slightly soft and campact. Description Coix Seed is ovoid or broad ovoid seed. thickwalled and lignified xylem fibers appear in groups of various sizes. Acid-insoluble Ash Not more than 0. Identification Weigh 1 g of pulverized Codonopsis Pilosula Root.0%. long cylindrical.Codonopsis Pilosula Root from Codonopsis tangshen consists of the root. (3) Root of Codonopsis tangshen . Extract Content Dilute ethanol-soluble extract— Not less than 35. modesta . (Umbelliferae). Coicis Semen Coix Seed is the ripe seed of Coix lachryma-jobi Linné var. External surface is grayish brown to dark brown. Under a magnifying glass. with numerous warty prominent stem scars and buds on the root stock. T. Acid-insoluble Ash Not more than 2. Dense transverse annulations are occurring below the root stock. In the xylem. slightly curved. frequently up to over half length of the root. Codonopsis Pilosula Root has the characteristic odor and slightly sweet taste. Ash Not more than 6.Codonopsis Pilosula Root from Codonopsis pilosula consists of the root. knotted rhizome. External surface is yellowish white to grayish white. the fractured surface is less cleft. External surface is grayish yellowe to yellowish brown.2 mL (50 g). frequently with blackish brown gelatinous substances at the fractured area of the rootlet. Dorsal side is mostly white and powdery. Description (1) Root of Codonopsis pilosula .0%.KP VIII 1023 Ash Not more than 7. from which the seed coat has been removed. Texture is dense and hard.6 mL (10.0%. External surface is yellowish brown to grayish brown. In the furrow on the ventral surface. but rarely remaining as grains of 5 μm to 25 μm in diameter. Description Cnidium Rhizome is irregular massive. Acid-insoluble Ash Not more than 1. Under a microscope. Loss on Drying Not more than 13.0 g). with gathered nodes and with knobbed protrusions on the node.0%.0% .Codonopsis Pilosula Root from Codonopsis pilosula var. Starch grains are usually gelatinized. a transverse section reveals cortex and pith with scattered oil canals.0% Essential Oil Content Not less than 0. Dorsal side is distended and ventral side is longitudinally and deeply furrowed in the center. boil and cool. Codonopsis Pilosula Root Coix Seed Codonopsis Pilosulae Radix Codonopsis Pilosula Root is the root of Codonopsis pilosula Nannfeldt.5%. 5 cm to 10 cm in length and 3 cm to 5 cm in diameter. Crystals of calcium oxalate are not obsered. with distinctly longitudinal wrinkles. Cnidium Rhizome Cnidii Rhizoma Cnidium Rhizome is the rhizome or the rhizome passed through hot water of Cnidium officinale Makino or Ligusticum chuanxiong Hort. modesta L. Fractured surface is more cleft and the bark is grayish yellow or pale brown. Some is up to half length of the root while the transverse annulations are rare or absent in some cultivars. Whole root is showing longitudinal wrinkles and scattered transverse lenticel-like protrudings. 10 cm to 45 cm in length and 5 mm to 20 mm in diameter. occasionally cut lengthwise. Texture is slightly hard or tenacious. the bark is pale yellowish white or pale brown and the wood is pale yellow. Fractured surface is somewhat evenly. 10 cm to 35 cm in length and 5 mm to 25 mm in diameter. gradually sparse downwards. nearly smooth and with numerous lenticels. Ash Not more than 12. Identification Mix 1 mL of Condurango Fluidextract with 5 mL of water. Ash Not more than 3. Description Coptis Rhizome is irregular. the yellowish spot shows the Rf value about 0. Coptis chinensis Franchet. (2) Place a small amount of Coix Seed on a slide glass.63 Loss on Drying Not more than 14. Perform the test with the test solution as directed under the Thin-layer Chromatography. ethanol and glycerin (5 : 3 : 2) as the first solvent and a suitable quantity of a mixture of purified water and ethanol (3 : 1) as the second solvent. from which the roots have been removed practically. Under a microscope.0%. Develop the plate with a mixture of petroleum ether. calculated on the dried basis. a transverse section reveals a cork layer composed of several layers of thin-walled cells. usually 10 μm to 15 μm in diameter and compound starch grains have a reddish brown color. add 5 mL of water. filter.2% of berberine [as berberine chloride (C20H18CINO4: 371. External surface is grayish brown to dark brown. Y. and acetic acid (10 : 3 : 0. Coptis deltoidea C. or more or less scaly and rough. Purity Foreign matter—The xylem and other foreign matter do not exceed 2. 4 cm to 15 cm in length and 1 mm to 6 mm in thickness. Packaging and Storage Preserve in tight containers.0%. and heat the clear solution: turbidity is produced. Description Condurango is tubular or semi-tubular pieces of bark. 3 μm to 20 μm in diameter. and use this solution as the test solution. Identification Weigh l g of pulverized Condurango. Fractured surface is rather fibrous. Parenchyma cells contain starch grains. Packaging and Storage Preserve in tight containers. Part II scope. Condurango Fluid Extract Method of preparation Take medium powder of Condurango and the fluid extract as directed under Fluid Extracts using a suitable quantity of a mixture of purified water. Coix Seed adheres to the teeth on chewing. and filter.0% (6 hours). 2 cm to 4 cm. Coptis Rhizome is the rhizome of Coptis japonica Makino.1024 Monographs. but it becomes almost clear upon cooling. add 10 mL of methanol. cylindrical cells in the middle layer of pericarp. cool and filter: the clear filtrate becomes turbid on heating. and thin and numerous starch grains in the cell wall. Coix Seed has slightly characteristic odor and slightly sweet taste. heat on a water bath for 10 minutes. Coptis Rhizome contains not less than 4. coexisting with fixed oil and with aleuron grains in parenchyma cells. and small spheroidal starch grains. a transverse section reveals irregular. Cork layer is pale grayish brown. External surface is grayish yellowish brown. rarely up to 10 cm in length and 2 mm to 7 mm in diameter. Spot 5 μL of the test solution on the plate of silica gel for thin-layer chromatography. or rosette aggregates of calcium oxalate. Condurango has slight odor and bitter taste. Generally. with ring nodes and with numerous remains of rootlets. but becomes clear again upon cooling. Articulate latex tubes are scattered in both cortices. Condurango Fluidextract has characteristic odor and bitter taste. have a blue purple color. Cheng et Hsiao or Coptis teeta Wallich (Ranunculaceae). remains of petiole are present at one end. Description Condurango Fluide extract is brown liquid. ethylacetate. add drop-wise iodine TS and examine under a microscope: nearly equi-diameter and obtuse polygonal simple starch grains. (3) Weigh 1 g of pulverized Coix Seed. polygonal cells in endosperm. Condurango Coptis Rhizome Coptidis Rhizoma Condurango Cortex Condurango is the bark of the trunk of Marsdenia condurango Reichenbach fil. (Asclepiadaceae). if necessary. Inner surface is pale grayish brown and longitudinally striated.81)]. Fractured surface is fibrous on the outer region and generally granular in the inner region. Identification (1) Add iodine TS drop-wise to a transverse section of Coix Seed: a dark red-brown color develops in the endosperm and a dark gray color develops in the scutellum. slightly curved and often branched. cortex is yellowish brown to reddish- .1) to a distance of about 10 cm and air-dry the plate. cylindrical rhizome. Primary cortex has numerous stone cell groups and secondary cortex contains phloem fiber bundles scattered inside the starch sheath consisting of one-cellular layer. Spray the iodide steam to the plate. Evaporate the filtrate to make 2 mL.0%. the relative deviation of the peak area of berberine is not more than 1. respectively. External surface is dark red-urple to dark purple. . Assay Weigh accurately about 0. Column temperature: A constant temperature of about 40 o C . System suitability System performance: Dissolve 1 mg each of Berberine Chloride RS and Palmatine RS in 10 mL of methanol. Repeat the above procedure twice with the residue. Cornus Fruit has slight odor and sour and slightly sweet taste. Combine all filtrates.0%. Column: A stainless steel column. (2) Weigh 0. a transverse section of Coptis Rhizome reveals a cork layer. Spot 5 μL each of the test solution and the standard solution on a plate of silica gel with a fluorescent indicator for thin-layer chromatography. When the procedure is run with 20 μL of this solution under the above operating conditions.KP VIII 1025 yellowish brown. Cornus Fruit Ash Not more than 4. Perform the test with 20 μL each of the test solution and the standard solution as directed under the Liquid Chromatography according to the following operating conditions. Separately. add l mL of hydrochloric acid and l to 2 drops of hydrogen peroxide TS and shake: a redpurple color develops. dissolve in methanol to make exactly 100 mL and use Description Cornus Fruit is the fruit. using 30 mL and 20 mL volumes of a mixture of methanol and dilute hydrochloric acid (100 : 1). Perform the test with the test solution and the standard solution as directed under the Thin-layer Chromatography. The texture is soft. shake for 2 minutes. filter and use the filtrate as the test solution. Operating conditions Detector: An ultraviolet absorption photometer (wavelength: 345 nm). heat under a reflux condenser on a water-bath for 30 minutes. Determine the peak areas. Amount (mg) of berberine [berberine chloride (C20H18ClNO4)] = amount (mg) of Berberine Chloride RS. Loss on Drying Not more than 11. and meullary ray is distinct. Coptis Rhizome colors the saliva yellow on chewing. flattened oblong.0% (105 o C . Separately.5 g of pulverized Coptis Rhizome. Flow rate: Adjust the flow rate so that the retention time of berberine is about 10 minutes. stone cells or stone cells with thick and lignified cells are sometimes recognized.5%. Coptis Rhizome has slight odor and extremely bitter and lasting taste.4 g of monobasic potassium phosphate and 1. weigh accurately about 10 mg of Berberine Chloride RS (previously determine the water content). To the last residue. add 10 mL of water. of berberine for the test solution and the standard solution. Examine under ultraviolet light (main wavelength: 365 nm): one spot among the spots from the test solution and a yellow to yellow-green fluorescence spot from the standard solution show the same color and the same Rf value. In pith.7 g of sodium lauryl sulfate in l000 mL of a mixture of water and acetonitrile (1 : 1). Parenchyma cell of the cortex usually exhibits groups of stone cells near the cork layer and yellow phloem fibers near the cambium. System repeatability: When the test is repeated 6 times with the standard solution under the above operating conditions. Cornus Fruit contains not less than 0.0% Cornus Fruit is the ripe fruit of Cornus officinalis Siebold et Zuccarini (Cornaceae).38). packed with octadecylsilyl silica gel (5 μm to 10 μm in particle diameter). AT and AS. 6 hours). add methanol to make exactly 100 mL and use this solution as the test solution. dissolve in l mL of methanol and use this solution as the standard solution. composed of thin-walled cork cells. water and acetic anhydride (7 : 2 : 1) to a distance of about 10 cm and air-dry the plate. xylem is yellow to reddish yellow. lustrous and with coarse wrinkles. A calculated on the anhydrous basis × T AS Identification (1) Weigh 0. cool and filter. palmatine and berberine are eluted in this order and clearly dividing each peak. Pith is large. A crack-ike scar is formed by removal of true fruit. from which the seeds have been removed. add 20 mL of methanol. weigh l mg of Berberine Chloride RS. Under a microscope. allow to stand for 10 minutes with occasional shaking and filter. Parenchyma cells contain minute starch grains. this solution as the standard solution.5% of loganin (C17H26O10: 390.5 g of pulverized Coptis Rhizome. and pith is yellowish brown. 15 mm 20 mm in length. add 10 mL of methanol. and about 1 cm in width. Xylem consists chiefly of vessels. Develop the chromatogram with a mixture of n-butanol. tracheae and wood fibers.5 g of pulverized Coptis Rhizome. shake well and filter. 4 mm to 6 mm in inside diameter and 15 cm to 25 cm in length. A scar of calyx is present at upper part and a scar of fruit stalk at base. To 2 to 3 drops of the filtrate. Mobile phase: Dissolve 3. Corni Fructus Acid-insoluble Ash Not more than 1. add 30 mL of a mixture of methanol and dilute hydrochloric acid (100 : 1). Column temperature: A room temperature. Cornus Fruit RMPM standard solution and the standard solution as directed under the Thin-layer Chromatography. Part II Identification Weigh 1 g each of pulverized Cornus Fruit or Cornus Fruit RMPM. A pointed hilum and a caruncle scar are present at one end. Amount(mg)of loganin(C17H26O10 ) = amount(mg)of LoganinRS × AT AS Operating conditions Detector: An ultraviolet absorption photometer (wavelength: 240 nm). add methanol to make exactly 100 mL and use this solution as the test solution. Develop the plate with a lower layer of a mixture of dichloromethane. Column: A stainless steel column. Extract Content Dilute ethanol–soluble extract— . Ash Not more than 3.0%. of loganin for the test solution and the standard solution. extract with a reflux condenser on a water-bath for 2 hours and filter. filter and use these solutions as the test solution or Cornus Fruit RMPM standard solution. Corydalis Tuber Corydalis Tuber Corydalis Tuber is the tuber of Corydalis ternata Nakai or other species of the same genus (Papaveraceae). Endosperm cells are almost circular. Ash Not more than 3. dissolve in 100 mL of methanol and use this solution as the standard solution. Seperately. and with crystals of calcium oxalate. add 50 mL of methanol. Spray evenly diluted sulfuric acid TS and heat at 105 o C for 10 minutes: the spots from the test solution and the spots from Cornus Fruit RMPM standard solution show the same color and the same Rf value.0%. add 10 mL of dilute acetic acid. Under a microscope. Mobile phase: A mixture of methanol and water (30 : 70). External surface of the testa is dark reddish brown to grayish brown with sporadic black spots. a slightly dented chalaza at the other end. l cm to 2 cm in diameter. add 10 mL each of ethanol. Testa is thin and brittle. methanol and water (60 : 35 : 15) to a distance of about 10 cm and air-dry the plate. dissolve in 2 mL of ethanol and use this solution as the standard solution.5%. AT and AS.0 mL/minute. weigh 1 mg of Loganin RS. transverse section shows a cavity like a lens and two thin cotyledons are contained in the cavity. To the filtrate.2 g. a pointed hilum which is not distinct. Cornus Fruit RMPM standard solution and the standard solution on a plate of silica gel for thin-layer chromatography. packed with octadecylsilyl silica ge1 (5 µm to 10 µm in particle diameter).0%. Flow rate: 1. from which the testa has been removed. The weight of one seed is approximately 0. External surface is grayish yellow to grayish brown. Purity Foreign matter—The amount of fruit stalk and other foreign matter contained in Cornus Fruit is less than 2. a transverse section reveals epidermal cells of seed coat are long quadangular. A raphe makes a distinct line from hilum to chalaza. with stem scar at one end and with several warty protrusion at the base. Corydalis Tuber is almost odorless and has bitter taste. Crotonis Semen Croton Seed is the seed of Croton tiglium Linné (Euphorbiaceae). Description Corydalis Tuber is nearly flattened spherical or polygonal tuber. 4 mm to 6 mm in inside diameter and 15 cm to 25 cm in length. Spot 10 μL each of the test solution. Croton Seed is odorless and tastes oily at first and pungent later. endosperm is covered with a membranous perisperm. Fractured surface is smooth or granular and yellow to grayish yellowish brown.5 g of pulverized Corydalis Tuber. The back surface of the seed is slightly curved. Perform the test with the test solution. Identification Weigh 0. cool and filter. irregular sawlike and bented beneath primary layer. Croton Seed Ash Not more than 5. filled with aleurone grains and fatty oil. Under a magnifying glass. Perform the test with 10 µL each of the test solution and the standard solution as directed under the Liquid Chromatography according to the following operating conditions and determine the peak areas. triangular seed. heat on a waterbath for 3 minutes with occasional shaking. Weigh accurately about 10 mg of Loganin RS.1026 Monographs. and 7 mm to 9 mm in width and 5 mm to 6 mm in thickness. 10 mm to 15 mm in length. add 3 drops of Meyer’s TS: an orange-yellow precipitate is produced. To 5 mL of the filtrate. Assay Weigh accurately about 1 g of pulverized Cornus Fruit. Texture is hard. Description Croton Seed is slightly ovate. respectively. and one spot among the spots from the test solution and a spot from the standard solution show the same color and the same Rf value. shake for 5 minutes. of Curcuma wenyujin Y.. the outermost layer usually consists of cortex layer with 4 to 10 layers or a part of cortex. External surface is grayish brown. Curcuma Root from Curcuma longa has characteristic odor and very pungent taste. Spot 10 μL each of the test solution and the standard solution on a plate of silica gel for thin-layer chromatography. A transverse section is orange in center. Texture is hard and a transverse section is grayish brown with horn. endodermis ring is distinct and parenchyma is star-like scattered. The rhizome is irregularly ovoid. and yellowish brown to reddish brown in outer surface. Curcuma Root from Curcuma phaeocaulis has characteristic odor and weak taste Loss on Drying Not more than 16. boiled or steamed thoroughly. Under a microscope. Curcuma longa Linné. (Zingiberaceae). gradually changes into brown color and returns to reddish orange color when it keeps long. sonicate for 1 hour.0%. add 3 mL of methanol. slightly thick and big.0%. H. Chen et C. slightly curved. G.KP VIII 1027 Not less than 18. Spray evenly the plate with diluted sulfuric acid TS and heat at 105 o C for 10 minutes: one spot among the spots from the test solution and a spot from the standard solution show the same color and the same Rf value. Description 1) Curcuma wenyujin—Curcuma Root from Curcuma wenyujin is ellipsoidal and ovoid root tuber.7) to a distance of about 10 cm and air-dry the plate. Ash Not more than 7. 10 mm to 12 mm in diameter. 10 mm to 18 mm in diameter. curved. Curcuma Root from Curcuma kwangsiensis has characteristic odor and slight pungent and bitter taste. 2) Curcuma longa—Curcuma Root from Curcuma longa is pyramidal root tuber. Add 1 drop of ammonia TS : the color develops as dark blue-black immediately.0%. Curcuma Root from Curcuma wenyujin has characteristic odor and slight bitter taste. with ring-nodes. (2) Take a small amount of pulverized Curcuma Longa Rhizoma and add 1 drop each of ethanol and ether on the filter paper. One layer of endodermis divides cortex and stele. sand crystals or solitary crystals of calcium oxalate and gelatinized starch grains are observed in the parenchyma cells. Under a magnifying glass. 4) Curcuma phaeocaulis—Curcuma Root from Curcuma phaeocaulis is long ellipsoidal root tuber. Curcuma Longa Rhizoma has characteristic odor and bitter and irritating taste and the color of saliva becomes yellow. External surface is grayish brown. cylindrical. Yellow substances. or coarse reticular wrinkled. Removed with powder when the filter paper is dried : the filter paper becomes yellow. Separately. The rhizome with cork layer is yellowish red and lustrous. (3) Weigh 1 g of pulverized Curcuma Longa Rhizoma. or the root tuber from which the periderm has been removed. slightly flat. 15 mm to 35 mm in length. add 1 drop each of sulfuric acid and ethanol and mix them on the glass : a purplish red color develops. Endodermis ring is distinct. 1 cm to 3 cm in diameter and 2 cm to 5 cm in length. methanol and formic acid (94 : 4 : 0. . 20 mm to 65 mm in length. 3) Curcuma kwangsiensis—Curcuma Root from Curcuma kwangsiensis is long conical. about 1 cm in diameter and 2 cm to 6 cm in length. External surface is shallow longitudinal. and dried. Ling. Add saturated boric acid solution and boil : reddish orange color develops. and often secondary rhizome.5 g of pulverized Curcuma Longa Rhizoma. Liang. one end thin or long. Lee et C. 12 mm to 25 mm in diameter. or fusiform. or grayish yellow with longitudinal winkles. Ash Not more than 9. 10 mm to 15 mm in diameter. Identification (1) Weigh 0. with uneven longitudinal and pale brown wrinkles.0%. or Curcuma phaeocaulis Val. dissolve 1 mg of Curcumin RS in 10 mL methanol and use this as the standard solution. 25 mm to 45 mm in length. F. Perform the test with the test solution and the standard solution as directed under the Thin-layer Chromatography. or long globular root tuber. Curcuma Root Curcumae longae Radix Curcuma Root is the dried steamed root tuber. or both ends tapering. Develop the plate with a mixture of dichloromethane. filter and use filtrate as the test solution. Oil cells are scattered in parenchyma tissue.0%. Description Curcuma Longa Rhizome consists of primary rhizome. Curcuma Longa Rhizome Curcumae Longae Rhizoma Curcuma Longa Rhizome is the rhizome. The cortex and stele consist of parenchyma tissues and vascular bundles scattered. 35 mm to 70 mm in length. Curcuma kwangsiensis S. The texture is hard and difficult to break and the fractured surface is horny and lustrous like wax. Acid-insoluble Ash Not more than 1. The rhizome without cork layer is dark yellowish red and powdery. of Curcuma longa Linné (Zingiberaceae). Secondary rhizome is cylindrical with two obtuse ends. 0%. flat cylindrical. 1 mL of silicon resin). numerous vascular bundles are scattered as spots or lines. cylindrical. Purity Foreign matter – Cynomorium Herb contains less than 5. Texture is weak and easy to be broken and powdery. Texture is hard and uneasily broken. Fractured surface is reddiwh brown. ethyl acetate and acetic anhydride (92 : 5 : 5) to a distance of about 10 cm and air-dry the plate.0 g.5%. 1 cm to 2 cm in diameter and 2 mm to 5 mm in thickness. with remains of stem at one end. 15 mm to 25 mm in length and 5 mm to 10 mm in diameter. Dissolve each of the residues to 0. Dictamnus Root Bark has characteristic odor and slightly bitter taste.3 mL (50. frequently and small protruding granular dots. Loss on Drying not more than 10.5 mL of ethyl acetate and use these solution as the test solution and the standard solution of Cyperus Rhizome RMPM. occasionally white and powdery. The several spots from the test solution and the spots from the standard solution of Cyperus Rhizome RMPM show the same color and the same Rf value. Parenchyma cell has starch grains. Ash Not more than 3. heat in a water bath for 3 minutes and filter. Perform the test with the test solution and the standard solution of of Cyperus Rhizome RMPM as directed under the Thin-layer Chromatography. with slightly thin lower part. respectively. a transverse section reveals fiber bundles as brown spots lined in rings along circumference. . vascular bundles appear as red-brown spots and numerous secretary cells are scattered as minute yellow-brown spots. Under a microscope. The transverse section is red-brown to pale yellow. 5 cm to 15 cm in length. Deve1op the plate with a mixture of toluene. Eavaporate the filterates to dryness. Description Cyperus Rhizome is fusiform rhizome. sometimes with remains of triangular. clusters of calcium oxalate and oil drops. with waxy luster.0% Identification Weigh 1 g each of pulverized Cyperus Rhizome and Cyperus Rhizome RMPM.5 g of pulverized Dictamnus Root Bark. somewhat lamellar. Description Dictamnus Root Bark is the root bark. Here and there in the cortex. and when outer layer is peeled off. Examine the plate under ultraviolet light (wavelength: 254 nm). from which flower stalk has been removed.0% of flower stalk and the other foreign matters. Cynomorium Herb has slightly odor and slightly bitter and astringent taste. Cell wall is very thick and lignified in stone cell-shape. Part II Cynomorium Herb Cynomorii Herba Cynomorium Herb is the stem of Cynomorium songaricum Ruprecht (Cynomoriaceae). Description Cynomorium Herb is the stem. add 5 mL of ether. Fracture is uneven.0% Extract Content Dilute ethanol–soluble extract— Not less than 25. dark brown scales. Add 1 to 2 drops of Mayer TS to 5 mL of the filtrate: a yellowish white precipitate is produced. Cyperus Rhizome has characteristic odor and taste. Identification Weigh 0. slightly curved. The thickness of cortex is approximately equal to or slightly smaller than the diameter of stele. Stele is powdery and its color turns pale. with 5 to 8 irregular ring nodes and with hair-like fiber bundles on each node. shake for 1 hour and filter. with distinct longitudinal furrows and irregular pits. In the stele. longitudinally wrinkled. The fiber is long polygon or quadrilateral. Under a magnifying glass. External surface is grayish brown to grayish blackish brown. 2 cm to 5 cm in diameter. from which rootlets have been removed. External surface is grayish white or grayish yellow. External surface is reddish brown to deep brown.1028 Monographs. Ash not more than 8. Inner surface is almost pale yellow. Spot 5 μL each of the test solution and the standard solution of Cyperus Rhizome RMPM on a plate with fluorescent indicator for thin-layer chromatography. Acid-insoluble Ash Not more than 1. coarse. transverse section reveal fibers singly scattered in cortex and phloem. numerous glittering small spots are observed on exposing to light.0% Dictamnus Root Bark Dictamni Cortex Cyperus Rhizome Dictamnus Root Bark is the root bark of Dictamnus dasycarpus Turczaininov (Rutaceae). add 10 mL of diuted acetic acid. with rootlet scars. 5 cm to 20 cm in length. Texture is hard. Essential Oil Content Not less than 0. Cyperi Rhizoma Cyperus Rhizome is the rhizome of Cyperus rotundus Linné (Cyperaceae). distance of about 10 cm and air-dry the plate. Dolichos Seed Dioscorea Rhizome Dioscoreae Rhizoma Dioscorea Rhizome is the rhizome or the dried steamed rhizome (rhizophore) of Dioscorea japonica Thunberg or Dioscorea baratas Decaisne (Dioscoreaceae). add 2 mL of chloroform. and is soft like fur.The burnt one is reddish brown or dark brown.0% of the xylem tissue and other foreign matter. To the each residue. the upper surface and both side are marked by raised of depressed circular frond scar. 5 cm to 15 cm in length. Spot 10 μL each of the test solution and Dioscorea Rhizome RMPM standard solution on a plate of silica gel for thin-layer chromatography. To the filtrate.0%. mostly curved. flattendellipsoidal or flatten-ovoid. add 50 mL of ethanol and 5 mL of acetic acid. Ash Not more than 6. smooth.5%.5 g of pulverized Dioscorea Rhizome. External surface is milky white to yellowish white.0% (6 hours). Extract Content Dilute ethanol-soluble extract— Not less than 14. add 2 mL of ethanol and use each solution as the test solution or Dioscorea Rhizome RMPM standard solution. warm on a water-bath for 2 to 3 minutes and filter. Fractured surface is milky white. add 10 mL of water. .0%. lustrous. Extract Content than 14. and 2 mm to 5 mm in thickness. and 4 mm to 7 mm in thickness. Loss on Drying Not more than 12.0%. rarely by remains of frond-bases and fibrous roots. transverse section reveals vascular bundles rarely scattered. (2) Weigh 0. Perform the test with the test solution and Dioscorea Rhizome RMPM standard solution as directed under the Thin-layer Chromatography. cylindrical or irregular cylindrical. Spray evenly diluted sulfuric acid TS and heat at 105 o C for 10 minutes: the spots from the test solution and the spots from Dioscorea Rhizome RMPM standard solution show the same colors and the same Rf values Loss on Drying Not more than 14. 8 mm to 12 mm in length. Dolichos Seed has characteristic odor and taste is weak and bean-like on chewing. Description Dolichos Seed is the seed. Acid-insoluble Ash Not more than 0. Description Drynaria Rhizome is the rhizome. add 1 drop of dilute iodine TS: a blue color develops. Texture is hard. To the filtrate.0%. occasionally longitudinally split or transversely cut.0%.KP VIII 1029 Purity Xylem⎯ Dictamnus Root Bark contains not more than 5. 6 mm to 9 mm in diameter. with mucilage cell and starch grains in parenchyma tissue. External surface is yellowish white.5 mL of acetic anhydride. Loss on Drying Not more than 12. smooth and powdery. Under a microscope. from which the scaly pieces (ramenta) have been burned off. Identification (1) Weigh 0. Water-soluble extract—Not less Drynaria Rhizome Drynaria Rhizoma Drynaria Rhizome is the rhizome of Drynaria foutunei J. External surface is closely covered with deep brown to dark brown hairy ramenta. Testa is thin and brittle. Ash Not more than 8. flattened cylindrical. (3) Weigh 1 g each of pulverized Dioscorea Rhizome or Dioscorea Rhizome RMPM. add 0. shake well and add 0. yellowish white cotyledons inside. heat under a reflux condensor for 30 minutes. eyebrow-shaped caruncle at the edge of one side. Dioscorea Rhizome is nearly odorless and tasteless. with 2 plump. with a white. heat carefully for about 5 minutes and filter.0%. 10 mm to 15 mm in width.5 g of pulverized Dioscorea Rhizome.0%.5 mL of sulfuric acid carefully to make two layers: a pale red to reddish brown color appears at the zone of contact and bluish green to green color at upper layer. Description Dioscorea Rhizome is the rhizome. 5 cm to l5 cm in length and 10 mm to 40 mm in diameter. The texture is hard and breakable. Smith (Polyodiaceae). branched.0%. Develop the plate with a mixture of cyclohexane and ethyl acetate (3 : 1) to a Dolichoris Semen Dolichos Seed is the ripe seed of Dolichos lablab Linné (Leguminosa). . Acid-insoluble Ash Not more than 1. filter and evaporate on a water-bath to dryness. Texture is light. Acid-insoluble Ash Not more than 1. prominent.0%. Ash Not more than 5. (2) Foreign matter—Ephedra Herb does not contain stems of Equisetaceae or Gramineae plants. A. contains not less than 0. To the residue. thin cylindrical to ellipsoidally cylindrical. Perform the test with the test solution and the standard solution as directed under the Thin-layer Chromatography. Under a magnifying glass. when dried. water and acetic anhydride (7 : 2 : 1) to a distance of about 10 cm and air-dry the plate.819 AS 10 Operating conditions Detector: An ultraviolet absorption photometer (wavelength: 210 nm). Develop the plate with the upper layer of the mixture of ethylacetate. Determine the peak areas. Ephedra intermedia Schrenk et C. packed with octadecylsilyl silica gel for liquid chromatography (5 μm to 10 μm in particle diameter). filter and use the filtrate as the test solution. Separately. Assay Weigh accurately about 0. of ephedrine in the standard solution. Pipet 2. Ephedra Herb has slight odor and astringent and slightly bitter taste and paralyzes slightly sensation on the tongue. water.7% of total alkaloids [as ephedrine (C10H15NO: 165. Perform the test with the test solution as directed under the Thinlayer Chromatography. AS. 4 mm to 6 mm in inside diameter and 15 cm to 25 cm in length. Part II fragile and easily broken. formic acid and benzene (12 : 3 : 2. add 1 mL of methanol and use this solution as the test solution. the transverse section of the stem appears as circle and ellipse. ATE and ATF. usually being opposite at every node. Amount (mg) of total alkaloids = amount (mg) of Ephedrine Hydrochlor ide RS × A TE + A TF 1 × × 0 . Develop the plate with a mixture of n-butanol.5 g of pulverized Drynaria Rhizome. the outer volume grayish green to yellow-green and the center filled with a redpurple substance or hollow. Ash Not more than 11. Numerous parallel vertical furrows are on the surface. filter and evaporate the filtrate. Fracture is reddish brown.0%. Acid-insoluble Ash Not more than 2.9). Drynaria Rhizome has slight characteristic odor and weak and slight astringent taste.5 g of pulverized Ephedra Herb. add 20 mL of diluted methanol (1 in 2). Separately. pale brown to brown. Around the fractured surface is fibrous and easily split vertically. Repeat this procedure twice with the residue using 20 mL volumes of diluted methanol (l in 2). respectively.23)].0%.23) and as pseudoephedrine (C10H15NO: 165.0%. Ephedra Herb.1030 Monographs. adhering at the base to form a tubular sheath around the stem. Spot 5 μL each of the test solution and the standard solution on a plate of silica gel with fluorescent indicator for thin-layer chromatography. Column: A stainless steel column. dissolve 5 mg of Naringin RS in l mL of methanol and use this solution as the standard solution. sonicate. add diluted methanol (1 in 2) to make exactly 100 mL and use this solution as the standard solution. centrifuge and separate the supernatant liquid. Purity (1) Woody stem—Less than 5. Spray evenly the plate with 2% ninhydrin-ethanol solution and heat at 105 o C for 10 minutes: spot of the Rf value about 0.35 is reddish purple. previously dried in a desiccator (silica gel) for 24 hours. or any other foreign matter. Description Ephedra Herb is the terrestrial stem. 5 cm to 25 cm in length. previously dried at 105 o C for 3 hours and dissolve in diluted methanol (1 in 2) to make exactly 20 mL. add 30 mL of methanol. The leaves are 2 to 4 mm in length. Spray with 1% Aluminium chloride TS in ethanol on the plate and examine under ultraviolet light at (main wavelength: 365 nm): a spot from the test solution and a spot from the standard solution show the same color and the same Rf value. weigh accurately about 50 mg of Ephedrine Hydrochloride RS. shake for 30 minutes. Ephedra Herb is pale green to yellowish green.5 g of pulverized Ephedra Herb. of ephedrine and pseudoephedrine (the relative retention time to ephedrine is about 0. Meyer or Ephedra equisetina Bunge (Ephedraceae). add diluted methanol (1 in 2) to make exactly 100 mL and use this solution as the test solution. in the test solution and the peak area. Ephedra Herb Ephedrae Herba Ephedra Herb is the terrestrial stem of Ephedra sinica Stapf. Identification Weigh 0. Scaly leaves are at the node volume. add 10 mL of methanol. 1 mm to 2 mm in diameter and 3 cm to 5 cm in length of internode. Spot 10 μL of the test solution on a plate of silica gel for thin-layer chromatography. Column temperature: A constant temperature of about 45 °C. Combine all the extracts. shake for 2 minutes.5 : 1) to a distance of about 12 cm and air-dry the plate.0 mL of the solution. Mobile phase: A mixture of a solution of sodium lauryl sulfate (1 in 128). Identification Weigh 0. with vascular bundles yellow dotted and arranged in a ring. Perform the test with 10 μL each of the test solution and the standard solution as directed under the Liquid Chromatography according to the following operating conditions. acetonitrile and phosphoric acid . in a glass-stoppered centrifuge tube. Assay Weigh accurately about 1 g of pulverized Epimedium Herb. Acid-insoluble Ash Not more than 1. pale yellowish brown to slightly purplish and greenish brown. and perform the test as directed under the Liquid Chromatography according to the following operating conditions. The base of leaflet is cordate to deeply cordate. Description Epimedium Herb is composed of a stem and a ternate to triternate compound leaf. mesophyll composed of upper epidermis. dissolve each in diluted methanol (l in 2) to make 100 mL. the relative standard deviation of the peak area of ephedrine is not more than 1. Epimedium Herb Epimedii Herba Epimedium Herb is the aerial part of Epimedium koreanum Nakai. System suitability System performance: When the test is repeated . Under a microscope. packed with octadecylsilyl silica gel for liquid chromatography (5 μm to 10 μm in particle diameter). cortex of 4 to 10 layers of sclerenchymatous cells. weigh accurately 10. pilose with distinct vein. Loss on Drying Not more than 12. weigh1 mg of Icariin RS. clearly dividing each peak. of the test solution and of the standard solution. Epimedium pubescens Maximowicz. single-layered palisade. Develop the plate with a mixture of ethylacetate. and water (8 : 2 : 1) to a distance of about 10 cm and air-dry the plate. a transverse section of the leaf reveals 3 to 6 vascular bundles in midvein. add 40 mL of 70 % solution of ethanol and proceed in the same manner. and the lateral leaflet is asymmetry.2 cm in length. add 50 mL of 70 % solution of ethanol under a reflux condenser for 1 hour and filter. add 70 % solution of ethanol to make exactly 100 ml and use this solution as the test solution. System repeatability: When the test is repeated 6 times with the standard solution under the above operating conditions. 2 cm to 8 cm in width. ethanol. vascular bundle 13 to 30 in number.5%. To the residue. add 70 % solution of ethanol to make exactly 20 mL. and use this solution as the standard solution.0 % (6 hours). Under a microscope. Epimedium Herb (Berberidaceae). Determine the peak areas.1 cm to 0. Extract Content Dilute ethanol-soluble extract— Not less than 15. Epimedium wushanense T. Epimedium Herb has slightly odor and slightly bitter taste. easily broken. add 20 mL of methano1. and the inner surface is pale green to pale gray-greenish brown. When the procedure is run with 10 μL of this solution under the above operating conditions. ephedrine and atropine are eluted in this order. globular to ovoid. spongy tissue and lower epidermis. The leaflet is ovoid to broadly ovoid or ovoid-lanceolate.0 %. add in 1 mL of methanol and use this solution as the standard solution. respectively. The petiole and stem is cylindrical. a transverse section of the stem reveals a single to several-layered hypodermis. The apex of leaflet is acuminate with needle hair on margin. or Epimedium sagittatum Maximowicz. Column: A stainless column. Column temperature: a room temperature. Amount (mg) of icariin (C33H40O15) A 1 = amount (mg) of Icariin RS × T × AS 4 Operating conditions Detector: An ultraviolet absorption photometer (wavelength: 214 nm). Examine under ultraviolet light (main wavelength: 254 nm): one spot among the spots from the test solution and a dark reddish spot from the standard solution show the same color and the same Rf value. Pipet 10 μL each of the test solution and the standard solution. and the petiolule is 15 mm to 70 mm in length. Combine the filtrates. System suitability System performance: Weigh l mg of Ephedrine Hydrochloride RS and 4 mg of Atropine Sulfate RS. sclerenchymatous.3% of icariin (C33H40O15: 676. Epimedium Herb contains not less than 0. shake for 15 minutes to mix. Herb. Take exactly 5 ml of this solution. Epimedium brevicornum Maximowicz. Ying.0%.KP VIII 1031 (640 : 360 : 1). and add methanol to make exactly 100 mL. filter and use the filtrate as the test solution. Mobile phase: a mixture of acetonitrile and water (28 : 72) Flow rate: 1. Separately. sometimes lustrous. 4 mm to 6 mm in inside diameter and 15 cm to 25 cm in length. Identification Weigh 2 g of pulverized Epimedium Ash Not more than 8. The leaf margin is globular to orbicular. 3 cm to 20 cm in length.66). Spot 10 μL each of the test solution and the standard solution on a plate of silica gel with fluorescent indicator for thin-layer chromatography. Epimedium Herb has 8 to 20 vascular bundles in petiole and 6 to 15 vascular bundles in petiolule.0 mg of icariin RS. The multicellular hair is on epidermis. calculated on the basis of the dried material. Flow rate: Adjust the flow rate so that the retention time of ephedrine is about 14 minutes. Separately. S. AT and AS. and papery or coriaceous. 0.0 mL/min. Perform the test with the test solution and the standard solution as directed under the Thin-layer Chromatography. The outer surface is green to greenish brown.0 %. Texture is fragile and easily broken. Mesophyll appears the solitary and clustered crystals. curved. varying in size. from which periderm is removed. Loss on Drying Not more than 14. oblong to obovate. Add 0. sparsely scattered large cells without chloroplast.0%. weigh 5 mg of Ursolic Acid RS. Ash Not more than 8. Develop the plate with a mixture of n-hexane and ethyl acetate (1 : 1) to a distance of about 10 cm and air-dry the plate. Acid-insoluble Ash Not more than 6. Eribotrya Leaf Eriobotryae Folium Eriobotrya Leaf is the leaf of Eriobotrya japonica Lindley (Rosaceae). with distinct longitudinal wrinkles and lenticels. Ash Not more than 2. Midrib appears the vascular bundle collateral. shake for 2 to 3 minutes and filter. The unbroken Euryale Seed is 5 mm to 8 cm in diameter.5 mL of lead subacetate TS to 2 mL of the filtrate: pale yellowish brown precipitation is produced. stone cells and fiber layer in the phloem. Tomentum is unicellular. and medullary ray consisting of 2 to 3 rows of cells. 12 cm to 30 cm in length and 4 cm to 9 cm in width. Lichen is sometimes attached to Eucommia Bark. The inner surface is smooth. with yellowish brown tomentose. 4 to 5 layers of palisade tissue. Loss on Drying Not more than 10. Spray evenly the plate with sulfuric acid TS for spray and heat at 105 o C for 10 minutes: one of the spots from the test solution and the spot from the standard solution are the same color and the Rf value. around one third of whole. Lower surface is pale colored and densely yellow tomentose. formig interrupted ring and pericycle fibre bundles arranged in phloem. Eriobotrya Leaf has rarely odor and slightly bitter taste. Eucommia Bark Eucommiae Cortex Eucommia Bark is the stem bark of Eucommia ulmoides Oliver (Eucommiaceae). sometimes reddish brown. Upper part of small vescular bundle has lignified tissue. with two edges curved inwards. surrounded by solitary crystal of calium oxalate. Perform the test with the test solution and the standard solution as directed under the Thin-layer Chromatography.3 g of pulverized Eriobotrya Leaf. Description Eriobotrya Leaf is the leaf. with fine wrinkeld longitudinally.5 mm in length. silvery and elastic rubber threads.0%. brown or dark brown.5 g of pulverized Eriobotrya Leaf.0%. heat for 5 minutes in a water-bath. Upper surface is graeyish brown. Description Eucommia Bark is the stem bark. Loss on Drying Not more than 15.5%.0%. Extract Content Dilute ethanol-soluble extract— Not less than 9. transverse section reveals thin cuticle. add 10 mL of water. and smooth. External surface is pale grayish brown to grayish brown. often cut.0%. margin is sparsely serrate and entire is near base. Identification (1) Weigh 0. Fracture surface is white and powdery. Separately. Ash Not more than 10. yellowish brown to greenigh brown.0%. Part II six times with 10 μL of the standard solution under the above operating conditions: the relative standard deviation of the peak area of icariin is not more than 1. filter and use the filtrate as the test solution. Petiols is very short. and 3 mm to 7 mm in thickness. flattened. Purity Foreign matter—The amount of cortex and other foreign matter contained in Euryale Seed is not more than 2. Eucommia Bark has charateristic odor and slightly bitter taste. Euryale Seed is odorless and has weak taste.0% (6 hours).1032 Monographs. lustrous. Extract Content Dilute ethanol-soluble extract— Not less than 15. transverse section reveal the paranchyma cells containing rubber mass in the paranchyma tissue. add 10 mL of methanol. Under a microscope. dense. (2) Weigh 0. Euryale Seed Euryales Semen Euryale Seed is the ripe seed of Euryale ferox Salisbury (Nymphaeaceae).0%. Fracture is linked up by fine. Under a microscope. curved into the xylem tissue.0%. Spot 10 μL each of the test solution and the standard solution on a plate of silica gel for thin-layer chromatography. External surface has a reddish brown cortex and the other end is yellowish white. . cool. dissolve it in 5 mL of methanol and use this solution as standard solution. Description Euryale Seed is the round seed. 25 μm in thickness and about 1.0%. Apex is acute. dissolve to make exactly 50 mL of methanol.0%. respectively. Flow rate: 1.0%. Determine the peak areas. Mobile phase: A mixture of acetonitrile and water (50:50). cool and filter. Evaporate the filtrate to dryness. To residue. External surface is dark brown to grayish brown. . and perform the test as directed under the Liquid Chromatography according to the following operating conditions. Use a column giving elution of evodiamine and rutecarpin in this order and clearly dividing each peak. heat for 5 minutes in water-bath. 2. spray Dragendorff's TS for spraying and allow to stand: a yellow-red color develops.5 mm to 5 mm in diameter. Matured pericarp is split to reveal five loculi and each loculus containing obovoid or globular seeds of a lustrous brown to blackish brown or bluish black. add 20 mL of methanol. Amount (mg) of evodiamine (C 19H21N3O) = amount (mg) of Evodiamine RS × ATE 1 × ATR 10 Amount (mg) of rutecarpin (C 18H13N3O) = amount (mg) of Rutecarpin RS × ASE ASR × 1 10 Operating conditions Detector: An ultraviolet absorption photometer (wavelength: 254 nm). cool and filter. Seperately. respectively. heat for 5 minutes on a water-bath. spheroidal or globular fruit. add exactly 20 mL of methanol and use this solution as the standard solution. Separately.5%. (ii) Take 0. packed with octadecylsilyl silica gel for liquid chromatography (5 to 10 μm in particle diameter). add 20 mL of methanol and proceed in the same manner. ASE and ASR.1% of a mixture of the contents of evodiamine (C19H21N3O: 307. Spray evenly dilute sulfuric acid TS on the plate and examine under ultraviolet light (main wavelength: 365 nm): two spot among the several spots from the test solution and the spot from the standard solution (1) and the standard solution (2) show the same color Purity (1) Peduncle—Less than 5. dissolve in 1 mL of methanol and use these solutions as the standard solution (1) and the standard solution (2). Perform the test with the test solution as directed under the Thin-layer Chromatography. sonicate for 1 hour and filter. 2 mm to 5 mm in length. add methanol to make exactly 50 mL and use this solution as the test solution. Assay Weigh accurately about 0. covered densely with hairs. with many oil sacs appearing as hollow pits and often with peduncle. To this solution. ATE and ATR. Under a microscope.2 mL of the test solution and add 0. Pipet 10 μL each of the test solution and the standard solution. Description Evodia Fruit is flattened. Develop the plate with a mixture of hexane and ethyl acetate (3 : 2) to a distance of about 10 cm and air-dry the plate. System suitability System performance: Proceed with 10 μL of the standard solution under the above operating conditions. add gently 2 mL of p-dimethylaminobenzaldehyde TS and warm on a water-bath: a purple-brown ring develops at the zone of contact.39) and rutecarpin (C18H13 N3O: 287. a transverse section reveals hard hairs of epidermis of epicarp. Evodia fruit contains not less than 0.8 mL of dilute acetic acid. Spot 20 μL each of the test solution and the standard solution on a plate of silica gel with a fluorescent indicator for thin-layer chromatography. bodinieri Huang (Rutaceae). (i) Spot one drop of the test solution on a filter paper. Ash Not more than 8.5 g of the fine powder of Evodia Fruit.0%.32). add 3 mL of dilute acetic acid to the residue. 4 to 6 mm in inside diameter and 15 to 25 cm in length. weigh 1 mg of evodiamine RS and 1 mg of rutecarpin RS. add 25 mL of methanol. Combine all the filtrates. Column temperature: An ordinary temperature. of the test solution and. warm for 2 minutes on a water-bath. Take exactly 2 mL of this solution. of the standard solution. Perform the following tests using the filtrate as the test solution. Evodia Fruit has characteristic odor and purgent taste followed by lasting bitterness taste.0 mL/min. air-dry. officinalis Huang or Evodia rutaecarpa Bentham var. add 20 mL of methanol. Evodia rutaecarpa Bentham var. weigh accurately 10 mg of evodiamine RS and 10 mg of rutecarpin RS. Evodia Fruit Evodiae Fructus Evodia Fruit is the fruit of Evodia rutaecarpa Bentham.KP VIII 1033 and the same Rf value. filter after cooling and use the filtrate as the test solution. (2) Weigh 1 g of pulverized Evodia Fruit. Identification (1) Weigh 1 g of pulverized Evodia Fruit. Column: A stainless column. System repeatability: When the test is repeated six times with 10 μL of the standard solution under the above operating conditions: the relative standard deviation of the peak area of evodiamine and rutecarpin is not more than 1. (2) Foreign matter—The amount of foreign matter other than peduncles contained in Evodia Fruit is not more than 1. add gently 0. Ash Not more than 5. Texture is hard. Description Forsythia Fruit is ovoid to long ovoid capsule fruit. Extract Content Dilute ethanol-soluble extract— Not less than 18. Nogyo—Nogyo is dehiscent from apex or to two segments. and inner surface is yellowish brown and smooth. One large oil canal is present between each ridge and two oil canals are on the ventral side. The outer surface is covered with numerous scaly bracts. External surface is grayish yellow-green to grayish yellow. externally greenish brown.0%. Two mericarps are closely attached with each other and with five longitudinal ridges. with acute apex and sometimes with a peduncle at the base. Identification (1) Weigh 0. a transverse section reveals ridges near the ventral side are far protruded than those on the dorsal side.5 mL of sulfuric acid to form two layers: a red-purple color develops at the zone of contact.0 g). a transverse section reveals spherical pollen grains. Under a microscope. 3 mm to 8 mm in length. Description Farfarae Flower is the flower bud. allow to stand for 2 minutes and filter. To l mL of the filtrate. RMPM. add 10 mL of hexane.0%. Essential Oil Content Not less than 0. scattered with pale gray and small ridged dots and with two longitudinal furrows. 10 mm to 25 mm in length and 5 mm to 10 mm in diameter.7 mL (50. Forsythia Fruit has slightly characteristic odor and bitter taste. with a longitudinal septum. steamed and dried is called Chunggyo. Ash Not more than 10. 1 mm to 3 mm in width and occasionally with 2 mm to 10 mm of a fruit stalk. Part II Farfarae Flower Farfarae Flos Farfarae Flower is the flower bud of Tussilago farfara Linné (Compositae). yellowish green. Perform the test with this as directed under the Thin-layer Chromatography. Fennel Foeniculi Fructus Fennel is the well ripe fruit of Foeniculum vulgare Miller (Umbelliferae). clavate.0%. solitary or 2 to 3 accreted at the base. 15 to 25 mm in length and 5 to 10 mm in width. the rectangle epidermis of calyx. The outer side of bracts is purplish red or pale red. Description Fennel is cylindrical cremocarp fruit. shake well. (2) Foreign matter—The amount of foreign matter other than the fruit stalk is not more than 1. showing white hairs after riping. Chunggyo—Chunggyo is mostly indehiscent. followed by bitterness. add l0 . Exteranl surface is yellowish brown to reddish brown. Fennel has characteristic odor and sweet taste at first. allow to stand for 5 minutes. mostly fallen off.0%. The body is light. Develop the plate with a mixture of hexane and ethyl acetate (20 : l) to a distance of about 10 cm and air-dry the plate. with less small grayish white maculates. Acid-insoluble Ash Not more than 1. The upper part is broader and the lower part is gradually slender or blunt.5%. slender and winged at one side. and the inner side is densely covered with white flocky hairs.2 g of pulverized Forsythia Fruit. Seeds are numerous. shake well.1034 Monographs. Farfarae Flower is aromatic and taste is slightly bitter and pungent. Under a microscope.5 g each of pulverized Fennel and Fennel RMPM.0% of residual pedicels and foreign matter. External surface is pale brown to dark brown. filter and use the filtrates as the test solution and the standard solution of Fennel Forsythia Fruit Forsythiae Fructus Forsythia Fruit is the fruit of Forsythia virdissima Lindley or Forsythia suspensa Vahl (Oleaceae). Loss on Drying Not more than 8. Texture is brittle and seeds are brown. The greenish fruit collected when it is beginning to ripen. Spot 5 μL each of the test solution and the standard solution of Fennel RMPM on a plate of silica gel with a fluorescent indicator for thinlayer chromatography. long. Purity Foreign matter—Farfarae Flower contains less than 2. The fruit collected when it is ripened perfectly is called Nogyo. Identification Weigh 0. Examine under ultraviolet light (main wavelength: 254 nm): the several spots from the test solution and the spots from the standard solution of Fennel RMPM show the same color and the same Rf value.5%. and thickend cell wall in subsequently strung beads. add 2 mL of acetic anhydride. Acid-insoluble Ash Not more than 1. (2) Weigh l g of pulverized Forsythia Fruit.0%.0%. Purity (1) Fruit stalk —The amount of fruit stalk is not more than 3. Add 1 drop of Mayer TS carefully to 2 mL of the filtrate: the solution becomes turbid. 3 mm to 8 mm in height.1 g of magnesium and l mL of hydrochloric acid and allow to stand: a pale red to yellow-red color develops. The fractured surface is powdery-white. Texture is hard and brittle. regardless of the size.0%. and the fractured surface is white and starchy. (3) Julpaipyon—Jupaipyon is bulb. warm for 5 minutes on a water-bath with occasional shaking. add 10 mL of dilute acetic anhydride. and slices cut from the outer single scale leaf of a bulb. (2) Jupai—Jupai is whole bulb. shake for 5 minutes and filter.KP VIII 1035 mL of methanol. highly starchy. the smaller one. Don. Hsia. cool and filter. add 3 mL of dilute hydrochloride to the re- Ash Not more than 5. highly starchy. (2) Weigh 0. Fritillaria prezewalskii Maximowicz or Fritillaria delavayi Franchet (Liliaceae). outer surface is milky white to pale yellow. The apex is closed. Loss on Drying Not more than 15.5 g of Fritillaria Bulb. plump and fleshy.5 g of Fritillaria Bulb. with subcylinderical and slightly tapering buds and 1 to 2 scales inside. 4 mm to 11 mm in height and 4 mm to 16 mm in diameter. The bulb with central bud removed. Fritillaria unibracteata Hsiao et K. Add 1 to 2 droplets of Mayer TS carefully to 2 mL of the filtrate: the solution becomes turbid. (2) Chungpai—Chungpai is slightly oblate bulb. (2) Foreign matter—The amount of foreign matter other than branchlets contained in Forsythia Fruit is not more than 1. Outer surface is white.0%.0%. with the large scale closely embracing the small one.5 g of Fritillaria Thunbergii Bulb. Add 1 mL of sulfuric acid carefully to 2 mL of the filtrate: a red color develops at the zone of contact. Externally the outer scale leaves are two. . Texture is hard and fragile. add 10 mL of dilute acetic acid. Let stand for a while: the upper layer shows green. Fritillaria Bulb Bulbus Fritillariae Cirrhosae Fritillaria Bulb is the bulb of Fritillaria cirrhosa D. The apex is open with buds. To 5 mL of the filtrate. easily broken. (3) Weigh 2 g of Fritillaria Bulb. embraced. covered with white powder. with the central bud not removed. Description (1) Daipai—Daipai is bulb and the outer single scale leaf of a bulb. airdry and spray Dragendorff’s TS: a yellowish red color is produced. Ash Not more than 5. 3 mm to 8 mm in diameter. (2) Weigh 0. containing 2 to 3 small scale leaves and dried shrunken stem remains.0%. Songpai is odorless and slightly pungent taste. cut surface even. Extract Content Dilute ethanol-soluble extract— Not less than 9. shake for 5 minutes and filter. Outer scale leaves are two.5 g of Fritillaria Thunbergii Bulb. External surface is white. cool and filter. Drop one drop of this filtrate on the filter paper. Identification (1) Weigh 0. and oblate. add 5 mL of acetic anhydride. Occasionally the remains of fibrous roots are found.0%. almost uniform in size. varying considerably in size. sidual. 1 cm to 2 cm in diameter. almost in reniform holding to each other. 1 to 2 small scales inside and slender cylindrical remains of a stem. Purity (1) Branchlet—Less than 5. 1 cm to 2 cm in height and 20 mm to 35 mm in diameter. is commonly known as Jupai. shake for 5 minutes and filter. Description (1) Songpai—Songpai is conical to fu`siform bulb. 10 mm to 15 mm in height and 10 mm to 25 mm in diameter. even and slightly pointed with a grayish brown disk at central part. C. cut into thick slice freshly is called Julpaipyon. shake for 5 minutes and filter.0%. add 0. Let stand for a while: the upper layer shows green. powdery-white. Extract Content Dilute ethanol-soluble extract— Not less than 10. warm for 2 minutes in a water bath. the outer scale leaves 2. Texture is hard and fragile. almost in crescent shape. The surface of edge is pale yellow. Add 1 mL of sulfuric acid carefully to 2 mL of the filtrate: a red color develops at the zone of contact. add 5 mL of acetic anhydride. Let stand for a while: a white precipitate is produced. inner surface is white or pale brown. Daipai has slightly characteristic odor and a slightly bitter taste. Evaporate all the filtrate to dryness. warm in a water-bath for 2 minutes and filter. add 20 mL of methanol. Fritillaria Thunbergii Bulb Fritillariae Thunbergii Bulbus Fritillaria Thunbergii Bulb is the bulb of Fritillaria thunbergii Miquel (Liliaceae) and other species of the same genus. Fritillaria Bulb is divided by figures. Songpai or Chunhpai.0%. fracture surface is white to yellowish white. The base is globular. Let stand for a while: a white precipitate is produced. Identification (1) Weigh 0. elliptical or subrounded. the uncovered part appearing crescent. The larger one is removed from the central bud and commonly known as Daepai. Spot 20 μL each of the test solution and the standard solution on a plate of silica gel for thin-layer chromatography. Atractylodes Rhizome White. extract with a reflux condenser for 1 hour and filter. Perform the test with the test solution and the standard solution as directed under the Thin-layer Chromatography.1036 Monographs. 2. Ash Not more than 6.Pulverize Gamisoyosan Extract Granuels. Gamisoyosan Extract Granules Gamisoyosan Extract Granules contains not less than 3. Mentha Herb 0. Vacuum-concentrate the filtrate until the filtrate becomes 10 mL and use this solution as the standard solution. add 10 mL of water.0%. Extract Content Dilute ethanol-soluble extract— Not less than 9. Develop the plate with a mixture of toluene. extract with a reflux condenser for 1 hour and filter. warm for 5 minutes on a water-bath with occasional shaking. Spot 20 μL each of the test solution and the standard solution on a plate of silica gel for thin-layer chromatography.0%. Vacuum-concentrate the filtrate until the filtrate becomes 10 mL and use this solution as the test solution. Inside of the mass is pale brown.46) in Peony Root and Moutan Root Bark. weigh equivalent to 1 g of Angelica Gigas Root. Identification (1) Weigh 0. add 20 mL of methanol. Gambir Gambir is the dried aqueous extract prepared from the leaves and young twigs of Uncaria gambir Roxburgh (Rubiaceae). Bupleurum Root. and 8. Gambir has slight odor and extremely astringent and bitter taste. shake for 5 minutes. Gamisoyosan Extract Granules is prepared as directed under Granules. warm for 2 minutes in a water-bath. Ash Not more than 5. Vacuumconcentrate the filtrate until the filtrate becomes 10 mL and use this solution as the test solution.64 g to 2. put into the extractor. Moutan Root Bark. add eight to ten fold of water. Vacuum-concentrate the filtrate under 60 o C until it becomes 1. add 3 mL of dilute hydrochloride to the residual. add 100 mL of methanol. Part II (3) Weigh 2 g of Fritillaria Thunbergii Bulb.36 g of Dry extract. extract for 2 to 3 hours at 80 o ~ 100 C and filter. add 100 mL of methanol.67 g Ginger.Pulverize Gamisoyosan Extract Granules.3 mg of total paeoniflorin (C23H28O11: 480. Peony Root 1. weigh 1 g of Atractylodes Rhizome White.0%. extract with a reflux condenser for 1 hour and filter. weigh 1 g of Angelica Gagas Root. weigh each crude drugs.33 g Pulverize the above crude drugs to coarse powder. dissolve with 20 mL of dilute ethanol for 2 minutes and filter. Acid-insoluble Ash Not more than 1.91 g to 1. (2) Weigh 0. (2) Atractylodes Rhizome White . Identification (1) Angelica Gigas Root . Mix l mL of the filtrate with 9 mL of dilute ethanol and to this solution.45 g of Viscous extract or concentrate in a suitable method until it becomes 0. add 100 mL of methanol. cool and filter. Develop the plate with a mixture of hexane and acetone (7 : 1) to a distance of about 10 cm and air-dry the plate. cool and filter. add 10 mL of water. Drop one drop of this filtrate on the filter paper. airdry and spray Dragendorff’s TS: a yellow-red color is produced.0%.6 mg of glycyrrhizic acid (C42H62 O16: 822. weigh equivalent to 1 g of Atractylodes Rhizome White. warm in a water-bath for 5 minutes with occasional shaking and filter. extract with a reflux condenser for 1 hour and filter. Perform the test with the test solution and the standard solution as directed under the Thinlayer Chromatography.37) in Gardenia Fruit for a dose (one sachet). Separately. water and acetic acid (500 : 500 : 5 : 2) to a distance of about 10 cm and air-dry the plate. Description Gambir is the aqueous extract from the leaves and young twigs.0%.2 g of pulverized Gambir.5%. Poria.00 g Licorice. add 100 mL of methanol. add 10 mL of water. Separately. Spray evenly the plate with the solution made by dissolving 5 g of pdimethylaminobenzaldehyde in 100 mL of 10% sulfuric acid and heat at 105 o C for 10 minutes: one spot among the spots from the test solution and a spot from . Cool the filtrate and add 2 to 3 drops of gelatin TS: a white turbidity or precipitate is produced. Gardenia Fruit 0.0 mg of Geniposide (C17H24O10 : 388. ether.93) in Licorice. Vacuumconcentrate the filtrate until the filtrate becomes 10 mL and use this solution as the standard solution. Method of preparation for a dose (one sachet) Angelica Gigas Root. Spray evenly the plate with vanillin-sulfuric acid TS: one spot among the spots from the test solution and a spot from the standard solution show the same color and the same Rf value. shake for 5 minutes. add 1 mL of vanillin-hydrochloric acid TS: a pale red to red-brown color develops. Evaporate all the filtrate. brown to dark brown and brittle massed. Loss on Drying Not more than 15. Extract Content Dilute ethanol-soluble extract— Not less than 70.1 g of pulverized Gambir. weigh 1 g of Poria. add 10 mL of water. add 100 mL of methanol. methanol and water (26 : 14 : 5) to a distance of about 10 cm and airdry the plate. Spray evenly the plate with po anisaldehydesulfuric acid TS and heat at 105 C for 10 minutes: one spot among the spots from the test solution and a spot from the standard solution show the same color and the same Rf value. Vacuum-concentrate the filtrate until the filtrate becomes 10 mL and use this solution as the standard solution. extract with a reflux condenser for 1 hour and filter. weigh 1 g of Bupleurum Root RMPM. add 100 mL of methanol. add 100 mL of methanol. Spray evenly the plate with sulfuric acid TS for o spray and heat at 105 C for 10 minutes: one spot among the spots from the test solution and a spot from the standard solution show the same color and the same Rf value. add 100 mL of methanol. weigh equivalent to 1 g of Licorice.Pulverize Gamisoyosan Extract Granules. Develop the plate with a mixture of hexane and acetone (7 : 3) to a distance of about 10 cm and air-dry the plate. Separately. (5) Peony Root . add 10 mL of water. Spot 20 μL each of the test solution and the standard solution on a plate of silica gel for thin-layer chromatography. (3) Poria . Vacuum-concentrate the filtrate until the filtrate becomes 10 mL and use this solution as the test solution. shake for 5 minutes. weigh equivalent to 1 g of Poria. Perform the test with the test solution and the standard solution as directed under the Thin-layer Chromatography. Develop the plate with a lower layer of the mixture of chloroform. (8) Gardenia Fruit . Vacuumconcentrate the filtrate until the filtrate becomes 10 mL and use this solution as the standard solution. add 100 mL of methanol.KP VIII 1037 the standard solution show the same color and the same Rf value.Pulverize Gamisoyosan Extract Granules. add 10 mL of water. Perform the test with the test solution and the standard solution as directed under the Thin-layer Chromatography. Vacuumconcentrate the filtrate until the filtrate becomes 10 mL and use this solution as the standard solution. Develop the plate with a mixture of chloroform. Vacuum-concentrate the filtrate until the filtrate becomes 10 mL and use this solution as the standard solution. Vacuum-concentrate the filtrate until the filtrate becomes 10 mL and use this solution as the standard solution. Spray evenly the plate with po anisaldehyde. Spot 20 μL each of the test solution and the standard solution on a plate of silica gel with fluorescent indicator for thin-layer chromatography.Pulverize Gamisoyosan Extract Granules. add 10 mL of water. Separately. extract with a reflux condenser for 1 hour and filter.Pulverize Gamisoyosan Extract Granules. weigh 1 g of Licorice. weigh equivalent to 1 g of Peony Root. extract with a reflux condenser for 1 hour and filter. Perform the test with the test solution and the standard solution as directed under the Thin-layer Chromatography. Vacuumconcentrate the filtrate until the filtrate becomes 10 mL and use this solution as the test solution. Spot 20 μL each of the test solution and the standard solution on a plate of silica gel for thin-layer chromatography. extract with a reflux condenser for 1 hour and filter. shake for 5 minutes.sulfuric acid TS and heat at 105 C for 10 minutes: one spot among the spots from the test solution and a spot from the standard solution show the same color and the same Rf value. extract with a reflux condenser for 1 hour and filter. Separately. (4) Bupleurum Root . Vacuum-concentrate the filtrate until the filtrate becomes 10 mL and use this solution as the test solution. extract with a reflux condenser for 1 hour and filter. extract with a reflux condenser for 1 hour and filter. Vacuum-concentrate the filtrate until the filtrate becomes 10 mL and use this solution as the test solution. Develop the plate with a mixture of chloroform and methanol (95 : 5) to a distance of about 10 cm and air-dry the plate. extract with a reflux condenser for 1 hour and filter. Examine under ultraviolet light (main wavelength: 254 nm): one spot among the spots from the test solution and a spot from the standard solution show the same color and the same Rf value. toluene and formic acid (6 : 6 : 5 : 3) to a distance of about 10 cm and air-dry the plate. add 100 mL of methanol. Spot 20 μL each of the test solution and the standard solution on a plate of silica gel for thin-layer chromatography. add 100 mL of methanol. Spot 20 μL each of the test solution and the standard solution on a plate of silica gel for thin-layer chromatography. Perform the test with the test solution and the standard solution as directed under the Thin-layer Chromatography. Separately. shake for 5 minutes. add 100 mL of methanol. Vacuumconcentrate the filtrate until the filtrate becomes 10 mL and use this solution as the test solution. weigh 1 g of Moutan Root Bark RMPM. extract with a reflux condenser for 1 hour . add 100 mL of methanol. shake for 5 minutes. extract with a reflux condenser for 1 hour and filter.Pulverize Gamisoyosan Extract Granules. shake for 5 minutes. chloroform. weigh equivalent to 1 g of Bupleurum Root. weigh equivalent to 1 g of Gardenia Fruit. shake for 5 minutes. weigh equivalent to 1 g of Moutan Root Bark. add 100 mL of methanol. Perform the test with the test solution and the standard solution as directed under the Thin- layer Chromatography. Spray evenly the plate with p-anisaldehyde-sulfuric acid TS and heat at 105 o C for 10 minutes. add 100 mL of methanol. (6) Licorice . extract with a reflux condenser for 1 hour and filter. weigh 1 g of Peony Root. add 10 mL of water. add 10 mL of water. Develop the plate with a mixture of ethyl formate. (7) Moutan Root Bark .. methanol and water (30 : 10 : 1) to a distance of about 10 cm and air-dry the plate.Pulverize Gamisoyosan Extract Granules. Separately. Spray evenly the plate with o p-anisaldehyde-sulfuric acid TS and heat at 105 C for 10 minutes: one spot among the spots from the test solution and a spot from the standard solution show the same color and the same Rf value. 1038 Monographs. extract twice repetitively. weigh equivalent to 1 g of Mentha Herb. AT and AS . weigh accurately and pulverize. add 100 mL of methanol. weigh equivalent to 1 g of Ginger. shake for 5 minutes. Separately. Particle Size Distribution Test It meets the requirement. Disintegration Test It meets the requirement.Pulverize Gamisoyosan Extract Granules. weigh accurately and pulverize. add 100 mL of methanol. Separately. add 50 mL of chloroform. Vacuumconcentrate the filtrate until the filtrate becomes 10 mL and use this solution as the standard solution. To the residue. Weigh accurately equivalent to about 10 mg of glycyrrhizic acid. Mobile phase: 60% methanol Flow rate: 1. Spot 20 μL each of the test solution and the standard solution on a plate of silica gel for thin-layer chromatography. add 100 mL of methanol. Vacuum-concentrate the filtrate until the filtrate becomes 10 mL and use this solution as the standard solution. dissolve in methanol to make exactly 50 mL and use this solution as the standard solution. Vacuum-concentrate the filtrate until the filtrate becomes 10 mL and use this solution as the test solution. Vacuum-concentrate the filtrate until the filtrate becomes 10 mL and use this solution as the standard solution. calculated on the anhydrous basis × AT AS Operating conditions Detector: An ultraviolet absorption photometer (wavelength: 254 nm).Pulverize Gamisoyosan Extract Granules. Determine the peak areas. To the residue. Vacuumconcentrate the filtrate. Spray evenly the plate with p-anisaldehyde sulfuric aco id TS and heat at 105 C for 10 minutes: one spot among the spots from the test solution and a spot from the standard solution show the same color and the same Rf value. Spot 20 μL each of the test solution and the standard solution on a plate of silica gel for thin-layer chromatography. After cooling. Assay (1) Total paeoniflorin of Peony Root and Moutan Root Bark . respectively Amount (mg) of paeoniflor in (C 23 H 28 O11 ) = amount (mg) of Paeoniflor in RS. Develop the plate with a mixture of chloroform and methanol (3: 1) to a distance of about 10 cm and air-dry the plate. take the chloroform latyer in separatory funnel. Separately.Take not less than about 20 sachets of Gamisoyosan Extract Granules. add 100 mL of methanol. Column temperature: A room temperature. extract with a reflux condenser for 1 hour and filter. of the test solution and the standard solution. After cooling.0 mL/min (2) Glycyrrhizic Acid of Licorice . add 100 mL of methanol. Vacuum-concentrate the filtrate until the filtrate becomes 50 mL and use this solution as the test solution. add 50 mL of 3 mol/mL sulfuric acid TS and hydrolyze in a water bath for 1 hour. Develop the plate with a mixture of ethyl acetate-acetone (10 : 3) to a distance of about 10 cm and air-dry the plate. weigh accurately about 10 mg of Paeoniflorin RS (separately determined the water content). Pipet 20 μL each of the test solution and the standard solution and perform the test as directed under the Liquid Chromatography according to the following operating conditions. add 10 mL of water. add 100 mL of methanol. Perform the test with the test solution and the standard solution as directed under the Thin-layer Chromatography. extract with a reflux condenser for 1 hour and filter. add methanol to make exactly 50 mL and use the solution as the stan- . Part II and filter. add 30 mL of chloroform.Take not less than about 20 sachets of Gamisoyosan Extract Granules. 4 mm to 6 mm in inside diameter and 15 cm to 25 cm in length. Perform the test with the test solution and the standard solution as directed under the Thin-layer Chromatography. (10) Mentha Herb . weigh 1 g of Gardenia Fruit RMPM. packed with octadecylsilyl silica gel for liquid chromatography (5 μm to 10 μm in particle diameter). weigh 1 g of Mentha Herb. add 10 mL of water. Vacuum-concentrate the filtrate until the filtrate becomes 10 mL and use this solution as the test solution. Vacuumconcentrate the filtrate until the filtrate becomes 10 mL and use this solution as the test solution. Separately. shake for 5 minutes. weigh 1 g of Ginger. Weigh accurately equivalent to about 10 mg of paeoniflorin. Spray evenly the plate with vanillino sulfuric acid TS and heat at 105 C for 10 minutes: one spot among the spots from the test solution and a spot from the standard solution show the same color and the same Rf value. extract with a reflux condenser for 1 hour and filter. extract three times repetitively and combine chloroform layers and filter through anhydrous sodium sulfurate. extract with a reflux condenser for 1 hour and filter. Spray evenly the plate with vanillin-sulfuric acid TS and heat at o 105 C for 10 minutes: one spot among the spots from the test solution and a spot from the standard solution show the same color and the same Rf value. add 10 mL of water. add 100 mL of methanol. Develop the plate with a mixture of hexane and ethyl acetate (85 : 15) to a distance of about 10 cm and air-dry the plate. (9) Ginger . heat and extract with a reflux condenser in a water bath for 3 hour. add 50 mL of water. Column: A stainless steel column. extract with a reflux condenser for 1 hour and filter. Perform the test with the test solution and the standard solution as directed under the Thin-layer Chromatography. shake for 5 minutes. extract with a reflux condenser for 1 hour and filter. Spot 20 μL each of the test solution and the standard solution on a plate of silica gel for thin-layer chromatography. combine the filtrate. heat and extract with a reflux condenser in a water bath for 30 minutes. Description Gardenia Fruit is nearly long ovoid to ovoid fruit. Column temperature: A room temperature. Internally Gardenia Fruit is divided into two loculi. Determine the peak areas. Column temperature: An ordinary temperature. add 10 mL of water. add methanol to make exactly 50 mL and use the solution as the standard solution. prepare the solution. add 100 mL of methanol and extract twice repetitively. water and acetic anhydride (78 : 19 : 3) Flow rate: 1. respectively Amount (mg) of geniposide (C17 H 24 O10 ) = amount (mg) of Geniposide RS. weigh accurately and pulverize. prepared in the same manner as the test solution. Spray evenly p-anisaldehyde-sulfuric acid TS on the plate and heat at 105 o C for l0 minutes: .0 mL/min (3) Geniposide of Gardenia Fruit . heat and extract with a reflux condenser for 1 hour. shake for 5 minutes. containing a mass of seeds in yellow-red to dark red placenta. To 1 mL of the filtrate.0 mg of potassium bichromate in water to make exactly l0 mL. respectively. Column: A stainless steel column. Pipet 20 μL each of the test solution and the standard solution and perform the test as directed under the Liquid Chromatography according to the following operating conditions. markedly raised ridges. Identification (1) Weigh 1 g of pulverized Gardenia Fruit.KP VIII 1039 dard solution. Separately. AT and AS . dissolve l mg of Geniposide RS in 1 mL of methanol and use this solution as the standard solution. Gardenia Fruit has slight odor and bitter taste. 4 mm to 6 mm in inside diameter and 15 cm to 25 cm in length. Separately. AT and AS . Separately. Pipet 10 μL each of the test solution and the standard solution and perform the test as directed under the Liquid Chromatography according to the following operating conditions. Weigh accurately equivalent to about 10 mg of geniposide. usually having 6. add 20 mL of methanol. warm for 3 minutes on a water-bath. rarely 5 or 7.Take not less than about 20 sachets of Gamisoyosan Extract Granules. add 100 mL of warm water. dissolve the residue in methanol to make exactly 50 mL and use this solution as the test solution. calculated on the anhydrous basis × AT AS Operating conditions Detector: An ultraviolet absorption photometer (wavelength: 254 nm). take the supernatant and filter. Gardenia Fruit Gardeniae Fructus Gardenia Fruit is the well ripe fruit or the fruit passed through hot water of Gardenia jasminoides Ellis (Rubiaceae). blackish brown or yellow-red. and filter after cooling. calculated on the anhydrous basis × AT AS Operating conditions Detector: An ultraviolet absorption photometer (wavelength: 254 nm). Calyx or its scar is present at the upper end and sometimes a fruit stalk at the lower end. previously dried in a desiccator (silica gel) for 24 hours. respectively. Mobile phase: A mixture of 15% methanol and acetic anhydride (100 : 1) Flow rate: 1. pericarp is thin and bittle. add 100 mL of water. of the test solution and the standard solution. about 5 mm in major axis. Develop the plate with a mixture of ethyl acetate and methanol (3 : 1) to a distance of about 10 cm and air-dry the plate. weigh accurately about 10 mg of Geniposide RS (separately determined the water content). weigh accurately about 10 mg of Glycyrrhizic acid RS (separately determined the water content).0 mL/min Packaging and Storage Preserve in tight containers. Seed is nearly circular. Amount (mg) of glycyrrhiz ic (C 42 H 62 O 16 ) = amount (mg) of Glycyrrhiz ic acid RS. To the residue. packed with octadecylsilyl silica gel for liquid chromatography (5 μm in particle diameter). cool. flat. and use this solution as the standard solution. 4 mm to 6 mm in inside diameter and 15 cm to 25 cm in length.0 g each of pulverized Gardenia Fruit and Gardenia Fruit RMPM. Mobile phase: A mixture of methanol. add water to make 10 mL: the color of the resulting solution is yellow and is not lighter than that of the following control solution. packed with octadecylsilyl silica gel for liquid chromatography (5 μm in particle diameter). warm the mixture between 60 o C and 70 o C for 30 minutes with frequent shaking. of the test solution and the standard solution. Column: A stainless steel column. Spot 10 μL each of the test solution and the standard solution on a plate of silica gel for thin-layer chromatography. External surface is yellowish brown to blackish brown. 1 cm to 5 cm in length and 10 mm to 15 mm in width. Perform the test with the test solution and the standard solution as directed under the Thin-layer Chromatography. Determine the peak areas. (2) Weigh 1. filter and use the filtrates as the test solution and the standard solution of Gardenia Fruit RMPM. Control solution—Dissolve 2. Combine the filtrates. vacuum-concentrate the filtrate. Develop the plate with a mixture of ethyl acetate. The texture is hard. heat on a water bath under a reflux condenser for 1 hour and filter. 2 to 5 cm in width and 1 to 2 cm in thickness. Gentian has characteristic odor and sweet at first. Ash Not more than 6. Not less than 17. Spot 5 μL each of the test solution and the standard solution of Gastrodia Rhizoma RMPM on a plate of silica gel for thin-layer chromatography. Examine under ultraviolet light (main wavelength: 254 nm): one spot among the several spots from the test solution and a dark purple spot from the standard solution show the same color and the same Rf value. Gentian is the root and rhizome of Gentiana lutea Linné (Gentianaceae). on it. and fractured surface is yellow-brown to black-brown. Spray diluted sulfuric acid TS to the plate. add 10 mL of methanol. Perform the test with the test solution and the standard solution of Gastrodia Rhizoma RMPM as directed under the Thin-layer Chromatography.0%. 5 to 15 cm in length. 10 mm in both inside diameter and in height. Perform the test with the test solution as directed under the Thin-layer Chromatography. The xylem consists chiefly of parenchyma.1 g of pulverized Gentian. add 5 mL of 70 % solution of methanol. respectively. Separately. Extract Content Dilute ethanol-soluble extract— Gentian Gentianae Luteae Radix et Rhizoma Description Gentian consists of root and rhizome. shake for 5 minutes and filter and use the filtrate as the test solution. Spot 10 μL each of the test solution and the standard solution on a plate of silica gel with fluorescent indicator for thin-layer chromatography. a transverse section reveals fine needles of calcium oxalate in parenchyma cells. dissolve 1 mg of gentiopicroside RS in 10 mL of methanol and use this solution as the standard solution. a purplish-red color develops. . add 10 mL of water. Under a microscope. Gastrodia Rhizoma has slight odor and sweet taste. and filter.1040 Monographs. lustrous. nearly cylindrical. slat-shped cylindrical to a long fusiform. heat the plate at 105 o C for 10 minutes. Under a microscope. (2) Weigh 0. The secondary cortex of the parenchyma is with irregularly distributed phloem. boil on a water bath for 5 minutes. Put a glass ring. External surface is dark brown. The rhizome is short with fine transverse wrinkles and sometimes with buds and remains of leaves at the upper edge. methanol and water (7 : 2. Parenchyma of the xylem and the cortex contain oi1 droplets.5 g of pulverized Gentian.5 : 0. Ash Not more than 6. with irregulary longitudinal wrinkles. previously dried in a desiccator (silica gel) for 48 hours.5 g each of pulverized Gastrodia Rhizoma and Gastrodia Rhizoma RMPM.0%.0%. minute needle crystals of calcium oxalate and very rarely starch grains 10 μm to 20 μm in diameter. The spots from the test solution and the spots from the standard solution of Gastrodia Rhizoma RMPM show the same color and the same Rf value. later persistently bitter taste.0%. To the filtrate add 2 to 4 drops of iodine TS. Description Gastrodia Rhizoma is somewhat tortuous caulis. sometimes lateral cutting.5 g of pulverized Gastrodia Rhizoma. Identification (1) Weigh 0. Part II The several spots from the test solution and the spots from the standard solution of Gardenia Fruit RMPM show the same color and the same Rf value. with individual or clustered vessels and tracheids and exhibits some sieve tubes of xylem. with lateral roots.4%. Use the filterates as the test solution and the standard solution of Gastrodia Rhizoma RMPM. anhydrous ethanol and water (8 : 2 : 1) to a distance of about 10 cm and air-dry the plate. on a slide glass. Identification 1) Weigh 0. Acid-insoluble Ash Not more than 0. External surface is light yellowish white to yellow-brown. Loss on Drying Not more than 13. 2) Weigh 0. Ash Not more than 6. Deve1op the plate with a mixture of dichloromethane. then cover with another slide and heat gently and gradually: pale yellow crystals are sublimed on the upper slide and the crystals are insoluble in water or in ethanol and soluble in potassium hydroxide TS. The root is longitudinally and deeply wrinkled and more or less twisted: 10 cm to 50 cm in length and 2 cm to 4 cm in diameter.0%. Fractured surface is yellowish brown and not fibrous and the cortex and xylem has a cambium and its neighborhood tinged dark brown. one spot among the spots from the test solution and a dark purple spot from the standard solution show the same color and the same Rf value. and ring nodes. and horny. a transverse section of the root reveals several layers of collenchyma adjoined internally to 4 to 6 layers of thinwalled cork.25) to a distance of about 10 cm and air-dry the plate. Gastrodia Rhizoma Gastrodiae Rhizoma Gastrodia Rhizoma is the caulis et rhizoma of Gastrodia elata Blume (Orchidaceae). Outer surface of the root is externally yellowish brown to grayish yellowish brown. Extract Content Dilute ethanol-soluble extract— Not less than 15. shake for 20 minutes. Ash Not more than 10. and irregularly scattered sieve tubes. short rhizome. often is irregularly branched. a transverse section of the young root reveals epidermis. the outermost layer is endodermis consisting of characteristic cells divided into a few daughter cells. at both ends. External surface is grayish white to pale grayish brown and often with white powder. Ash Not more than 7. grayish yellow-green to grayish brown.KP VIII 1041 Acid-insoluble Ash Not more than 3. long roots around. exodermis and a few layers of primary cortex. plate or sand crystals of calcium oxalate and oil drops.0%. and has longitudinal. Ginger is 2 cm to 4 cm in length.0%. 1 cm to 2 cm in diameter and with pale gray-yellow periderm or without the periderm. sieve tubes existing in xylem. yellow substances as essential and rarely crystals of calcium oxalate. Acid-insoluble Ash Not more than 1. and numerous slender. and air-dry the plate. rarely with sieve tubes.1 g of Geranium Herb. Geranium Herb is the aerial part collected before or when flowering of Geranium thunbergii Siebold et Zuccarini (Geraniaceae). vessels arranged rather radially in xylem. Acid-insoluble Ash Not more than 3. the rhizome has large pith. Stem is slender and long. Spot 10 μL of the test solution on a plate of silica gel with fluorescent indicator for thin-layer chromatography. Under a microscope. Secondary cortex has dents here and there. greenbrown. filer and to the filtrate. Develop the plate with a mixture of ethyl acetate. Description Ginger consists of rhizome. about 3 mm in diameter. Stem and leaf are covered with soft hairs. Under a microscope.4% of 6-gingerol (C17H26O4: 294. filter. Identification Weigh 0. Identification Weigh 0. . and fractured surface of the root is smooth and yellowbrown.0%. coarse wrinkles on the outer surface. add 10 mL of methanol. are swelled warty. a transverse section reveals vascular bundles and secretes scattered all over the surface as small dark brown dots. The root is 10 to 15 cm in length. and use the filtrate as the test solution.5 g of pulverized Gentian Root and Rhizome. Starch grains are usually absent. and water (8 : 2 : 1) to a distance of about 10 cm.0%. Packaging and Storage Preserve in tight containers. often with collenchyma of l to 2 layers contacting the inner side. Description Gentian Root and Rhizome is cylindrical.0%. Perform the test with the test solution as directed under the Thin-layer Chromatography. Ginger.0%. usually. Fractured surface is somewhat fibrous. Leaf is divided palmately into 3 to 5 lobes and 2 cm to 4 cm in length. Gentiana truflora Pallas or Gentiana manshurica Kitagawa (Gentianaceae). Geranium Herb Geranii Herba Gentian Root and Rhizome Gentianae scabrae Radix et Rhizoma Gentian Root and Rhizome is the root and the rhizome of the Gentiana scabra Bunge. sometimes attached buds. Examine under ultraviolet light (main wavelength: 254 nm): one spot among the several spots form the test solution and a dark purple spot from the standard solution show the same color and the some Rf value. The rhizome is about 2 cm in length.39). Each lobe is oblong to obovate and its upper margin is crenate. flexible. powdery. Purity Foreign matter—The amount of the root and other foreign matter contained in Geranium Herb is not more than 2. Geranium Herb has slight odor and astringent taste. Description Geranium Herb is the aerial part of stem with leaves opposite. pale yellowish brown. Separately. Gentian Root and Rhizome has slight characteristic odor and extremely bitter and lasting taste. vascular bundles contain a few fibers. and parenchyma cells contain starch grains. when dried. Ginger Zingiberis Rhizoma Ginger is the dried rhizome of Zingiber officinale Roscoe (Zingiberacece). add l drop of ferric chloride TS: a dark blue color develops. Parenchyma cells contain needle.5%. contains not less than 0. dehydrated ethanol. dissolve 1 mg of gentiopicroside RS in 1 mL of methanol and use this solution as the standard solution. and has buds or short remains of stems at the top. flat and divided cortex and stele. The branched parts are slightly compressed or slightly curved ovoid or oblong-ovoid. add 10 mL of water. Under a magnifying glass. and about 7 mm in diameter. margin is lobed into 1 to 3 pieces.5 % of total flavonoids. add 40 mL of 60 % solution of acetone and proceed in the same manner.0 mg of Quercetin Dihydrate RS. of 6-gingerol of the test solution and the standard solution. dissolve in methanol to make exactly 100 mL and use this solution as the standard solution. about 4 mm to 6 mm in inside diameter and 15 cm to 25 cm in length. Ginkgo Leaf has characteristic odor and astringent taste. Use this solution as the standard solution. Determine the peak areas.0 g of pulverized Ginger. and dissolve in 20 ml of methanol. add methanol to make exactly 100 mL and use this solution as the test solution. Develop the plate with a mixture of hexane. 4 cm to 8 cm in width and petiole is 2 cm to 7 cm. Pipet 10 μL each of the test and the standard solution and perform the test as directed under the Liquid Chromatography according to the following operating conditions.gingerol (C 17 H 26 O 4 ) A = amount (mg) of 6 . Column: A stainless steel column. Purity Foreign matter—not more than 5. filter and use the filtrate as the test solution.0 % Assay Weigh accurately about 2. add 60 mL of methanol. acetone and acetic anhydride (10 : 7 : 1) to a distance of about 10 cm and air-dry the plate. Under a microscope. 100 o C to 105 o C . calculated on the basis of the dried material.4-dinitrophenylhydrazine TS and heat at 105 o C for 10 minutes: one spot of the several spots from the test solution and a brown spot from the standard solution show the same color and Rf value. Combine the filtrates and add 60 % solution of acetone to make exactly 100 ml. Allow to cool to room temperature and use this solution as the test solution. Separately. the upper surface reveals globular epidermal cells. warm and extract and filter. 2 hours) Ash not more than 11. rinsing with 30 ml of methanol. respectively.4 ml of hydrochloric acid. To the residue. Mobile phase: A mixture of acetonitrile and water (45 : 55). Pipette 10 ml of the supernatant liquid in a 10 ml brown-glass vial.5 g of pulverized Ginkgo Leaf. Identification Weigh 0. Perform the test with the test solution and the standard solution as directed under the Thin-layer Chromatography.5 g of pulverized Ginkgo leaf. Determine the peak areas. kaempferol (the relative retention . Add 4. Ginkgo Leaf Ginkgo Folium Ginkgo Leaf is the leaf of Ginkgo biloba Linné (Ginkgoaceae). add 50 mL of 60 % solution of acetone under a reflux condenser for 30 minutes and filter. weigh accurately about 10 mg of 6-Gingerol RS. weigh accurately 10.0 ml with methanol. Identification Weigh 2 g of pulverized Ginger. 3 cm to 8 cm in length. Evaporate 50 ml of the solution to eliminate the acetone.0 % of stems and not more than 2. Ash Not more than 8. Loss on Drying not more than 11. AT and AS. dilute to 50 ml with water and centrifuge.0 g.0 % of other foreign matter. Ginkgo Leaf contains not less than 0. Leaf vein is parallel along with the fan shape.0%. To the residue. Assay Weigh accurately about 2. of quercetin. Flow rate: Adjust the flow rate so that the retention time of 6-gingerol is about 7 minutes. Separately. Column temperature: A room temperature. Description Ginkgo Leaf is fan-shaped leaf. Spray evenly the plate with 2.0 % (1. add 5 mL of acetone. packed with octadecylsilyl silica gel for liquid chromatography (5 µm to 10 µm in particle diameter). Add 15 ml of dilute hydrochloric acid and 5 ml of water and dilute to 50. Combine all the filtrates. dissolve 1 mg of 6-Gingerol RS in l mL of acetone and use this solution as the standard solution. Vascular bundles are externally surrounded and mesophyll has large schizogenous glands containing yellowish brown secretion. add 10 mL of ethanol. Cortex is primarily sponge cells. Stopper and heat on a water bath for 25 minutes. Packaging and Storage Preserve in tight containers. and ATI. and contains large rosette aggregates of calcium oxalate. extract with a reflux condensor for 2 hours and filter.1042 Monographs. Pipet 10 μL each of the test solution and the standard solution. add 30 mL of methanol and proceed in the same manner. Separately. Add a small amount of magnesium and 1 drop of hydrogen chloride to 1 mL of the filtrate: a red color develops. Leaf base is cuneate and the leaf is brittle. ATQ. Amount (mg) of 6 . and perform the test as directed under the Liquid Chromatography according to the following operating conditions. Part II Ginger has a characteristic odor and extremely pungent taste. Spot 10 μL of the test solution and the standard solution on a plate of silica gel for thin-layer chromatography.Gingerol RS × T AS Operating conditions Detector: An ultraviolet absorption photometer (wavelength: 280 nm). shake for 3 minutes. ATK. add 20 mL of methanol.29). 2) Weigh 2g of pulverized Ginseng. main root. combine the supernatant liquids. Column: A stainless column. add 30 mL of diluted methanol (3 in 5). methanol. and air-dry the plate. Aggregate crystal of calcium oxalate is observed in parenchyma cell of phloem. sometimes with curved crown and with short remains of rhizome.0%.0%.5 minutes. Meyer (Araliaceae). Identification 1) On a section of Ginseng. and brown in the neighborhood of the cambium. a transverse section reveals thin-walled parenchyma cell containing filled with starch grains. Develop the plate with the lower layer of a mixture of chloroform. put in a glass-stoppered centrifuge tube. and cortex is scattered secret vessels filled with yellow to yellow-red secretion. with longitudinal wrinkles and scars of rootlets. Mobile phase A: dissolve 0. Repeat the procedure with the residue using 15 mL of diluted methanol (3 in 5). add l mL of methanol. add 3 mL of 0. respectively. add dilute iodine TS drop-wise: a dark blue color is produced on the surface. allow to stand for 30 minutes. Purity Foreign matter—The amount of the stems and other foreign matter contained in Ginseng is not more than 2. as quercetin) of Quercetin Dehydrate RS × A T + A TK + A TI × 2 × 2. Amount (mg) of total flavonoids = amount (mg. boil gently under a reflux condenser in a water-bath for 15 minutes. Ginseng has characteristic odor and taste. and heat at 110°C for 5 minutes: one of the spots from the test solution and a red-purple spot from the standard solution show the same color and the same Rf value.5). Under a microscope. in the test solution and the peak area. weigh l mg of Ginsenoside Rg1 RS. Mobile phase B: methanol Time (minutes) Mobile phase A (%) Mobile phase B (%) 0 60 40 1 60 40 20 45 55 21 0 100 Flow rate: 1. at first slightly sweet. centrifuge.3 of phosphoric acid to 1000 mL of water and adjust with phosphoric acid to make a pH of 2. The resolution of each peak between the peaks.514 AS Operating conditions Detector: An ultraviolet absorption photometer (wavelength: 370 nm). and use this solution as the standard solution. Extract Content Dilute ethanol-soluble extract— Not less than 14. Column temperature: 25 o C . Fractured surface is practically flat. light yellow-brown. often branching 2 to 5 lateral roots from the middle. Pipet 10mL of this solution.KP VIII 1043 time to quercetin is about 1.4) and isoramnetin (the relative retention time to quercetin is about 1. and water (13 : 7 : 2) to a distance of about 10 cm.0. followed by a slight bitterness. 4 mm in inside diameter and 12. and add diluted methanol (3 in 5) to make exactly 50mL. Mobile phase: Control the mobile phase A and B stepwise or gradient as the following conditions. Ginseng is 5 cm to 20 cm in length. A. filter.0 mL/min. of kaempferol and of isoramnetin. Description Ginseng is thin and long cylindrical roots. Spot 10 μL each of the test solution and the standard solution on a plate of silica gel for thin-layer chromatography. System suitability System performance: The retention time of quercetin adjust at about 12. cool. and use this solution as the sample solution. Perform the test with the test solution and the standard solution as directed under the Thin-layer Chromatography. is not less than 1. Sepa- .5. Ginseng contains not less than 0. Loss on Drying Not more than 15. AS. and use the filtrate as the test solution. from which rootlets and cork layer has been removed.20% of ginsenoside Rb1 (C54H92O23: 1109. of quercetin in the standard solution. 5 mm to 30 mm in diameter.1 mol/L hydrochloric acid TS and diluted methanol (3 in 5) to make exactly 20 mL. packed with octadecylsilyl silica gel for liquid chromatography (5 μm in particle diameter).0 g of pulverized Ginseng. calculated on the basis of dried material. Ginseng Ginseng Radix Ginseng is the root of Panax ginseng C.10% of ginsenoside Rg1 (C42H72O14: 801. Spray evenly sulfuric acid TS for spray on the plate. shake for 15 minutes.0% (6 hours) Ash Not more than 5%. Separately. Assay (1) Ginsenoside Rg1—Weigh accurately about 1.5 cm in length. External surface is pale yellow-brown to pale grayish brown. add 3 mL of dilute sodium hydroxide TS.01) and not less than 0. and separate the supernatant liquid. Amount (mg) of ginsenoide Rg 1 (C 42 H 72 O 14 ) = amount (mg) of Ginsenoide Rg 1 RS. 3 mm to 10 mm in width. AT and AS. When the procedure is run with 10 mL of this solution under the above operating conditions.0% of stem and other foreign material. packed with octadecylsilyl silica gel for liquid chromatography (5 μm in particle diameter). System suitability System performance: Dissolve 1 mg each of ginsenoside Rg1 RS and ginsenoside Re in diluted methanol (3 in 5) to make 10 mL.1044 Monographs. Column temperature: A constant temperature of about 30 o C . the relative standard deviation of the peak area of ginsenoside Rb1 is not more than 1. External surface is purple brown to deep brown. of ginsenoside Rg1. pale reddish brown. Xylem is yellowish white. Slice of Gleditsia Spine is 1 mm to 3 mm in thickness. Texture is light. Flow rate: Adjust the flow rate so that the retention time of ginsenoside Rb1 is about 20 minutes. and use this solution as the standard solution. acute at apex. .6 mm in inside diameter and 15 cm in length.0%. Purity Foreign matter—Not more than 3. Column temperature: A constant temperature of about 40 o C . Separately. System repeatability: When the test is repeated 6 times with 10 mL of the standard solution under the above operating conditions.0% Extract Content Dilute ethanol-soluble extract— Not less than 10. Column: A stainless steel column 4. Main spines are flattened conical or conical. Gleditsia Spine is odorless and has weak taste. Description 1) Gleditsia japonica -Gleditsia Spine from Gleditsia japonica consists of main spines and 1 to 2 branched spines.5. hard and uneasily broken. calculated on the anhydrous basis × AT AS Operating conditions Detector: An ultraviolet absorption photometer (wavelength: 203 nm). calculated on the anhydrous basis × AT AS Operating conditions Detector: An ultraviolet absorption photometer (wavelength: 203 nm). weigh accurately about 10 mg of ginsenoside Rb1 RS (previously determine the water) dissolve in diluted methanol (3 in 5) to make exactly 100 mL. (2) Ginsenoside Rb1—Use the sample solution obtained in (1) as the sample solution. 3 cm to 15 cm in length or longer. and determine the peak areas. Gleditsia Spine Gleditsiae Spina Gleditsia Spine is the thorn of Gleditsia japonica Miquel var. packed with octadecylsilyl silica gel for liquid chromatography (5 μm in particle diameter). Flow rate: Adjust the flow rate so that the retention time of ginsenoside Rg1 is about 25 minutes. System suitability System performance: Dissolve 1 mg each of ginsenoside Rb1 RS and ginsenoside Rc in diluted methanol (3 in 5) to make 10 mL. usually tapering-tupped.0% Ash Not more than 2. System repeatability: When the test is repeated 6 times with 10 mL of the standard solution under the above operating conditions. Loss on Drying Not more than 10. When the procedure is run with 10 mL of this solution under the above operating conditions. easily broken. Perform the test with exactly 10 mL each of the sample solution and standard solution as directed under Liquid Chromatography according to the following conditions. Mobile phase: A mixture of water and acetonitrile (7:3). and determine the peak areas. Branched spines are 1 cm to 6 cm in length.5%. ginsenoside Rb1 and ginsenoside Rc are eluted in this order with the resolution between these peaks being not less than 3. Column: A stainless steel column 4. pith is lax.6 mm in inside diameter and 15 cm in length. 2) Gleditsia sinensis -Gleditsia Spine from Gleditsia sinensis has more circular. ginsenoside Rg1 and ginsenoside Re are eluted in this order with the resolution between these peaks being not less than 1. koraiensis Nakai or Gleditsia sinensis Lamark (Leguminosae). hard main spines and branched spines than those of Gleditsia Spine from Gleditsia japonica. Mobile phase: A mixture of water and acetonitrile (4:1). dissolve in diluted methanol (3 in 5) to make exactly 100mL. Perform the test with exactly 10 mL each of the sample solution and standard solution as directed under Liquid Chromatography according to the following conditions. of ginsenoside Rb1 Amount (mg) of ginsenoide = amount (mg) of Ginsenoide Rb 1 (C 42 H 72 O 14 ) Rb 1 RS. and use this solution as the standard solution.5%. weigh accurately about 10 mg of Ginsenoside Rg1 RS (previously determine the water). AT and AS. and texture is fragile. the relative standard deviation of the peak area of ginsenoside Rg1 is not more than 1. Part II rately. Angelica Gigas Root. Peony Root. 10 cm to 20 cm in length. Dissolve each of the residues to 1 mL of ethanol and use these solutions as the test solution and the standard solution of Glehnia Root RMPM. Spray evenly the plate with diluted sulfuric acid TS and heat at 105 o C for 10 minutes: one of the spots from the test solution and the reddish purple spot from the standard solution are the same color and the Rf value. Glehnia Root is brittle and easily breakable and the fractured surface is powdery. Develop the plate with a mixture of toluene. add 10 mL of ether. Hawthorn Fruit has a number of wrinkles. filter and use the filtrate as the test solution. Spot 4 μL each of the test solution and the standard solution on a plate of silica gel for thin-layer chromatography. Hawthorn Fruit has a dent about 5 mm in diameter sometimes circled with a sepal. Schizonepeta Spike. Poncirus Immature Fruit. 5 mm to 15 mm in diameter.0%.3 mg of glycyrrhizic acid (C42H62 O16: 822. Perform the test with the test solution and the standard solution of of Glehnia Root RMPM as directed under the Thin-layer Chromatography. Angelica Dahurica Root. The several spots from the test solution and the spots from the standard solution of Glehnia Root RMPM show the same color and the same Rf value.5%. cortex is pale milky white to milky yellow and sometimes has clefts. formic acid (20 : 4 : 0. and shake for 2 minutes. Under a magnifying glass. Gardenia Fruit.7 mg of peoniflorin (C23H28O11 : 480. fruit stalk or its mark is observed. The seed is divided ball-shaped. the residue is dissolved in 1 mL of anhydrous acetic acid. Hawthorn Fruit Crataegi Fructus Hawthorn Fruit is the ripe fruit of Crataegus pinnatifida Bunge and its varieties (Rosaceae). At one side. Hyunggeyungyo Extract Granules Hyunggeyungyo Extract Granules contains no less than 2. Method of preparation for a dose (one sachet) Platycodon Root. Bupleurum Root 0. sonicate for 20 minutes and filter. Xylem is pale yellow and dense. dissolve it in 1 mL of ethyl acetate and use this solution as standard solution. Saposhnikovia Root.0%. Hawthorn Fruit has characteristic odor and slightly sour taste. Spot 5 μL each of the test solution and the standard solution of Glehnia Root RMPM on a plate for thin-layer chromatography. add 10 mL of acetone.5) to a distance of about 10 cm and air-dry the plate.5g Pulverize the above crude drugs to coarse powder. (2) Weigh 1 g of pulverized Hawthorn Fruit. extract for 2 to 3 hours at 80 o C and filter. Identification Weigh 1 g each of pulverized Glehnia Root and Glehnia Root RMPM.83 g Licorice.9 mg of baicalin (C21H18O11 : 446. 7 to 15 mm in diameter. Ash Not more than 6. add 4 mL of ethyl acetate. and filter. put into the extractor. Spray evenly diluted sulfuric acid TS to the plate. and 7.94 g to ~ 100 . Separately. each kern contains a seed of each.KP VIII 1045 Glehnia Root Glehniae Radix Glehnia Root is the root and rhizome of Glehnia littoralis Fr. 6 to 8 mm in length. sonicate for 15 minutes. External surface is reddish brown or with spotted grayish brown-grayish. Identification (1) Weigh 1 g of pulverized Hawthorn Fruit. After removing the ether layer.93) in Licorice. Acid-insoluble Ash Not more than 1. Cnidium Rhizome. Scutellaria Root 0. Glehnia Root has slight odor and slightly sweet taste. spherical. 5. weigh 1 mg of Ursolic Acid RS. and oil canals are scattered as brown dots. ethyl acetate. Transverse slices of the middle part shows 5 kerns. Perform the test with the test solution and the standard solution as directed under the Thin-layer Chromatography. Schmidt ex Miquel (Umbelliferae).0 mg of geniposide (C17H24O10 : 388. Deve1op the plate with a mixture of cyclohexane and ethyl acetate (2 : 1) to a distance of about 10 cm and air-dry the plate.46) in Peony Root. weigh each crude drugs. Forsythia Fruit.36) in Scutellaria Root for a dose (a sachet). Ash Not more than 6. External surface is pale yellow-brown to red-brown and detached branched roots and reveals scars of the branched roots. and occasionally cut longitudially. add eight to ten fold of water.37) in Gardenia Fruit. Description Glehnia Root is slight cylindrical root. and add 1 to 2 drops of sulfuric acid: a reddish purple color develops. heat the plate at 105 o C for 10 minutes. At the other side. Description Hawthorn Fruit is the fruit. Evaporate the filtrate to dryness o in vacuum under 60 C until it becomes 1. 1. respectively. external surface is light brown and the texture is hard. Eavaporate the filterates to dryness. add 100 mL of methanol. Hyunggeyungyo Extract Granules is prepared as directed under Granules. Vacuum-concentrate the filtrate until the filtrate becomes 10 mL and use this solution as the test solution. shake for 5 minutes. Vacuum-concentrate the filtrate until the filtrate becomes 10 mL and use this solution as the test solution. add 10 mL of water. Separately. weigh equivalent to 1 g of Angelica Gigas Root. Separately. weigh accurately about 1 g of pulverized Bupleurum Root RMPM. add 100 mL of methanol. Spray evenly the plate with sulfuric acid TS for spray o and heat at 105 C for 10 minutes: one spot among the spots from the test solution and a spot from the standard solution show the same color and the same Rf value. Spot 20 μL each of the test solution and the standard solution on a plate of silica gel for thin-layer chromatography. ether. add 100 mL of methanol.92 g to 1. add 100 mL of methanol. (5) Angelica Gigas Root . shake for 5 minutes. Perform the test with the test solution and the standard solution as directed under the Thinlayer Chromatography. water and acetic acid (500 : 500 : 5 : 2) to a distance of about 10 cm and air-dry the plate. weigh accurately about 1 g of pulverized Angelica Dahurica Root. extract with a reflux condenser for 1 hour and filter. shake for 5 minutes. methanol and water (65 : 35 : 10) to a distance of about 10 cm and air-dry the plate. weigh accurately about 1 g of pulverized Licorice. add 10 mL of water. Separately. extract with a reflux condenser for 1 hour and filter. Vacuumconcentrate the filtrate until the filtrate becomes 10 mL and use this solution as the test solution. extract with a reflux condenser for 1 hour and filter. weigh equivalent to 1 g of Angelica Dahurica Root. Separately. (2) Angelica Dahurica Root . extract with a reflux condenser for 1 hour and filter. extract with a reflux condenser for 1 hour and filter. (3) Bupleurum Root . Vacuum-concentrate the filtrate until the filtrate becomes 10 mL and use this solution as the test solution. add 10 mL of water. Vacuum-concentrate the filtrate until the filtrate becomes 10 mL and use this solution as the standard solution. Develop the plate with a mixture of chloroform. extract with a reflux condenser for 1 hour and filter. shake for 5 minutes. Spray evenly the plate with vanillin-sulfuric acid TS: one spot among the spots from the test solution and . Spot 20 μL each of the test solution and the standard solution on a plate of silica gel with a fluorescent indicator for thin-layer chromatography. add 100 mL of methanol. Develop the plate with a mixture of chloroform. Spot 20 μL each of the test solution and the standard solution on a plate of silica gel for thin-layer chromatography. Indentification (1) Platycodon Root . Examine under ultraviolet light (main wavelength : 365 nm) : one spot among the spots from the test solution and a spot from the standard solution show the same color and the same Rf value. Perform the test with the test solution and the standard solution as directed under the Thin-layer Chromatography. Develop the plate with a mixture of hexane and ethyl acetate (1 : 1) to a distance of about 10 cm and air-dry the plate. Vacuum-concentrate the filtrate until the filtrate becomes 10 mL and use this solution as the standard solution. Part II 2. extract with a reflux condenser for 1 hour and filter. weigh equivalent to 1 g of Licorice. (4) Licorice . add 100 mL of methanol. weigh equivalent to 1 g of Bupleurum Root. extract under a reflux condenser for 1 hour and filter. Vacuum-concentrate the filtrate until the filtrate becomes 10 mL and use this solution as the standard solution. weigh accurately about 1 g of pulverized Platycodon Root. Vacuum-concentrate the filtrate until the filtrate becomes 10 mL and use this solution as the test solution.Pulverize Hyunggeyungyo Extract Granules.75 g of Viscous extract or concentrate in a suitable method until it becomes 0. add 10 mL of water. Vacuum-concentrate the filtrate until the filtrate becomes 10 mL and use this solution as the standard solution. Perform the test with the test solution and the standard solution as directed under the Thin-layer Chromatography. add 100 mL of methanol. Develop the plate with a mixture of toluene. Perform the test with the test solution and the standard solution as directed under the Thin-layer Chromatography. Spot 20 μL each of the test solution and the standard solution on a plate of silica gel for thin-layer chromatography. Spray evenly the plate with sulfuric acid TS o for spray and heat the plate at 105 C for 10 minutes: one spot among the spots from the test solution and a spot from the standard solution show the same color and the same Rf value. weigh equivalent to 1 g of Platycodon Root. Separately. add 100 mL of methanol.1046 Monographs. Spray evenly the plate with p-anisaldehyde-sulfuric aco id TS and heat at 105 C for 10 minutes: one spot among the spots from the test solution and a spot from the standard solution show the same color and the same Rf value. Develop the plate with a mixture of chloroform and methanol (95 : 5) to a distance of about 10 cm and air-dry the plate. extract with a reflux condenser for 1 hour and filter. add 10 mL of water. Vacuum-concentrate the filtrate until the filtrate becomes 10 mL and use this solution as the standard solution. Perform the test with the test solution and the standard solution as directed under the Thin-layer Chromatography.30 g of Dry extract. add 100 mL of methanol.Pulverize Hyunggeyungyo Extract Granules. methanol and water (30 : 10 : 1) to a distance of about 10 cm and air-dry the plate.Pulverize Hyunggeyungyo Extract Granules. shake for 5 minutes.Pulverize Hyunggeyungyo Extract Granules. extract with a reflux condenser for 1 hour and filter. weigh accurately about 1 g of pulverized Angelica Gigas Root. add 100 mL of me- thanol. Spot 20 μL each of the test solution and the standard solution on a plate of silica gel for thin-layer chromatography.Pulverize Hyunggeyungyo Extract Granules. Vacuumconcentrate the filtrate until the filtrate becomes 10 mL and use this solution as the standard solution. Separately.Pulverize Hyunggeyungyo Extract Granules. Spray evenly the plate with sulfuric o acid TS for spray and heat at 105 C for 10 minutes. Vacuum-concentrate the filtrate until the filtrate becomes 10 mL and use this solution as the standard solution. Separately. Spot 20 μL each of the test solution and the standard solution on a plate of silica gel with a fluorescent indicator for thin-layer chromatography. weigh equivalent to 1 g of Saposhnikovia Root. extract with a reflux condenser for 1 hour and filter. weigh accurately about 1 g of pulverized Saposhnikovia Root. Develop the plate with a mixture of hexane and ethyl acetate (1 : 1) to a distance of about 10 cm and air-dry the plate. weigh equivalent to 1 g of Peony Root. Vacuum-concentrate the filtrate until the filtrate becomes 10 mL and use this solution as the standard solution. Separately. Develop the plate with a lower layer of the mixture of chloroform. weigh equivalent to 1 g of Forsythia Fruit. add 100 mL of methanol. weigh equivalent to 1 g of Cnidium Rhizome. Perform the test with the test solution and the standard solution as directed under the Thinlayer Chromatography. shake for 5 minutes. add 100 mL of methanol. Perform the test with the test solution and the standard solution as directed under the Thin-layer Chromatography. weigh equivalent to 1 g of Poncirus Immature Fruit Root.Pulverize Hyunggeyungyo Extract Granules. Separately. Vacuum-concentrate the filtrate until the filtrate becomes 10 mL and use this solution as the standard solution.sulfuric acid TS and heat at 105 C for 10 minutes: one spot among the spots from the test solution and a spot from the standard solution show the same color and the same Rf value. extract with a reflux condenser for 1 hour and filter. weigh accurately about 1 g of pulverized Peony Root.Pulverize Hyunggeyungyo Extract Granules. Examine under ultraviolet light (main wavelength: 365 nm): one spot among the spots from the test solution and a spot from the standard solution show the same color and the same Rf value. shake for 5 minutes. extract with a reflux condenser for 1 hour and filter. methanol and water (26 : 14 : 5) to a distance of about 10 cm and airdry the plate. Vacuum-concentrate the filtrate until the filtrate becomes 10 mL and use this solution as the test solution. (8) Peony Root . add 100 mL of methanol. add 100 mL of methanol. extract with a reflux condenser for 1 hour and filter. Examine under ultraviolet light (main wavelength: 365 nm): one spot among the spots from the test solution and a spot from the standard solution show the same color and the same Rf value. add 10 mL of water. (7) Forsythia Fruit . Spot 20 μL each of the test solution and the standard solution on a plate of silica gel with a fluorescent indicator for thin-layer chromatography. Spot 20 μL each of the test solution and the standard solution on a plate of silica gel with a fluorescent indicator for thin-layer chromatography. add 100 mL of methanol.Pulverize Hyunggeyungyo Extract Granules. formic acid and water (5 : 3 : 1 : 1) to a distance of about 10 cm and air-dry the plate. Perform the test with the test solution and the standard solution as directed under the Thin-layer Chromatography. methyl ethyl ketone. Spray evenly the plate with p-anisaldehydeo sulfuric acid TS and heat at 105 C for 10 minutes. weigh accurately about 1 g of pulverized Cnidium Rhizome. extract with a reflux condenser for 1 hour and filter. Vacuumconcentrate the filtrate until the filtrate becomes 10 mL and use this solution as the test solution. add 10 mL of water. Develop the plate with a mixture of cyclohexane and ethyl acetate (9 : 1) to a distance of about 10 cm and air-dry the plate. Spray evenly the plate with po anisaldehyde. shake for 5 minutes. shake for 5 minutes. (10) Cnidium Rhizome .Pulverize Hyunggeyungyo Extract Granules. (9) Poncirus Immature Fruit Root . add 100 mL of methanol. Develop the plate with a mixture of ethyl acetate. Perform the test with the test solution and the standard solution as directed under the Thin-layer Chromatography. add 10 mL of water. extract with a reflux condenser for 1 hour and filter. extract with a reflux condenser for 1 hour and filter. add 100 mL of methanol. Vacuum-concentrate the filtrate until the filtrate becomes 10 mL and use this solution as the test solution. Perform the test with the test solution and the standard solution as directed under the Thin-layer Chromatography. (6) Saposhnikovia Root . add 10 mL of water. extract with a reflux condenser for 1 hour and filter. Develop the plate with a mixture of ethyl acetate and hexane (5 : 1) to a distance of about 10 cm and air-dry the plate. Vacuum-concentrate the filtrate until the filtrate becomes 10 mL and use this solution as the test solution. weigh accurately about 1 g of pulverized Poncirus Immature Fruit Root RMPM. Vacuum-concentrate the filtrate until the filtrate becomes 10 mL and use this solution as the standard solution. shake for 5 minutes. weigh accurately about 1 g of pulverized Forsythia Fruit. extract with a reflux condenser for 1 hour and filter. add 100 mL of methanol. Separately. Vacuum-concentrate the filtrate until the filtrate becomes 10 mL and use this solution as the test solution. Spot 20 μL each of the test solution and the standard solution on a plate of silica gel with a fluorescent indicator for thin-layer chromatography.KP VIII 1047 a spot from the standard solution show the same color and the same Rf value. Examine under ultraviolet light (main wavelength: 365 nm): one spot among the spots from the test solution and a spot from the standard solution show the same color and the same Rf value. extract with a reflux condenser for 1 hour and filter.. add 100 mL of methanol. add 100 mL of methanol. add 10 mL of water. Spot 20 μL each of the test solution and the standard solution on a plate of silica gel with a fluorescent indicator for thin-layer chromatography. Examine under ultraviolet light (main wavelength: 365 nm): one spot among the spots from the test solution . weigh accurately about 1 g of pulverized Scutellaria Root RMPM. respectively Amount (mg) of glycyrrhizic acid (C 42 H 62 O16 ) = amount (mg) of Glycyrrhizic Acid RS. Vacuum-concentrate the filtrate until the filtrate becomes 10 mL and use this solution as the test solution. Vacuum-concentrate the filtrate until the filtrate becomes 10 mL and use this solution as the standard solution. Assay (1) Glycyrrhizic Acid of Licorice . water and acetic anhydride (78 : 19 : 3) Flow rate: 1.Take not less than about 20 sachets of Hyunggeyungyo Extract Granules. add 30 mL of chloroform. Column temperature: A room temperature. Spot 20 μL each of the test solution and the standard solution on a plate of silica gel for thin-layer chromatography. Separately. 4 mm to 6 mm in inside diameter and 15 cm to 25 cm in length. weigh equivalent to 1 g of Scutellaria Root.1048 Monographs. extract with a reflux condenser for 1 hour and filter. Spray evenly the plate with ferric chloride-methanol TS : one spot among the spots from the test solution and a spot from the standard solution show the same color and the same Rf value. shake for 5 minutes. Spray evenly the plate with po anisaldehyde. shake for 5 minutes. weigh equivalent to 1 g of Schizonepeta Spike. Spray evenly the plate with vanillin-sulfuric acid TS and heat at standard solution as directed under the Thin-layer Chromatography. extract with a reflux condenser for 1 hour and filter. weigh equivalent to 1 g of Gardenia Fruit. Vacuum-concentrate the filtrate until the filtrate becomes 10 mL and use this solution as the standard solution. extract with a reflux condenser for 1 hour and filter. add 50 mL of chloroform. of the test solution and the standard solution. Perform the test with the test solution and the standard solution as directed under the Thin-layer Chromatography. heat and extract with a reflux condenser for 3 hour. add 50 mL of 3 mol/mL sulfuric acid TS and hydrolyzed in a water bath for 1 hour. as the standard solution. weigh 1 g of pulverized Gardenia Fruit RMPM. (12) Schizonepeta Spike . weigh and pulverize. extract with a reflux condenser for 1 hour and filter. After cooling.Take not less than .Pulverize Hyunggeyungyo Extract Granules. add 100 mL of methanol. acetone and chloroform (40 : 35 : 25) to a distance of about 10 cm and air-dry the plate. Vacuum-concentrate the filtrate. Develop the plate with a mixture of hexane and ethyl acetate (17 : 3) to a distance of about 10 cm and air-dry the plate. Column: A stainless steel column. (11) Gardenia Fruit . Pipet 10 μL each of the test solution and the standard solution and perform the test as directed under the Liquid Chromatography according to the following operating conditions. Perform the test with the test solution and the calculated on the anhydrous basis × AT AS Operating conditions Detector: An ultraviolet absorption photometer (wavelength: 254 nm). prepared in the same manner as the test solution. Weigh accurately equivalent to about 10 mg of glycyrrhizic acid.Pulverize Hyunggeyungyo Extract Granules. heat and extract with a reflux condenser in a water bath for 30 minutes. After cooling. Separately. packed with octadecylsilyl silica gel for liquid chromatography (5 μm to 10 μm in particle diameter). dissolve the residue in methanol to make exactly 50 mL and use this solution as the test solution Separately. Determine the peak areas. shake for 5 minutes. o 105 C for 10 minutes: one spot among the spots from the test solution and a spot from the standard solution show the same color and the same Rf value. AT and AS . add 100 mL of methanol. extract with a reflux condenser for 1 hour and filter. use the solution. Separately. Spot 20 μL each of the test solution and the standard solution on a plate of silica gel with a fluorescent indicator for thin-layer chromatography. Mobile phase: A mixture of methanol. Perform the test with the test solution and the standard solution as directed under the Thinlayer Chromatography. take the chloroform layer in separatory funnel. extract with a reflux condenser for 1 hour and filter. Develop the plate with a mixture of chloroform and methanol (3 : 1) to a distance of about 10 cm and air-dry the plate. Particle Size Distribution Test It meets the requirement. add 100 mL of methanol. Vacuum-concentrate the filtrate until the filtrate becomes 10 mL and use this solution as the test solution. add 10 mL of water. Disintegration Test It meets the requirement. combine chloroform layers and filter through anhydrous sodium sulfurate. (13) Scutellaria Root .0 mL/min (2) Paeoniflorin of Peony Root . add 10 mL of water. Spot 20 μL each of the test solution and the standard solution on a plate of silica gel for thin-layer chromatography.Pulvarize Hyunggeyungyo Extract Granules. Vacuum-concentrate the filtrate until the filtrate becomes 10 mL and use this solution as the test solution. weigh accurately about 1 g of pulverized Schizonepeta Spike. extract three times repetitively. add 100 mL of methanol. Part II and a spot from the standard solution show the same color and the same Rf value. add 100 mL of methanol. Develop the plate with a mixture of toluene. Vacuumconcentrate the filtrate until the filtrate becomes 10 mL and use this solution as the standard solution. weigh accurately about 10 mg of Glycyrrhizic acid RS (separately determined the water content). add 10 mL of water. add 100 mL of methanol. add 50 mL of water.sulfuric acid TS and heat at 105 C for 10 minutes: one spot among the spots from the test solution and a spot from the standard solution show the same color and the same Rf value. Under a magnifying glass. Under a microscope. Afterward examine the test followed by the assay of Peony Root. Camus (Gramineae). weigh accurately about 10 mg of Geniposide RS (separately determined the water content). Add methanol to make exactly 100 mL and use this solution as the test solution.Take not less than about 20 sachets of Hyunggeyungyo Extract Granules. packed with octadecylsilyl silica gel for liquid chromatography (5 μm to 10 μm in particle diameter). (2) Weigh 2 g of pulverized Imperata Rhizome. yellowish white and with scattered brown spots. place 0. extract twice repetitively. chloroform and acetone (40 : 30 : 30) to a distance of about 10 cm and air-dry the plate. Separately. add 100 mL of methanol. add 100 mL of methanol. the vascular bundle is lateral and arranged radially between epidermis and endodermis. sonicate for 1 hour and filter. add 70 mL of methanol. Vascular bundles are scattered densely and irregularly as atactostele in the endodermis. add 20 mL of hexane. Fibers of bundle sheath are around the vascular bundles. Identification (1) Weigh l. weigh and pulverize. Pipet 20 μL each of the test solution and the standard solution and perform the test as directed under the Liquid Chromatography according to the following operating conditions. External surface is yellowish white with slight longitudinal wrinkles and with nodes at 2 cm to 3 cm intervals. Mobile phase: A mixture of 15% methanol and acetic anhydride (100 : 1) Flow rate: 1. AT and AS . Column temperature: A room temperature.5 mL of acetic anhydride by shaking and add carefully 0. Purity (1) Rootlet and scaly leaf—Less than 3.0 mL/min (4) Baicalin of Scutellaria Root . respectively Amount (mg) of geniposide (C17 H 24 O10 ) = amount (mg) of Geniposide RS.0%. shake for 5 minutes. allow the mixture to stand for 30 minutes with occasional shaking and filter. Column: A stainless steel column. Develop the plate with a mixture of cyclohexane. take the supernatant and filter. weigh accurately about 10 mg of Paeoniflorin RS (separately determined the water content). Separately. Determine the peak areas.5 mL of this solution in a test tube and mix with 0. Concentrate the filtrate to 5 mL and use this solution as the test solution. add 20 mL of 95% ethanol . but slightly sweet later. Spot 5 μL of the test solution on a plate of silica gel for thinlayer chromatography.0 g of pulverized Imperata Rhizome. Ash Not more than 5. Afterward examine the test followed by the assay of Scutellaria Root Packaging and Storage Preserve in tight containers. and often branched. extract with a reflux condenser for 1 hour. vacuumconcentrate the filtrate until the filtrate becomes 50 mL and use this solution as the test solution. 3 mm to 5 mm in diameter. . Thickness of cortex is slightly smaller than the diameter of the stele. Evaporate the filtrate to dryness. dissolve in methanol to make exactly 50 mL and use this solution as the standard solution. Spray evenly the plate with diluted sulfuric acid TS and heat at 105 o C for 10 minutes: spot of the Rf value about 0. weigh and pulverize. combine the filtrates. 4 mm to 6 mm in inside diameter and 15 cm to 25 cm in length. add methanol to make exactly 20 mL and use the solution as the standard solution. calculated on the anhydrous basis × AT AS Operating conditions Detector: An ultraviolet absorption photometer (wavelength: 254 nm). from which rootlets and scale leaves have been removed. weigh and pulverize. Weigh accurately equivalent to about 50 mg of baicalin.5 mL of sulfuric acid to make two layers: a red-brown color develops at the zone of contact and the upper layer produces a bluegreen to blue-purple color. Perform the test with the test solution as directed under the Thin-layer Chromatography.0%. long and thinly cylindrical. Pith is often hollow. and extract with a reflux condenser for 1 hour. Fractured surface is fibrous. of the test solution and the standard solution. (2) Foreign matter—The amount of foreign matter other than rootlets and scaly leaves is not more than 1. add 10 mL of water. . (3) Geniposide of Gardenia Fruit . Imperata Rhizome Imperatae Rhizoma Imperata Rhizome is the rhizome of Imperata cylindrica Beauvois var. Description Imperata Rhizome is the rhizome.6 is purple. koenigii Durand et Schinz ex A. Weigh accurately equivalent to about 50 mg of geniposide.Take not less than about 20 sachets of Hyunggeyungyo Extract Granules. cool and filter. Imperata Rhizome is odorless and tasteless at first. Stele is yellowish brown.KP VIII 1049 about 20 sachets of Hyunggeyungyo Extract Granules. To the residue.0%. Weigh accurately equivalent to about 10 mg of paeoniflorin. a transverse section reveals cortex. dissolve the residue in 5 mL of chloroform. A transverse section is irregularly round. Epicarp is thin and .0% (6 hours). Lee (Rhamnaceae). has dense ring band. 3 cm to 15 cm in length and about 5 mm in diameter. Column temperature: A constant temperature of about 50 o C .01 mol/L hydrochloric acid TS. Under a microscope. vessels and tracheids are arranged alternately. curved. External surface is red-brown to dark redbrown with wrinkles and lustrous. inermis Rehder or Zizyphus jujube Miller var. calculated on the basis dried material. Both ends of the Jujube is slightly dented. Amount (mg) of total alkaloids (emetine and cephaeline) = amount (mg) of Emetine Hydrochloride RS A + A TC × 0. with a scar of style on one end and a scar of fruit stalk on the other. Separately. cylindrical root and rhizome.0% of the total alkaloids [as emetine(C29H40N2O4: 480. Determine the peak areas.01 mol/ L hydrochloric acid TS to make exactly 100 mL and use this solution as the test solution. adjust the pH 4. Use a column giving elution of cephaeline and emetine in this order and clearly dividing each peak.67 kPa. The cortex thickens ring or semi-ring shape. Mobile phase: Dissolve 2 g of sodium 1-heptane sulfonate in 500 mL of water. consisting of brown thin-walled cork cells. dissolve in 0. in the test solution and the peak area. and unthickened parts are observed. Column: A stainless steel column. Thickness of cortex is up to about two-thirds of radius in thickened part. 2 cm to 3 cm in length and 1 cm to 2 cm in diameter. Loss on Drying Not more than 12. allow to stand for 1 hour with occasional shaking and filter. weigh accurately about 10 mg of Emetine Hydrochloride RS. Description Ipecac is a slender. Part II Acid-insoluble Ash Not more than l. 50 o C ) for 5 hours.1050 Monographs.01 mol/L hydrochloric acid TS. 4 mm to 6 mm in inside diameter and 10 cm to 25 cm in length. Jujube Acid-insoluble Ash Not more than 2.01 mo1/L hydrochloric acid TS to make exactly 100 mL and use this solution as the standard solution. System suitability System performance: Dissolve l mg each of Emetine Hydrochloride RS and cephaeline hydrofluoric acid in 10 mL of 0. External surface is dark grayish brown. P2O5. add 0. The powder irritates the mucous membrane of the nose.971 × TE × 0. and the cortex on the fractured surface is grayish brown.5 mL of hydrochloric acid. Richard or Cephaelis acuminate Karsten (Rubiaceae). shake for 15 minutes. Identification Weigh 0.5%. Description Jujube is the fruit. add 2.61)]. Flow rate: Adjust the flow rate so that the retention time of emetine is about 14 minute.5 g of pulverized Ipecac. add 30 mL of 0. Zizyphi Fructus Assay Weigh accurately about 0. packed with octadecylsilyl silica gel for Liquid Chromatography (5 μm to 10 μm in particle diameter). mostly twisted and sometimes branched. Ipecac Ipecacuanhae Radix et Rhizome Ipecac is the root and rhizome of Cephaelis ipecacuanha A. Parenchyma cells are filled with starch grains and sometimes with raphides of calcium oxalate. In the xylem.0%. in a glass-stoppered centrifuge tube. hoonensis T. cortex is easily separable from the xylem. centrifuge and separate the supernatant liquid.5%. ATE and ATC.0%. siccator (under reduced below 0.0 with acetic anhydride and add 500 mL of methanol. ASE. of emetine in the standard solution. When root is fractured. B. ellipsoidal or broad ovoid. Repeat this procedure twice with the residue using 30 mL volumes of 0.01 mol/L hydrochloric acid TS.64) and cephaeline (C28H38N2O4: 466. previously dried in a de- Jujube is the ripe fruit of Zizyphus jujuba Miller var. Collect the filtrate into an evaporation dish and add small pieces of chlorinated lime: circumference turns red. Ash Not more than 5. sclerenchyma cells are absent. System repeatability: When the test is repeated 6 times with the standard solution under the above operating conditions: the relative standard deviation of the peak area of emetine is not more than 1. and about one-ninth of radius in unthickened part. Ipecac has slight odor and the taste is slightly bitter and unpleasant.5 mg of pulverized Ipecac. Ipecac contains not less than 2.868 A SE Operating conditions Detector: An ultraviolet absorption photometer (wavelength: 283 nm). Perform the test with this solution under the above operating conditions. and the xylem is pale brown. respectively. Pipet 10 μL of the test solution and the standard solution and perform the test as directed under the Liquid Chromatography according to the following operating conditions. of emetine and cephaeline. Combine all the extracts. a transverse section of Ipecac reveals a cork layer. In the cortex. 30 cm to 60 cm in length and about 2 mm in diameter. Spot 5 μL of the test solution on a plate of silica gel for thin-layer chromatography. translucent membranous pericarp is visible. Add 1 mL of sulfuric acid to 2 mL of the filtrate: a reddish purple color develops at the zone of contact and a green color at the upper layer.3%. Description Kalopanax Bark is the long plate or semitubular bark. flattened and thin longitudinal wrinkles. add 10 mL of water. branched. External surface is grayish green to pale brown with five membranous winglets. transverse section reveals numerous fine pits and loose and light fractured surface like sponge. When the perianth stripped. 3 mm to 10 mm in height. Kochia Fruit Loss on Drying Not more than 3. transverse section reveals that the whole consists of aerenchymas. fusiform and divided into two loculi containing flat and ovoid seeds. sometimes with acute cornical and reddish brown to brown thorn. add 20 mL of ethanol and 1. Lacuna of cells forms in triangular or quadrilateral shape. Loss on Drying Not more than 9. Purity foreign matter—The amount of cork layer and other foreign matter contained in kalopanax bark is not more than 1. Ash Not more than 1. add 100 mL of methanol. 1 mm to 3 mm in diameter. Identification Weigh 0. A fractured surface is yellow to yellowish and fibrous. ellipsoidal and grayish yellow scars of thorn. Spray evenly the plate with sulfonic acid for spray and heat at 105 o C for 10 minutes: spot of the Rf value about 0. Ash Not more than 3. transfer the filtrate to a separatory funnel and extract with 20 mL of petroleum ether.0% Ash Not more than 10. Under a microscope. about 1 mm in length. and 1 mm to 3 mm in thickness. pointed fruit stalk scar and 5 to 10 radial veins. Perform the test with the test solution as directed under the Thin-layer Chromatography. Juncus Medulla Junci Medulla Juncus Medulla is the stem pith of Juncus effusus Linné (Juncaceae). External surface is grayish brown to reddish brown. surrounded by a persistent perianth. The seed is flattened ovoid. dark grayish brown spongy. black. flattened on touching. Develop the plate with a mixture of cyclohexane and ethyl acetate (10 : 7) to a distance of about 10 cm and air-dry the plate. External surface is white to pale yellowish white. Purity Rancidity—Jujube has no unpleasant. soft and adhesive. Wash the residue with 2 mL of ether.5 is purple. Evaporate the ether layer to dryness. filter and evaporate the filtrate to dryness. Description Kochia Fruit is oblate. rancid odor and taste. Concentrate to about 5 mL of the filtrate in vaccum. heat under a reflux condenser in a water bath for 1 hour. Kalopanax Bark Kalopanacis Cortex Kalopanax Bark is the bark of Kalopanax pictus Nakai (Araliaceae). add 5 mL of acetic anhydride. slenderly cylindrical. The center of dorsal surface has a slightly prominent. Kochia Fruit has slightly characteristic odor and slightly bitter taste.5 mL of hydrochloric acid. shake for 5 minutes and filter.0% Extract Content Dilute ethanol-soluble extract— Not less than 8.5 g of pulverized kalopanax bark. Description Juncus Medulla is the stem pith. Juncus Medulla is nearly odorless and taste is weak. with irregular longitudinal wrinkles. heat on a water bath for 1 hour under a reflux condenser and filter. five-pointed star shape fruit. use this solution as the test solution. Endocarp is extremely hard. dissolve the residue to 2 mL of ethanol and use the solution as the .0% Kochiae Fructus Kochiae Fruit is the well ripe fruit of Kochia scoparia Schrader (Chenopodiaceae). Under a magnifying glass. dissolve it in 1 mL of anhydrous ethanol. Mesocarp is thick. 1 cm to 3 cm in width.KP VIII 1051 leather.0%. and has slightly bitter and acrid taste.0%. Jujube has characteristic odor and sweet taste. Kalopanax Bark is odorless. with fine longitudinal wrinkles. Identification Weigh 2 g of pulverized Kochia Fruit. Each cells is nearly quadrilateral or rectangle.0% Identification Weigh 1 g of pulverized Juncus Medulla. 5 cm to 30 cm in length. Inner part of kalopanax bark is yellow to yellowish brown. Licorice contains not less than 2. Description 1) Glycyrrhiza uralensis. air dry. Extract Content Dilute tract⎯Not less than 8. and filter. and the lower surface is pubescent and grayish-green. One spot among several spots from the test solution and the spot from the standard solution show the same color and the same Rf value. irregular as being sparse or dense. the transverse section reveals severa1 layers of yellow-brown cork layers and 1 to 3 cellular layer of cork cortex inside the cork layer. weigh 5 mg of Oleanolic acid RS. Licorice has slight characteristic odor and sweet tastes.0%. bitter taste and astringent.0%. Spot 10 μL of test solution and the standard solution of Leonurus Herb RMPM on the plate of silica gel for thin-layer chromatography.93) and 1. dents.0% (6 hours). Place a drop of the filtrate to a filter paper. Under a microscope. Deve1op the plate with a mixture of chloroform and methnol (40 : 1) to a distance of about 10 cm and air-dry the plate. Spray 10 % solution of phosphomolybdic acid and heat the plate at 105 o C for 10 minutes. Spot 2 μL each of the test solution and the standard solution on a plate of silica gel for thin-layer chromatography. . and water (4 : 1 : 0. Leonurus Herb rus Herb RMPM.5% of glycyrrhizic acid (C42H62 O16: 822. Loss on Drying Not more than 13. add 30 mL of methanol. The vessels accompanied with xylem fibers surrounded by crystal cells and with xylem parenchyma cells: The parenchymatous pith is only in Licorice originated from rhizome. Transverse section is fibrous and yellowish white. Perform the test with the test solution and the standard solution as directed under the Thinlayer Chromatography. sonicate for 1 hour. Flowers are pubescent verticillatelly on axil. Loss on Drying Not more than 10. and heat for 20 minutes and filter.0% Extract Content Dilute ethanol-soluble extract— Not less than 15. The vessels are large radiated in medullary rays. with distinct rings of cambium.5) to a distance of about 10 cm and air-dry the plate. Add 1 mL of hydrochloric acid to the filtrate. Part II test solution. much powdery. warm for 2 minutes in a water-bath and filter. The rhizome is cylindrical with externally bud scars. with distinct longitudinally wrinkles. ethanol–soluble ex- Licorice Glycyrrhizae Radix et Rhizoma Leonuri Herba Leonurus Herb is the aerial part collected before or when flowering of Leonurus japonicus Houttuyn (Labiatae).39). evaporate to dryness. Ash Not more than 10. of Glycyrrhiza uralensis Fisher. lenticels and root hair scars. Develop the plate with a mixture of buthanol. formic acid. Description Leonurus Herb is the aerial part. Texture is hard. 1 mm to 5 mm in diameter. The root is cylindrical pieces. respectively. The cortex exhibits groups of phloem fibers with thick but incompletely lignified walls and surrounded by crystal cells. External surface is red-brown to grayish brown. add 5 mL of ethanol and use this solution as the standard solution.0% Acid-insoluble Ash Not more than 5. 25 cm to 100 cm in length and 5 mm to 35 mm in diameter. calyx is tubular. (Leguminosae).0%.Licorice from Glycyrrhiza uralensis consists of the root and rhizome. Separately. Leonurus Herb has characteristic odor. covered with white and short hairs. yellowish green-greenish brown. Peeled Licorice sometimes lacks periderm and a part of phloem. usually 5-lobed at the apex and pale green to greenish brown. Petal is pale reddish purple to brown. calculated on the dried basis. 2) Weigh 3 g each of pulverized Leonurus Herb and Leonurus Herb RMPM. add 2 mL of water to the residue. Identification 1) Weigh 5 g of pulverized Leonurus Herb. Stems are 30 cm to 60 cm in length. White huge pith is in fractured surface of the stem and texture is pliable. spray Dragendorff’s TS and allow to stand: a yellowish red color develops.0%. Glycyrrhiza glabra Linné or Glycyrrhiza inflate Batal. Use the filtrates as the test solution and the standard solution of Leonu- Licorice is the root and rhizome with or without the periderm. Perform the test with the test solution and the standard solution of Leonurus Herb RMPM as directed under Thin-layer Chromatography. Acid-insoluble Ash Not more than 2. the several spots from the test solution and the spots from the standard solution of Leonurus Herb RMPM show the same color and the same Rf value. Medullary rays are radiated and often have clefts. palmately ternate to lobed-ternate. and the center of the transverse section has pith. extract with a reflux condenser. Leaves are opposite.0% Ash Not more than 10.0% of liquiritin (C21H22O9: 418. composed of square stems and cauline leaves and flowers. The parenchyma cells contain starch grains and often solitary crystals of calcium oxalate. the upper surface is pale-yellow. Spray the dilute iodide-bismuth potassium TS to the plate.1052 Monographs. add 40 mL of methanol. Column temperature: A room temperature. Amount (mg) of glycyrrhiz ic acid (C 42 H 62 O 16 ) = amount (mg) of Glycyrrhiz ic Acid RS. Combine all the filtrates. Separately. 2) Liquiritin Weigh accurately about 0. Column: A stainless steel column. filter and use the filtrate as the test solution. prepared in the same manner as Glycyrrhizic acid. The external peel is not coarse. Mobile phase: A mixture of dilute acetic acid (1 in 15) and acetonitrile (3 : 2). Loss on Drying Not more than 12.0% (6 hours).0%. Determine the peak areas. Determine the peak areas. formic acid and acetic anhydride (15 : 2 : 1 : 1) to a distance of about 10 cm and air-dry the plate. Separately. sonicate for 1 hour and filtrate. and use a solution. of the test solution and the standard solution. System repeatability: When the test is repeated six times with the standard solution under the above operating conditions: the relative standard deviation of the peak area of glycyrrhizic acid is not more than 1. Separately.5 g of pulverized Licorice.0 mL/min. AT and AS. packed with octadecylsilyl silica gel for liquid chromatography (5 μm to 10 μm in particle diameter). Detector: An ultraviolet absorption photometer (wavelength: 254 nm). Use a column giving elution of glycyrrhizic acid and propyl parahydroxybenzoate in this order and clearly dividing each peak. add 10 mL of methanol. of the test solution and the standard solution. and its xylem is thick.0%. Flow rate: 1. dissolve in 70% ethanol to make exactly 100 mL and use this solution as the standard solution. Proceed with 20 μL of this solution under the above operating conditions. Flow rate: Adjust the flow rate so that the retention time of glycyrrhizic acid is about 10 minutes. add 70% ethanol to make exactly 100 mL and use this solution as the test solution. The lenticel is slender and not distinct. respectively. Column temperature: A room temperature. sonicate for 5 minutes. Ash Not more than 7. Mobile phase: A mixture of acetonitrile and 0. calculated on the anhydrous basis × AT AS Operating conditions Detector: An ultraviolet absorption photometer (wavelength: 276 nm).KP VIII 1053 2) Glycyrrhiza glabra-Licorice from Glycyrrhiza glabra Linné consists the root and rhizome.5%. add 30 mL of 70% ethanol and proceed in the same manner. Spot 2 μL each of the test solution and the standard solutions on a plate of silica gel with fluorescent indicator for thinlayer chromatography. Pipet 20 μL each of the test solution and the standard solution and perform the test as directed under the Liquid Chromatography according to the following operating conditions. 3) Glycyrrhiza inflate-Licorice from Glycyrrhiza inflate Batal. To the residue. and its texture is relatively firm and sometimes branched.5 g of pulverized Licorice. AT and AS. weigh accurately about 20 mg of Glycyrrhizic Acid RS (separately determined the water content). packed with octadecylsilyl silica gel for liquid chromatography (5 μm to 10 μm in particle diameter). The rhizome has many irregular buds and thick. dissolve in 70% ethanol to make exactly 100 mL and use this solution as the standard solution. Perform the test with the test solution and the standard solutions as directed under the Thin-layer Chromatography. Assay 1) Glycyrrhizic Acid Weigh accurately about 0. weigh each 5 mg of Glycyrrhizic Acid RS and Liquiritin RS. about 4 mm to 6 mm in inside diameter and l5 cm to 25 cm in length. Identification Weigh 2 g of pulverized Licorice. Pipet 20 μL each of the test solution and the standard solution and perform the test as directed under the Liquid Chromatography according to the following operating conditions. about 4 mm to 6 mm in inside diameter and l5 cm to 25 cm in length. as the test solution. consists the root and rhizome. respectively. The texture is tough and hard and have many woody fibers with little powdery. Acid-insoluble Ash Not more than 2. System suitability System performance: Dissolve 5 mg of Liquiritin RS and l mg of propyl parahydroxybenzoate in 70% ethanol to make 20 mL. System suitability System performance: Dissolve 5 mg of Glycyrrhizic Acid RS and l mg of propyl parahydroxybenzoate in 70% ethanol to make 20 mL. Column: A stainless steel column. water. largely grayish brown. weigh accurately about 10 mg of Liquiritin RS (separately determined the water content). Develop the plate with a mixture of ethyl acetate. add 40 mL of 70% ethanol. Examine under ultraviolet light (main wavelength: 254 nm): two spot among the several spots from the test solution and spots from the standard solution (1) and (2) show the same colors and the same Rf values. dissolve each in 1 mL of methanol and use these solutions as standard solutions (1) and (2). hard and sometimes branched. Proceed with 20 μL of this solution under the above operating conditions. Use a column giving elution of liquiritin and propyl parahydroxyben- . A calculated on the anhydrous basis × T AS Operating conditions Amount (mg) of liquiritin (C 21 H 22 O 9 ) = amount (mg) of Liquiritin RS.5% acetic acid (1 : 4). lustrous like shell. add dilute ethanol to make exactly 100 mL and use this solution as the test solution.1054 Monographs. Identification Weigh 0.0 g of Licorice Extract in 18ml of water and filter. A calculated on the anhydrous basis × T AS Packaging and Storage containers. Purity (1) Water-insoluble substances⎯Boil 5. centrifuge and use the supernatant liquid as the test solution. rods. Separately. Proceed as directed in the Assay under Licorice. cool.0 g of pulverized Crude Licorice Extract with 100 mL of water. Proceed as directed in the Identification under Licorice. Filter and evaporate the filtrate to a viscous extract. Filter the digested solution through a cloth filter. digest again for 12 hours and filter through a cloth filter. the fractured surface is dark yellow-red. centrifuge and use the supernatant liquid as the test solution. add 5 L of water or purified water and digest for 2 days. Crude Licorice Extract is brittle when colded. filter the mixture through tared filter paper. Licorice Extract Licorice Extract contains not less than 4. dissolve in dilute ethanol to make exactly 100 mL and use this solution as the standard solution. (C42H62O16: 822. Description Licorice Extract is brown to blackish brown. After cooling. Part II zoate in this order and clearly dividing each peak. or with a slight turbidity. add 20 mL of dilute ethanol and proceed in the same manner. wash with water and dry the residue at 105 o C for 5 hours: the residue is not more than 1. forming a clear solution. Purity Water-insoluble substances matter—Dissolve 2. Crude Licorice Extract has characteristic odor and sweet taste. Crude Licorice Extract Crude Licorice Extract contains not less than 6. After cooling. Amount (mg) of glycyrrhiz ic acid (C 42 H 62 O 16 ) = amount (mg) of Glycyrrhiz ic Acid RS. or masses. Evaporate the combined filtrates until the whole volume becomes 3000 mL. centrifuge and separate the supernatant liquid. To the residue. After cooling.5% of glycyrrhizic acid.0% of glycyrrhiza acid (C42H62O16: 822. Add 3 L of Water or Purified Water to the residue. dark yellow-red to blackish brown plates. Combine the extracts.5%.94). System repeatability: When the test is repeated six times with the standard solution under the above operating conditions: the relative standard deviation of the peak area of liquiritin is not more than 1. Proceed as directed in the Identification under Licorice.0% (1 g. Assay Weigh accurately about 0. Description Crude Licorice Extract is lustrous. add water to make 20 mL.8 g of Licorice Extract. To 10 mL of the filtrate.25 g.15 g of Licorice Extract.93). add 5 mL of ethanol: the solution is clear.6 g of Crude Licorice Extract add 10 mL of a mixture of ethanol and water (7 : 3). Identification Weigh 0. dissolve by warming if necessary. place in a glass-stoppered. Crude Licorice Extract soften when warmed. Assay Weigh accurately about 0. Examine the soluble substance on the filter paper under a microscope: the residue contains no starch grains. Crude Licorice Extract dissolves in water with turbidity. shake for 2 minitues. proceed as directed in the Ash under Crude Drugs Test).15 g of Crude Licorice Extract and proceed as directed in the Assay under Licorice Extract. filter the solution under pressure and evaporate the filtrate. viscous extract and has characteristic odor and sweet taste. add 1 L of ethanol and allow to stand in a cold place for 2 days. A calculated on the anhydrous basis × T AS Packaging and Storage Preserve in tight containers. Method of preparation Weigh 1 kg of fine cutting licorice. shake the mixture thoroughly and filter. Licorice Extract dissolves in water. Method of preparation Boil coarse powder of Licorice with Water or Purified Water. weigh accurately about 20 mg of Glycyrrhizic Acid RS (previously determined the water content). (3) Starch⎯Weigh about 1 g or pulverized Crude Licorice Extract. (2) Foreign matter⎯The filtrate obtained in (1) does dot have strong bitter taste. Ash Not more than 12. add 10ml of a mixture of ethanol and water (7 : 3). add 25 mL of dilute ethanol and heat at 50 o C for 30 minute with occasional shaking. Preserved in well-closed . centrifuge tube. Amount (mg) of glycyrrhiz ic acid (C 42 H 62 O 16 ) = amount (mg) of Glycyrrhiz ic Acid RS. Liriope Tuber from Liriope platyphylla consists of tuber. Transfer the filtrate into the separatory funnel. with the shape of long rectangle or round rectangle. simple starch grains. and allow to stand for 1 hour with occasional shaking. slightly semi-translucent and viscous. (2) Ophiopogon japonicus . Extract Content Dilute ethanol-soluble extract— Not less than 7. Protoxylem is observed in upper part of vessles and between the vessels are rarely fibers. vessels. bigger than epidermal cells. Extract Content than 30. add 1 to 2 drops of Mayer TS: the solution develops an opalescence. Description Linseed is the seed. flattened. Loss on Drying Not more than 14. transverse section appears epidermis. with lateral wrinkles and with scattering scars of rootlets. Cortex is relatively broade. Purity Foreign matter—Not more than 2. Liriope Tuber has slightly characteristic odor and slightly sweet taste and is hygroscopic.KP VIII 1055 Lindera Root Linderae Radix Lindera Root is the root of Lindera strychnifolia Fernandez-Villar (Lauraceae). Lindera Root has camphor-like odor. Description (1) Liriope platyphylla . Inside of cotyledons and endosperms reveals fatty oils and aleurone grains. 10 to 25 mm in diameter. Under a microscope. somewhat sharp at one end and somewhat rounded at the other. The fractured surface is pulverized. two thin-walled cell layers in middle layer. External surface is yellowish brown to brown. Exodermal cells are lined in 1 to 2 rows. with thin and small pillar in the center. Under microscope. and allow to stand after shaking well. fusiform. slightly horny. is difficult to break. cool and slightly bitter taste. rectangular or polygonal. a transverse section reveals brown. Ether-soluble extract—Not less Liriope Tuber Liriopis Tuber Liriope Tuber is the tuber of the Liriope platyphylla Wang et Tang or Ophiopogon japonicus Ker-Gawler (Liliaceae).Liriope Tuber from Ophiopogon japonicus is the tuber. Cortex parenchyma contains columnar crystals .0%. 1 to 15 μm in diameter and starch grains. is hard and dense in texture. Outer layer of endodermis has 1 to 3 rows of stone cells. In xylem. a transverse section reveals a cork layer consisting of partially cork stone cells and parenchyma cells is composed of oil cells and fibers. External surface is pale yellow to pale yellowbrown. Ash Not more than 5. xylem fibers and rays are arranged alternately.7 mm in thickness. fibrous cell layer and pigment cells containing reddish-brown ingredients in inner layer. Collenchymas are 810. Linseed has soft taste.0%. 10 mm to 25 mm in length and 3 mm to 5 mm in diameter.5%. wrinkled longitudinally. After cutting. Description Lindera Root is the fusiform of rosarylike root. 8 μm to 15 μm in diameter. Under a microscope. 2 to 4 compound.5 mm to 0. External surface is dark brown and lustrous.0%. Linseed is odorless. with 1 line of cells. External surface is pale yellow. and about 20 protoxylems are present in actiostele. 12 mm to 40 mm in length and 4 mm to 9 mm in diameter. but starch grains are not observed. with longitudinal wrinkles of various sizes. Linseed are muciliginous when moistened. oily and slippery but not rancid.0%. Endodermis is distinct. ovate and obliquely pointed at one end. cortex is flexible and friable. with inside and side wall thickened. add 10 mL of chloroform and 1 mL of ammonia TS. the transverse section shows outer membrane containing mucilage in outer layer. Linseed Lini Semen Linseed is the ripe seed of Linum usitatissimum Linné (Linaceae). Under a microscope. easy to broken. 4 to 5 layer exodermis inside the velamen and cortex of parenchyma cells inside the exodermis. and stele is strong and rough.0% (6 hours) Ash Not more than 2. Under a magnifying glass. Identification (1) Weigh 1 g of pulverized Lindera Root. It is about 4 mm to 6 mm in length and 2 mm to 3 mm in width and 0. thin membranous endosperm and 2 large cotyledons are observed. lignified. Inside of Linseed. Pipet the water layer. with needle raphides inside. Lindera Root. Fractured surface is nealy white. 10 to 15 cm in length. Parenchyma cells of cortex and xylem contain sandy and columnar crystals of calcium oxalate. Fractured surface of cortex is pale yellow-brown. slightly curved and bead-threaded shpae. a transverse section reveals brown to light yellowish brown and concentric circles and radially arranged lines brown. add 2 mL of dilute hydrochloric acid. Liriope Tuber has slightly characteristic odor and slightly sweet and mucous taste. with longitudinally fine wrinkles. Lithospermum Root from Arnebia euchroma has characteristic odor and slight bitter and astringent tastes. 7 cm to 20 cm in length and 10 mm to 25 mm in diameter. 6 cm to 10 cm in length and 5 mm to 15 mm in diameter. . To 3 mL of filtrate. heat in a test tube: red vapor evolves. Arnebia euchroma Johnst. normally ten layers overlapped and easily peeled off. a transverse section reveals clear surface.5 g of pieces or powder of Lithospermum Root.Lithospermum Root from Lithospermum erythrorhizon is rather slender conical root. shake for 30 minutes. Perform the test with the test solution as directed under the Thin-layer Chromatography. filter. a transverse surface reveals uneven surface and relatively small. Txture is hard. External surface is reddish purple or dark purple. Develop the plate with a mixture of ethyl acetate and ethanol (3 : l) to a distance of about 10 cm and airdry the plate: the spot of the Rf value about 0. the other surface is lustrous. Purity Rootlets—Less than 1. Sometimes remains of stem are present at the crown. yellowish white to yellow xylem. Lithospermum Root has slight characteristic odor and slight sweet taste. yellowish brown. Ash Not more than 11. Longan Arillus Longan Arillus Longan Arillus is the arill of Dimorcarpus longan Loureiro (Sapindaceae). Not more than 15. Identification (1) Weigh 0. (2) Weigh 0. Lithospermum Root is mostly with twisted and deep longitudinal furrows which sometimes reach to xylem. and Arnebia guttata Bunge (Boraginaceae). reddish purple cortex and slightly small and yellowish white xylem.0% (60 °C. almost twisted. Lithospermum Root Lithospermi Radix Lithospermum Root is the root of Lithospermum erythrorhizon Siebold et Zuccarini. Fractured surface is granular and with many clefts. 6 Ash Not more than 5. Under a magnifying glass. Part II and needle raphides of calcium oxalate. Longan Arillus has slight characteristic odor and sweet taste. add l to 2 drops of dilute hydrochloric acid: the color turns red again. External surface is dark purple to purple-brown.0%. To this solution. evaporate in vaccum at not more than 40 °C. External surface is reddish purple to purple-brown and lax. which condenses on the wall of the upper part of the tube into red-brown oil drops. Texture is lax. Description Longan Arillus is longitudinally broken and irregular thin slices. and xylem is yellow. (2) Arnebia euchroma-Lithospermum Root from Arnebia euchroma is irregular cylindrical root. Acid-insoluble Ash Not more than 3. a transverse section reveals a dark purple color at the outer volume of cortex and pale brown inner volume making irregular wave. Lithospermum Root from Arnebia guttata has characteristic odor and astringent taste.5 g of pulverized Lithospemum Root. shake well and filter. soft and light. cylindrical and twisted root. Identification Weigh 1 g of Longan Arillus. Under a magnifying glass. often branched. When soaked in water. frequently several slices agglutinated. slightly thin. (3) Arnebia guttata-Lithospermum Root from Arnebia guttata is conical. fleshy texture.1056 Monographs. thin and easily peeled. fragile and easily broken. add 5mL of ethanol. The center of the crown is often cracked and the surrounding part is red-purple. Spot 5 μL of the test solution on a plate of silica gel for thin-layer chromatography. Texture is soft and sticky. 2 to 4 cm in length and 1 cm to 2 cm in width and 2 mm to 4 mm in thickness. bar-shaped. add l mL of ethanol and to the red solution thereby obtained. Longan Arillus becomes a petal shape composed of 3 to 4 pieces. Oil drops are present in the exodermis. One surface is shrunkened. add 3 mL of Fehling TS and warm in a water-bath: a red precipitate is produced. Loss on Drying hours). Lithospermum Root is easily broken. Apex sometimes bears branched remains of stems. Under a magnifying glass.0%.0%. add l drop of sodium hydroxide TS: the red color changes to blue-purple. add 10 mL of water.0%. Ash Not more than 3. and cortex is coarse. Description (1) Lithospermum erythrorhizon.75 is reddish purple. External surface is dark reddish brown to blackish brown and semitransluscent. then add 1 mL of ethanol and use this solution as the test solution.5 g of pulverized Lithospermum Root. 6 cm to 20 cm in length. (3) Weigh 0. Crown is slightly large and apex bears one or more remains of a stem covered with short and stiff hairs. 15 mm to 40 mm in diameter..5%. normally several layers overlapped and easily peeled off. has characteristic odor.1 g of magnesium and 2 to 3 drops of hydrochloric acid to the filtrate: a pale brown to reddish brown color develops. occasionally cylindrical masses as the ossified bone of large mammal. Under a microscope. and parenchymatous cells . To 25 mL of the filtrate. and the lower surface is pale grayish green. externally grayish yellowish brown to purplish brown. add 5 mL of water. Loss on Drying Not more than 15. Description Longgu is irregular masses or fragments. add carefully 6 mL of hydrochloric acid and evaporate on a waterbath to dryness. 3 cm to 7 cm in length. and the inner part consists of pale brown porous volume. 1 cm to 3 cm in width. It is 15 mm to 35 mm in length and about 3 mm in diameter in upper part and 1. a transverse section of leaf reveals the outer surfaces to be composed of a single-layered epidermis. (2) The turbid solution. but somewhat fragile. Pass the gas evolved through calcium hydroxide TS: a white precipitate is produced. Add 1 to 2 drops of ferric chloride TS to the filtrate: a purple color develops. Several-layered collenchyma is beneath the epidermis and vascular bundles in the center in midvein. External surface is pale grayish white.0%. Glandular hairs contain brown secretion. and a spongy tissue is adjacent to lower epidermis in mesophyll. Lonicera Leaf and Stem Lonicerae Folium et Caulis Lonicera Leaf and Stem is the leaves and climbing stems of Lonicera japonica Thunberg (Caprifoliaceae). Filter this solution and neutralize with ammonia TS: the solution responds to the Qualitative Tests for calcium salt. heat for 2 minutes in a water-bath and filter. add 2 mL of dilute acetic acid and 2. The stem is 1 mm to 4 mm in diameter. Lonicera Flower has characteristic odor and weak and slightly bitter taste. 5-lobed at the apex. Description Lonicera Flower is the flower bud or the flower starting to bloom and the mixture of small clavate to conical flower bud and lip-shaped flower.0%. Longgu is odorless. shake to mix. Ash Not more than 9. (3) Weigh 0.KP VIII 1057 Longgu Fossila Ossis Mastodi Longgu is the ossified bone of large mammal and is mainly composed of calcium carbonate. lobes are pubescent. Under a magnifying glass. both surfaces are pubescent. dissolve in 10 mL of dilute hydrochloric acid: it evolves a gas and forms slightly brown and turbid solution. Description Lonicera Leaf and Stem is the leaves and climbing stems.5 g of pulverized Longgu. Prepare the control solution as follows: evaporate 3 mL of hydrochloric acid on a water–bath to dryness.5 mm in diameter in lower part. External surface is yellowish-white or greenish-white. The calyx is green. uni-cellular nonglandular hairs and multicellular glandular hairs on epidermis. Numbers of stamens are 5. When crushed. The upper surface is greenish brown. The texture is heavy and hard. with short petiole. it changes into pieces and powder. Purity (1) Heavy metals—Weigh 2 g of pulverized Longgu.0%. pale brownish hair is densely pubescent.2 g of pulverized Longgu according to Method 2 and perform the test (not more than 10 ppm). The outer part consists of a layer 2 mm to 10 mm in thickness and is dense in texture. Perform the test. about 2 mm in length. Identification (1) Weigh 0. dissolve in 5 mL of nitric acid by warming and add ammonium molybdate TS: a yellow precipitate is produced. Add 0. Purity Stems and leaves—Less than 5. obtained in (1). A palisade layer is adjacent to upper epidermis. gradually darken on keeping. add 2 mL of dilute acetic acid. Under a magnifying glass.5 g of pulverized Lonicera Flower. tasteless and strongly adhesive to the tongue on licking. heat and filter.0% (6 hours). pistil 1. (2) Weigh 2. sometimes with grayish black or yellow-brown spots here and there. The leaves is round and entire. 1 drop of ammonia TS and water to make 50 mL. Extract Content Dilute ethanol-soluble extract— Not less than 16.0 g of pulverized Lonicera Flower.0 mL of standard lead solution and add water to make 50 mL (not more than 20 ppm). Lonicera Flower Lonicerae Flos Lonicera Flower is the flower bud or the flower starting to bloom of Lonicera japonica Thunberg (Caprifoliaceae). add 10 mL of ethanol. and a transverse section of stem is round and hollow. add 10 mL of water. ovary glabrous. Identification (1) Weigh 0. Dissolve the residue in 50 mL of water and filter. (2) Arsenic—Prepare the test solution with 0.1 g of pulverized Longgu. Flow rate: 1. Extract Content Dilute ethanol-soluble extract— Not less than 12. Combine all filtrates. soft and tender. of betaine of the test solution and the standard solution. shake well. add 3 drops of ninhydrin solution (1 in 2). cool and. The concentrated solution is loaded on to column II and eluted with 10 mL of deionized water. add 50 mL of diluted methanol (1 in 2). add 2 drops of sodium hydroxide solution (1 in 10). contains not less than 0. Ash Not more than 9. Loss on Drying Not more than 12. and add 0. add 20 mL of dilute ethanol. fruit stalk and other foreign matter. packed with dimethylaminopropylsilylated silica ge1 (5 µm to 10 µm in particle diameter). a transverse surface reveals thin Assay Weigh accurately about 1. The eluate is collected and concentrated to 5 mL in vaccum. nearly flat. 20 to 50 Seeds are present inside. 5 mm to 15 mm in width and 1 mm to 3 mm in thickness. Lonicera Leaf and Stem has almost odorless and slightly astringent.0%. Repeat the above procedure with the residue using 50 mL of diluted methanol (1 in 2). about 2 mm in length and 1 mm to 2 mm in width. (2) Take 1 mL of the filtrate. 6 cm to 20 cm in length and 3 mm to 10 mm in diameter.5% of copper sulfate solution: a purple color develops.0 mL/minute. Perform the following tests using the filtrate as the test solution. packed 5 cm high with 1:2 ratio of cationic ion-exchange resin (H+ form) and strong basic anionic ion-exchange resin (OH.0 g of pulverized Lycium Fruit. with a scar of pistil stalk like small projection at the end and a scar of fruit stalk on the base. 3 cm to 10 cm in length. Column I: A glass tube 10 mm to 12 mm in inside diameter and 10 cm in length. and occasionally starch grains. heat under a reflux condenser in a water-bath for 2 hours and filter. Seed is kidney-shaped. packed 5 cm high with strong cationic ion-exchange resin (H+ form). filter. Part II contain aggregate crystals of calcium oxalate. Dissolve the residue in 1.0 with dilute hydrogen chloride. External surface is red to dark red. The eluate is combined and evaporated to dryness. External surface of seed is pale yellow or yellowish brown.form). Mobile phase: A mixture of acetonitrile and water (85 : 15). not fibrous. tough and crumpled. Separately. AT and AS. Lycium Root Bark is the rhizome of Lycium chinense Miller or Lycium barbarum Linné (Solanaceae). Lycium Fruit. Under a microscope. add .5% of betain (C5H11NO2: 117. Purity Stems—Lonicera Leaf and Stem does not contains the stems larger than 5 mm in diameter. followed by bitter taste. Pericarp is soft. dissolve in 1 mL of water and use this solution as the standard solution.0%. shake well and heat for 5 minutes: a purple color develops. weigh accurately about 10 mg of Betaine RS. Sarcocarp is pulpy. successively. Identification Weigh 1 g of pulverized Lycium Fruit. Column temperature: A room temperature. A fractured section is grayish white to yellowish brown.15). 30 mL of deionized water to the residue and adjust pH to 3.0%. Load the suspension on to the column I and elute with 60 mL of deionized water and discard it. Description Lycium Fruit is fusiform and sharp at one end. The column is eluted with 15 mL of diluted ammonia TS (2 in 5) and 15 mL of deionized water. External surface is grayish yellow to brownish yellow.1058 Monographs. Column: A stainless steel column. Lycium Root Bark Lycii Cortex Purity Foreign matter—Lycium Fruit contains less than 3. (1) Take 1 mL of the filtrate. respectively.0% (6 hours). Lycium Fruit has slightly odor and sweet taste. Column II: A glass 10 mm to 12 mm in inside diameter and 10 cm in length. when dried. Amount (mg) of betaine (C5 H11 NO2 ) = amount (mg) of Betaine RS × AT AS Operating conditions Detector: An ultraviolet absorption photometer (wavelength: 210 nm). Perform the test with 10 L each of the test solution and the standard solution as directed under the Liquid Chromatography according to the following operating conditions and determine the peak areas. Lycium Fruit Lycii Fructus Lycium Fruit is the dried fruit of Lycium chinense Miller or Lycium barbarum Linné (Solanaceae).0% of branch. 4 mm to 6 mm in inside diameter and 15 cm to 25 cm in length. extract under a reflux condenser for 15 minutes in a water-bath. evaporate to dryness in vaccum. Ash Not more than 6. Description Lycium Root Bark is the quilled to channeled or fragmentary rhizome. respectively.0 mL of water and use this solution as the test solution. slightly even with fine longitudinal striations. Texture is light and coarse. 5 g of pulverized Lycium Root Bark. and bracts and calyx are persistent. yellowish brown. External surface is grayish white to grayish brown and rough. Texture is fragile. Primary cortex is thin.KP VIII 1059 cork cells consisting of several layers of cells. Ash Not more than 6. Magnolia Bark contains not less than 0.33). Spray evenly Dragendorff's TS on the plate: the yellow spot shows in the range of the Rf value of near 0. leaves are lanceolate or oblong. at under a reflux condenser in a water-bath for 20 minutes. before flowering. 2) Weigh 0.3. a fractured section is yellowish white and the center part of pith is hollow. Purity Foreign matter—Not more than 5.0% Extract Content Dilute ethanol-soluble extracts Not less than 20. 2 mm to 6 mm in diameter. Under a microscope. add 10 mL of acetic anhydride.5 g of pulverized Lycium Root Bark. Assay Weigh accurately about 0.0% Acid-insoluble Ash Not more than 2. Magnolia officinalis Rehder et Wilson or Magnolia officinalis Rehder et Wilson var. a green color at the upper layer after allowing to stand. add 10 mL of water. 5 cm to 10 cm in length. 50 cm to 100 cm in length. Phloem fibers are lined step-wise between medullary rays in the secondary cortex and then these tissues show a latticework. Spot 10 μL of the test solution on a plate of silica gel for thin-layer chromatography. heat on a water bath for 2 minutes and filter. Combine the whole filtrates. dry Magnolol RS in a . Fiber groups are scattered in the pericycle. add 10 mL of methanol. 2 mm to 7 mm in thickness.0%. with hairs on both surface. Identification 1) Weigh 0. sometimes cork layer removed and externally red-brown. Add carefully 2 mL of sulfuric acid to 2 mL of the filtrate: a reddish-brown color appears at the zone of contact. Loss on Drying Not more than 10. When leaves are unfolded. but sometimes observed in the narrow medullary rays. Identification Weigh 1 g of pulverized Magnolia Bark. Lycopus Herb Lycopi Herba Lycopus Herb is the aerial part.8% of magnolol (C18H18O2: 266. mostly crumpled and petiole is short. Cut surface is extremely fibrous and it is pale red-brown to purplish brown. Flowers are aggregated in leaf axils in verticillate cymes. Repeat the above procedure with the residue using 40 mL of diluted methanol (7 in 10).0% Acid-insoluble Ash Not more than 3. a transverse section reveals a thick cork layer or several thin cork layers and internally adjoining the circular tissue of stone cells of approximately equal diameter. with white hair at distinct purple nodes. Oil cells are scattered in the primary and secondary cortex. heat on a water bath for 2 to 3 minutes: a purple color appears. and blackish green at the upper surface. Description Lycopus Herb is the fusiform aerial part. with a few braches and with equally shallow longitudinal furrows at the four side of stem. centrifuge and use the supernatant liquid as the test solution. Separately.0%. Apex is acute and margin is serrate.0% of xylem and other foreign matter Loss on Drying Not more than 12. biloba Rehder et Wilson (Magnoliaceae). External surface is yellowish green of purple.0% Ash Not more than 18. grayish green and densely glandular-dotted at the lower surface. Perform the test with this solution as directed under the Thin-layer Chromatography. add diluted methanol (7 in 10) to make exactly 100 mL and use this solution as the test solution. of Lycopus lucidus Turczaininov (Labiatae).0% Ash Not more than 5. 5 μm to 10 μm of starch grains and sometimes sclerenchymatous cells.0% Magnolia Bark Magnoliae Cortex Magnolia Bark is the bark of the trunk of Magnolia obovata Thunberg. Description Magnolia Bark is plate-like or semitubular bark. add 40 mL of diluted methano1 (7 in 10). Develop the plate with a mixture of nbutanol. Magnolia Bark has slight odor and bitter taste.0%. Interior surface is pale brown to dark purplish brown. Leaves are opposite. Lycopus Herb is odorless and has weak taste. parenchymatous cell and fibers containing of sandy crystals of calcium oxalate in cortex. Extract Content Dilute ethanol-soluble extract— Not less than 8. Add 1 mL of ninhydrin TS to 2 mL of the filtrate. corolla is mostly fallen off. cool and filter.5 g of pulverized Magnolia Bark. heat on a water bath for 5 minutes and filter. water and acetic anhydride (4 : 2 : 1) to distance of about 10 cm and air-dry the plate. stir for 10 minutes. Some bark is transversly broken and xylem is exposed. piperascens Malinvaud ex Holmes (Labiatae). Pith in the center consists of paranchymal cells. glandular hairs and scales both surfaces. yellowish brown or yellowish white. 5 mm to 20 mm in diameter. the relative deviation of the peak area of magnolol is not more than 1. Part II desiccator (silica gel) for 1 hour or more. from which the rootlets removed. Under a microscope.4 mL (50. System suitability System performance: Dissolve l mg each of Magnolol RS and Honokiol RS in diluted methanol (7 in 10) to make 10 mL. External surface is grayish yellow or dark gray. Vessels in xylem are scattered single or 2 to 3 in group and xylem fibers are developed. Under a microscope. Xylem is broad. heat on a water . When the procedure is run with 10 μL of this solution under the above operating conditions. consisting of stem with opposite leaves.1060 Monographs. The front surface of leafs is pale brown-yellow to light greenyellow and the back surface is pale green to light green- yellow. with longitudinal wrinkles and transverse cracks. Mentha Herb Menthae Herba Mentha Herb is the aerial part of Mentha arvensis Linné var.0% (6 hours). Weigh accurately about 10 mg. somewhat bented and varying in length. Description Morinda Root is compressed cornical root. Flow rate: Adjust the flow rate so that the retention time of magnolol is about l4 minutes. add 15 mL of dichloromethane. Morinda Root is odorless and has sweet. trasverse section of stem reveals the rectangle of fractured surface. Column: A stainless steel column. 1 mL of silicon resin). slightly astringent. Under a magnifying glass.5%. respectively. Mobile phase: A mixture of water. Identification Take l mL of the mixture of essential oil and xylene. Phloem is narrow with brown secretion in parenchyma.0. Petiole is 3 mm to 10 mm in length. Loss on Drying Not more than 15. Morinda Root is pressed flatly and dried. Identification Weigh 2. dissolve in diluted methanol (7 in 10) to make exactly 100 mL and use this solution as the standard solution. and add carefully 2 mL of sulfuric acid to make two layers: a deep red to red-brown color develops at the zone of contact. acetonitrile and acetic anhydride (50 : 50 : 1). Xylem is hard. Texture is tough. Stem is square. Perform the test with 10 μL each of the test solution and the standard solution as directed under the Liquid Chromatography according to the following operating conditions and determine the peak areas. Purity Foreign matter—The amount of roots and other foreign matter contained in Mentha Herb is less than 2.0%.0 g. obtained in the Essential oil content. leaf reveals hairs. AT and AS. and glandular hairs and scales are many in back surface. Essential Oil Content Not less than 0. System repeatability: When the test is repeated 6 times with the standard solution under the above operating conditions. 4 mm to 6 mm in inside diameter and 15 cm to 25 cm in length. of magnolol for the test solution and the standard solution. When smoothed by immersing in water. Mentha Herb has characteristic aroma and gives a cool feeling on keeping in the mouth.0%. Under a magnifying glass. scales and nonglandular hairs. 1 mm to 5 mm in diameter. with 1 line of vessels radially. Amount (mg) of magnolol (C18H18O2) A = amount (mg) of Magnolol RS × T AS Operating conditions Detector: An ultraviolet absorption photometer (wavelength: 289 nm). Column temperature: A constant temperature of about 20 o C . purple or pale purple and easily separatled from wood. Ash Not more than 11. packed with octadecylsilyl silica gel (5 μm to 10 μm in particle diameter). Several cells of stem contain clustered crystal of calcium oxalate and crystal of menthol. Acid-insoluble Ash Not more than 2. Morinda Root Morindae Radix Morinda Root is the root of Morinda officinalis How (Rubiaceae).5%. Description Mentha Herb is the aerial part. leaf is ovate to oblong. a transverse section reveals stone cells arrange in a ring in the outer part of phellderm and parenchymatous cells contain rhapides of calcium oxalate. cortex is thick. pale brown to red-purple and with fine hairs. 2 cm to 8 cm in length and 10 mm to 25 mm in width and margin irregularly serrated. with acute apex and base.0 g of pulverized Morinda Root. honokiol and magnolol are eluted in this order with a resolution between their peaks being not less than 5. AT and AS. Spray diluted sulfuric acid TS. Moutan Root Bark has characteristic odor and slight pungent and bitter taste. Acid-insoluble Content Not more than 1.17). Perform the test with the test solution as directed under Thin-layer Chromatography.0% of paeonol (C9H10O3: 166. then pipet 10. acetate (1 : 1) to a distance of about 10 cm and air-dry the plate.0%. 4 mm to 6 mm in inside diameter and 15 cm to 25 cm in length. Repeat the above procedure with the residue. dissolve it in l0 mL of methanol and use this solution as the standard solution. Ash Not more than 6. Examine under ultraviolet light (main wavelength: 254 nm): several spots from the test solution and the spots from Moutan Root Bark RMPM standard solution are the same color and the same Rf value. Develop the plate with a mixture of hexane and ethyl acetate (3 : 2) to a distance of about 10 cm and air-dry the plate. with small and transversely elongated ellipsoidal scars of lateral roots and with longitudinal wrinkles. Weigh accurately about 10 mg of it. Column temperature: A constant temperature of about 20 °C. 10 mm to 15 mm in diameter and 2 mm to 6 mm in thickness. using 40 mL of methanol.0 mL of this solution. One of the spots and the spot form the standard solution are the same color and the Rf value. Moutan Root Bark RMPM standard solution and the standard solution as directed under the Thinlayer Chromatography. add 10 mL of hexane. add methanol to make exactly 50 mL and use this solution as the standard solution. acetonitrile and acetic anhydride (65 : 35 : 2). then pipet 10. add methanol to make exactly 25 mL and use this solution as the test solution. When the procedure is run with 10 μL of this solution under the above operating conditions . packed with octadecylsilyl silica ge1 (5 μm to 10 μm in particle diameter). Purity (1) Xylem—Less than 5. System suitability System performance: Dissolve 1 mg of Paeonol RS and 5 mg of butyl paraoxybenzoate in 25 mL of methanol. dry Paeonol RS in a desiccator (calcium chloride for dryness) for more than l hour. Separately. dissolve in methanol to make exactly 100 mL. Inner surface is pale grayish brown to purplish brown and flat. Description Moutan Root Bark is the root bark. dissovle the residue to 1 mL of dichloromethane and use this solution as the test solution. add 40 mL of methanol. when dried. filter and use the filtrate as the test solution or Moutan Root Bark RMPM standard solution.KP VIII 1061 bath for 1 hour under a reflux condenser and filter.0%. tubular to semi-tubular. Ash Not more than 6. respectively.0%. Column: A stainless steel column. Separately. Develop the plate with a mixture of hexane and ethyl Amount (mg) of paeonol (C 9 H 10 O 3 ) = amount (mg) of Paeonol RS × AT 1 × AS 2 Operating conditions Detector: An ultraviolet absorption photometer (wavelength: 274 nm). Evaporate the filtrate to dryness.0% Acid-insoluble Ash Not more than 1. Spot 10 μL of the test solution on a plate of slica gel for thin-layer chromatography. Loss on Drying Not more than 13. Flow rate: Adjust the flow rate so that the retention time of paeonol is about 14 minutes.0%.0% Extract Content Dilute ethanol-soluble extract— Not less than 52. weigh l mg of Paeonol RS. Identification Weigh 2 g each of pulverized Moutan Root Bark or Moutan Root Bark RMPM.3 g of pulverized Moutan Bark.0% Moutan Root Bark Moutan Cortex Moutan Root Bark is the root bark of Paeonia suffruticosa Andrews (Paeoniaceae). On the inner and fractured surfaces white crystals often attached.73 of Rf value. shake for 3 minutes. External surface is dark brown to purplish brown. Fractured surface is coarse. 5 cm to 8 cm in length. of paeonol for the test solution and the standard solution. heat under a reflux condenser in a water-bath for 30 minutes. Combine the whole filtrates. Perform the test with 20 μL each of the test solution and the standard solution as directed under the Liquid Chromatography according to the following operating conditions and determine the peak areas. Moutan Root Bark. cool and filter. contains not less than 1. (2) Foreign matter—The amount of foreign matter other than xylem contained in Moutan Bark is not more than 1.0% Assay Weigh accurately about 0.0%. Perform the test with the test solution. and heat at 105 o C for l0 minutes: a purple spot appears at about 0.0 mL of this solution. Spot 10 μL of the test solution and the standard solution on a plate of silica gel with fluorescent indicator for thin-layer chromatography. Purity xylem—The amount of the xylem contained in Morinda Root is not more than 35. Mobile phase: A mixture of water. add methanol to make exactly 100 mL. 10 mm in diameter and 5 mm in thickness. boil under a reflux condenser in a water–bath for l5 minutes and filter. 2 to 3 cm in length.0% (6 hours). Loss on Drying Not more than 6.53 is purple. Mulberry Root Bark Mori Cotex Mulberry Root Bark is the root bark of Morus alba Linné (Moraceae). Ash Not more than 11. The seed is in the center of the fruit. Mume Fructus has characteristic odor and acidic taste. Description Mulberry Root Bark is the root bark. a transverse section of bark with periderm reveals 5 to l2 layers of cork cells in the outer volume. Evaporate the filtrate to dryness. ethanol-soluble ex- Myrrh Myrrha Myrrh is the gum-resin collected from the Commiphora molmol Engler or Commiphora myrrha Engler (Burseraceae). semi-tubular or banded. simple grain 1 μm to 7 μm in diameter. wrinkled and lusterless. shake for 5 minutes. and the latter Gum Myrrh. arranged alternately and stepwise with phloem parenchyma.0. often in fine lateral cuttings. with numerous longitudinal.5%. heat in a water-bath for 30 minutes.0%. Starch grains occur as spheroidal or ellipsoidal. Extract Content Dilute tract⎯Not less than 27. Identification (1) Weigh 0.0%.1062 Monographs. Description Myrrh is the gum-resin in a shape of ir- . dissolve the residue in 1 mL of ethanol and use this solution as the test solution. dissolve the residue in l0 mL of chloroform.0 g of pulverized Mulberry Root Bark. To the vaporized product. Mulberry Root Bark has lactiferous tubes and solitary crystals of calcium oxalate. Spot 10 μL of the test on a plate of silica gel for thin-layer chromatography.0 % Acid-insoluble Ash Not more than 1. A transverse section of the bark is white to pale brown and fibrous. add 20 mL of hexane.5 mL of the solution with 0. add 2 mL of acetic anhydride. (2) Weigh 1. System repeatability: When the test is repeated 6 times with the standard solution under the above operating conditions. Outer surface is dark to dark brown. Perform the test with the test solution as directed under the Thin-layer Chromatography. in the case of the bark with periderm. add 10 mL of methanol. fine wrinkles and numerous red-purple lenticels laterally elongated. with the resolution between their peaks being not less than 2. External surface is white to yellow-brown. easy to peel. 15 to 20 mm in diameter. Add dilute hydrochloride to the filtrate to acidify. shake well for 5 minutes and filter. Purity Foreign matter—The amount of the root xylem and other foreign matter contained in Mulberry Root Bark is not more than l. paeonol and butyl parahydroxybenzoate are eluted in this order. Ash Not more than 5. Description Mume Fructus is usually the spherical or spheroid fruit. Identification (1) Weigh 1 g of pulverized Mulberry Root Bark. Mulberry Root Bark has characteristic odor and is tasteless. To 1 mL of the filtrate. simple or compound grains.0%. Acid-insoluble Ash Not more than 1. mix 0. 1 mm to 6 mm in thickness. and its periderm is yellowbrown.0 g of pulverized Mume Fructus. 10 minutes: spot of the Rf value about 0. Under a microscope. (2) Weigh 1.0%. Develop the plate with a mixture of cyclohexane and ethyl acetate (3 : 1) to a distance of about 10 cm and air-dry the plate. Inner surface is dark yellow-brown and flat. 10 to 14 mm in length. from which periderm has been removed. the relative deviation of the peak area of paeonol is not more than 1. add water: a white precipitate is produced after adding acetate-lead TS.5%. Evaporate the filtrate to dryness. Phloem fibers or their bundles are scattered in the cortex. Spray evenly diluted sulfuric acid TS and heat at 105 o C for Mume Fruit Mume Fructus Mume Fruit is the unripe fruit of the Prunus mume Siebold et Zuccarini (Rosaceae) and fumed.5 mL of sulfuric acid to make two layers: a reddish-brown color develops at the zone of contact. tubular. Part II and calculate the resolution. Packaging and Storage Preserve in tight containers. The former is known as Gum Opoponax. add 10 mL of water.5 mL of sulfuric acid to form two layers: a reddish brown color develops at the zone of contact and a dark greenish-brown at the upper layer. add gently 0. cool and filter.5 g of pulverized Mume Fructus.5 mL of acetic anhydride in a test tube and add carefully 0. Under a microscope. slightly thick and bead-threaded with pitted space. The filtrate is evaporated to dryness: the residue becomes purplish red when contacted with bromine gas. sometime being removed the embryo. External surface is yellowish brown or reddish brown.KP VIII 1063 regular grain or mass. (2) Shake thoroughly a small quantity of pulverized Nelumbo Seed and some water and add several drops of iodide solution: a bluish-purple color is produced. shake for 5 minutes. add 0. add 10 mL of dilute acetic acid. fractured in irregular shape. yellowish brown and hard to peeled off. Nutmeg Acid-insoluble Ash Not more than 5. (3) Weigh 0. Texture is hard. Extract Content Dilute ethanol–soluble extract— Not less than 12. Purity Ethanol-insoluble substances—Weigh accurately about 2 g of finely pulverized Myrrh. At one end. Starch grains are mostly simple and occasionally 2 to 20 compounds. External surface is pale yellowish brown to reddish brown. 2 cm to 3 cm in length and about 2 cm in diameter.5 g of pulverized Nelumbo Seed. dark brown perisperm. and spicy slightly bitter . Nelumbo Seed is odorless and slightly oily and has sweet taste. and the color abate gradually after heating. Two plump cotyledons are yellowish white with green embryo at the space between two cotyledons. Packaging and Storage Preserve in well-closed containers. vortex and filter.5%. Ethanol extract is filtered with pre-weighed filtrator. and is sticky when chewed. aleurone grains. the bluish purple color produces again.0%. Cotyledon cell is oblong. brown or reddish brown. heat for 3 minutes with occasional stirring in a water-bath. long polygonal or round cells in pigment layer containing clustered crystals of calcium oxalate. the perisperm has a globular or elliptical large secretary cells containing essential oil. Seed coat is thin.0%. somewhat dented around edge. Nelumbo Seed Nelumbinis Semen Nelumbo Seed is the well-ripe seed of Nelumbo nucifera Gaertner (Nymphaeaceae). Add 2 to 3 drops of Dragendorff’s TS to 2 mL of the filtrate: a brownish-yellow precipitate is produced. and centrifuge. a transverse section shows thin. Nutmeg has characteristic odor. a transverse section reveals seed coat composed of quadrangular or polygonal epidermis cell. A small endosperm is bent near the hilum. usually with the endocarp. Under a magnifying glass. Identification (1) Weigh 1. fat and sometimes brown-yellowish red colorant.5 mL of the supernatant liquid add 1 droplet of αnaphthol solution. Ash Not more than 9. 1 cm to 3 cm in diameter. add 5 mL of ether. yellowish Myristicae Semen Nutmeg is the ripe seed of Myristica fragrans Houttuyn (Myristicaceae). Sometimes root bark or wood pieces are mixed. somewhat upto 10 cm. which is surrounded by a raised ring. bead-threaded thickened cell wall. To 0. and oily lustrous.0 g of pulverized Nelumbo Seed. mix well and add gently 1 mL of sulfuric acid: a purple color ring is produced at the contact of the two layers. Description Nelumbo Seed is uaually an ellipsoidal or subspheroidal seed.0%. oblong. add 30 mL of ethanol and warm for 30 minutes with occasional stirring. allow to cool. without luster or in the middle of luster and yellowish brown color. Liquid like yellowish brown milk are formed when grined and mixed in water. Description Nutmeg is ovoid or ellipsoidal seed. Identification (1) Triturat Myrrh with water: a yellowish brown emulsion is produced. repeat the above extract procedure three times with the residue with 15 mL of each ethanol for 5 minutes. smooth with fine longitudinal striations and relatively wide veins. where there is a small dark repression. The center of one end is papillate. Ash Not more than 5. The perisperm has a number of irregular protrusions and inserted to the pale yellowish white endosperm to make marblelike striations. Myrrh has characteristic aroma and bitter taste. Under a microscope. Usually white spots and marks are appeared and broken piecese are shining or semi-translucent. 10 to 17 mm in length and 5 to 12 mm in diameter. spiral vessels and round vessels. deep brown. there is a lighter-colored patch with brown lines radiating from the hilum. (2) Weigh 1 g of pulverized Myrrh. at the opposite end of the kernel. the endosperm is composed of subrounded parenchymatous cells which contain starch grains. cool and filter. Its embryo is extremely bitter. mostly with cracks. The aril and seed coat is removed when used. From this an ill-defined furrow runs to the chalaza.5 mL of water. The residue on the filtrator is washed several times with 5 mL of warm ethanol: the remaining insoluble substance is not more than 70% after oven drying at 100 °C and cooling in the desiccator (silica gel). centrifuge and separate the supernatant liquid. Amount (mg) of strychnine (C 21 H 22 N 2O 2) = amount (mg) of Strychnine Nitrate RS. add 3 mL of ammonia TS and 20 mL of chloroform. Texture is extremely hard. Develop the plate with a mixture of chloroform and hexane (7 : 3) to a distance of about l0 cm and airdry the plate. the margin and the central part are bulged a little. packed with . Essential Oil Content Not less than 0. Identification (1) Weigh 3 g of pulverized Nux Vomica.0 g). cool and add 5 drops of sulfuric acid drop-wise carefully along the wall of the test tube: the layer of sulfuric acid shows a purple color which turns immediately form red to redbrown. On both sides. about 7 mm in length.0 mL of this solution.8414 QS 5 Internal standard solution⎯A solution of barbital sodium in the mobile phase (l in 500). After cooling. (2) Take the remaining filtrate obtained in (l). QT and QS. To this solution. Identification (1) Weigh 1 g of pulverized Nutmeg. Pipet 10. and prominent at the one side and slightly dented at the other side. add 1 mL of potassium bichromate TS and allow to stand for 1 hour: a yellow-red precipitate is produced. Packaging and Storage Preserve in tight containers. Combine all the extracts and evaporate the ether in a water-bath. add l mL of water. Part II tastes. Nux Vomica Strychni Semen Nux Vomica is the well ripe seed of Strychnos nuxvomica Linné (Loganiaceae). Operating conditions Detector: An ultraviolet absorption photometer (wavelength: 210 nm). add 20 mL of ether. add exactly 10 mL of the internal standard solution.5%. is situated at one end between the inner surfaces of the endosperms. about 4 mm in inside diameter and about 15 cm in length. A white embryo. place in a glass-stoppered centrifuge tube and moisten with l mL of strong ammonia water. when dried. Stand the filtrate for 10 minutes in an ice water-bath: a white precipitate is produced. Repeat this procedure three times with the residue using 20 mL volumes of ether. Ash Not more than 3. Nux Vomica. of the peak area of strychnine to that of the internal standard for the test solution and the standard solution. the seed coat is thin and the interior consists of two horny. pale grayish yellow endosperms and leaving a central narrow cavity at the center. Remove most of the chloroform from the filtrate by warming in a water-bath. add 10 mL of methanol. stopper the centrifuge tube tightly.8 μm. respectively. Dissolve the residue in 10 mL of the mobile phase. warm for 3 minutes in a waterbath and filter while warm. Collect the precipitate by filtration and wash with l mL of water. weigh exactly about 75 mg of Strychnine Nitrate RS (determined the loss on drying before use) and dissolve in the mobile phase to make exactly 50 mL. Column: A stainless steel column. Perform the test with the test solution and the standard solution as directed under the Liquid Chromatography according to the following operating conditions. Transfer a part of the precipitate to a small test tube. Determine the ratios. Filter this solution through a membrane filter with a porosity not more than 0. previously dried at 60 o C for 8 hours. Acid-insoluble Ash Not more than 0. then add the mobile phase to make exactly 100 mL and use this solution as the standard solution. Ash Not more than 3.6. add 5 mL of diluted sulfuric acid (1 in 10) and warm in a water-bath while shaking well until the odor of chloroform is no longer perceptible. Assay Weigh accurately about 1 g of pulverized Nux Vomica. 1 cm to 3 cm in diameter and 3 mm to 5 mm in thickness. When cracked upon soaking in water.0%. discard the first 2 mL of the filtrate and use the subsequent filtrate as the test solution. macerate for 30 minutes with occasional shaking and filter. Expose the plate to iodine vapor: a yellow spot appears in the region of Rf value 0. calculated on the dried basis × QT 1 × × 0.05% of strychnine (C21H22N202: 334. add exactly 10 mL of the internal standard solution and add the mobile phase to make exactly 100 mL. Nux Vomica is odorless and it has very bitter and persisting taste. shake for 15 minutes. Description Nux Vomica is button-shaped. covered densely with lustrous suppressed hairs radiating from the center to the circumference. Separately. contains not less than 1. (2) Dissolve precipitate produced in (1) 5 mL of chloroform and use this solution as the test solution.5 mL (10. dissolve by warming.1064 Monographs.0%. filter through a pledget of absorbent cotton and add 2 mL of nitric acid to l mL of the filtrate: a red color develops. Spot 2 μL of the test solution on a plate of silica gel for thin-layer chromatography. Perform the test with this solution as directed under the Thin-layer Chromatography. The dot-like micropyle is situated at one point on the margin and from which usually a raised line runs to the center on one side.42). External surface is pale grayish yellow-green to pale grayish brown. 0.5 g of Nux Vomica Extract with 0.15% to 6. mix with occasionally shaking. Assay Weigh accurately about 2. Description Nux Vomica Extract Powder 10% is yellow-brown to grayish brown powder. and has slight. 10% Nux Vomica Extract Powder Nux Vomica Extract Powder 10% contains not less than 0. To this. add 15 mL of ammonia TS and shake. . Add 20 mL of ether. Flow rate: Adjust the flow rate so that the retention time of strychnine is about l7 minutes. May be prepared with an appropriate quantity of ethanol and purified water. place in a glass-stoppered centrifuge tube. Column temperature: A room temperature.68% of strychnine (C21H22N2O2: 334. stopper tightly. then warm and soften with stirring. Dry. dissolve by warming. Collect the precipitate by filtration and wash with l mL of water.61% and not more than 0. add exactly 10 mL of the internal standard solution and add the mobile phase to make exactly 100 mL. add 15 mL of ammonia TS and shake. preferably at a low temperature and dilute with a sufficient additional quantity of starch. Nux Vomica Extract has a characteristic odor and an extremely bitter taste. Repeat this procedure 3 times with the water layer. add 1 mL of potassium bichromate TS and allow to stand for 1 hour: a yellow-red precipitate is produced. Selection of column: When the procedure is run with 5 μL of the standard solution under the above operating conditions. warm on a water-bath with shaking until the odor of chloroform disappears. Method of preparation Nux Vomica Extract 100 g Starch. add 5 mL of diluted sulfuric acid (1 in 10). Method of preparation After defatting 1000 g of coarse powder of Nux Vomica with hexane. cool and add 5 drops of sulfuric acid drop-wise carefully along the wall of the test tube: the layer of sulfuric acid shows a purple color which turns immediately form red to redbrown.8414 QS 5 Internal standard solution⎯A solution of barbital sodium in the mobile phase (1 in 500). characteristic odor and bitter taste. shake for 15 minutes.41). Nux Vomica Extract Nux Vomica Extract contains 6.2 g of Nux Vomica Extract. Cool. Amount (mg) of strychnine (C 21 H 22 N 2O 2) = amount (mg) of Strychnine Nitrate RS.42). Preserve in light-resistant. Combine the extracts and prepare the dry extract as directed under Extracts. digest by the percolation method. Add 2 mL of nitric acid to the filtrate: a red color develops. lactose or their mixture little by little and mix well. Identification (1) Weigh 3. using 20-mL volumes of ether. stopper tightly. cool and filter through absorbent cotton.0 g of Nux Vomica Extract Powder 10%. add l mL of water.5 mL of ammonia TS and 10 mL of chloroform with occasional shaking. the internal standard and strychnine are eluted in this order and clearly dividing each peak. add 800 g of starch. Transfer a part of the precipitate to a small test tube. 10 mL of acetic acid and 240 mL of purified water as the first solvent and 70% ethanol as the second solvent. Proceed as directed in the Assay under Nux Vomica. Identification Extract 0.8 g of monobasic potassium phosphate in water to make 1000 mL and a mix with acetonitrile and triethylamine (45 : 5 : 1) and adjust the mixture with phosphoric acid to a pH of 3. evaporate the filtrate on a water-bath until most of the chloroform is removed and proceed as directed in the Identification under Nux Vomica. add 3 mL of ammonia TS and 20 mL of chloroform. Warm the filtrate on a water-bath and evaporate chloroform to remove. lactose or their mixture a sufficient quantity ⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯ To make 1000 g Take Nux Vomica Extract. Mobile phase: Dissolve 6. Packaging and Storage tight containers. add 100 mL of purified water.0 g of pulverized Nux Vomica Extract Powder 10%. digest for 30 minutes and filter. Filter the chloroform extract. using a mixture of 750 mL of ethanol. (2) Take the remained filtrate obtained (1). Add 20 mL of ether. calculated on the dried basis × QT 1 × × 0. Description Nux Vomica Extract is yellow-brown to brown powder. Assay Weigh accurately about 0. shake for 15 minutes. Combine the extracts and evaporate the ether on a water-bath. centrifuge to disperse the ether layer. lactose or their mixture to make 1000 g of the homogeneous powder.KP VIII 1065 octadecylsilyl silica gel for Liquid Chromatography (5 μm in particle diameter). Dissolve the residue in 10 mL of the mobile phase. place in a glass-stoppered centrifuge tube.81% of Strychnine (C21H22N2O2: 334. 90.42). Opium Alkaloids Hydrochloride is soluble in water. calculated on the dried basis × QT 1 × × 0. Nux Vomica Tincture contains not less than 0. in coarse powder 100 g 70% ethanol a sufficient quantity ⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯ To make 1000 mL Prepare as directed under Tinctures.0 mL of Nux Vomica Tincture into a glass-stoppered centrifuge tube. discard the first 2 mL of the filtrate and use the subsequent filtrate as the test solution. using 20 mL volumes of ether. Proceed as directed in the Assay under Nux Vomica. warm the filtrate on a water-bath to remove most of chloroform and proceed as directed in the Identification under Nux Vomica. (2). Opium Alkaloids Hydrochloride Description Nux Vomica Tincture is yellow-brown liquid.0% of Morphine (C17H19NO3: 285. Proceed as directed in the Assay under Nux Vomica. transfer to a separatory funnel. Filter the solution through a filter of 0. Preserve in light-resistant Nux Vomica Tincture rate the ether on a water-bath. weigh accurately about 75 mg of Strychnine Nitrate RS (determined loss on drying before using) and dissolve in the mobile phase to make exactly 100 mL. Separately. calculated on the dried basis × QT 1 × × 0. Assay Pipet 3. It may be prepare with an appropriate quantity of Ethanol and Purified Water in place of 70% ethanol.1066 Monographs. Opium Alkaloids Hydrochloride contains 47. Preserve in light-resistant. Dissolve the residue in 10 mL of the mobile phase. with the above ingredients. Amount (mg) of strychnine (C 21 H 22 N 2O 2) = amount (mg) of Strychnine Nitrate RS. Part II centrifuge to disperse the ether layer. Examine under ultraviolet light (main wave- . Repeat this procedure twice with the water layer. cool. Dissolve the residue with 10 mL of the mobile phase. using 20 mL of ether.34) and 34. respectively. add 2 mL of ammonia TS and 20 mL of chloroform and shake well for 2 to 3 minutes. Pipet 5.116% of Strychnine (C21H22 N2O2: 334. Combine the extracts and evaporate the ether on a water-bath. Perform the test with the test solution and the standard solutions as directed under the Thin-layer Chromatography. Develop the plate with a mixture of acetone.0 mL of this solution. shake for 15 minutes and centrifuge to disperse the ether layer. Packaging and Storage tight containers. add exactly 10 mL of the internal standard solution and add the mobile phase to make exactly 100 mL. dissolve 60 mg of Morphine Hydrochloride RS.0% to 41. Method of preparation Nux Vomica.8414 QS 5 Internal standard solution⎯A solution of barbital sodium in the mobile phase (1 in 500).0% to 52. stopper tightly. add exactly 5 mL of the internal standard solution. 10 mg of Codeine Phosphate RS and 10 mg of Papaverine Hydrochloride RS in 10 mL each of diluted ethanol (1 in 2) and use these solutions as the standard solution (1). Repeat this procedure three times with the water layer. add the mobile phase to make exactly 50 mL and use this solution as the standard solution. and has extremely bitter taste.7 (Method 2). slightly soluble in dehydrated ethanol. Description Opium Alkaloids Hydrochloride is white to pale brown powder.0% of other opium alkaloids.1 g of Opium Alkaloids Hydrochloride in 10 mL of diluted ethanol (1 in 2) and use this solution as the test solution.097% and not more than 0.8-μm or finer porosity. add 10 mL of ammonia TS and 20 mL of ether. Combine the extracts and evapo- Opium Alkaloids Hydrochloride consists of the hydrochloride of some of the main alkaloids obtained from opium. Packaging and Storage tight containers. Separately. toluene. Alcohol Number Not less than 6. add exactly 5 mL of the internal standard solution and add the mobile phase to make exactly 50 mL. Spot 20 μL each of the test solution and the standard solutions on a plate of silica gel with a fluorescent indicator for thin-layer chromatography. Identification Heat 20 mL of Nux Vomica Tincture on a water-bath to remove ethanol. Identification (1) Dissolve 0. dehydrated ethanol and strong ammonia water (20 : 20 : 3 : 1) to a distance of about 10 cm and air-dry the plate. (3) and (4). Filter the chloroform layer through absorbent cotton. Amount (mg) of strychnine (C 21 H 22 N 2O 2) = amount (mg) of Strychnine Nitrate RS. Opium Alkaloids Hydrochloride is colored by light. 40 mg of Noscapine Hydrochloride RS.8414 QS 5 Internal standard solution⎯A solution of barbital sodium in the mobile phase (1 in 500). 20 Specific gravity⎯ d 20 : About 0. 0 g of sodium lauryl sulfate in 500 mL of diluted phosphoric acid (1 in 1000) and adjust the pH to 3. 10 mL of 0.KP VIII 1067 length: 254 nm): each spot from the test solution is the same color and the same Rf value with the corresponding spot from the standard solution (1). and the peak area. 5 mL of water was passed through the column (packed with about 0. about 4.5 g.5 g). AT3. AS. (2). AT4. narceine and noscapine.8867 AS Amount (mg) of other opium alkaloid = amount (mg) of Morphine Hydrochloride RS. dissolve in water to make exactly 50 mL and use this solution as the standard solution. codeine. calculated on the anhydrous basis × A T1 × 0. AT1. the relative standard deviation of the peak area of morphine is not more than 1. When the procedure is run with 20 μL of this solution under the above operating conditions.5% (0. Mobile phase: Dissolve 1.0% (0.19A T 5 + A T 6 × 0. with many longitudinal wrinkles.0%.1 g of Opium Alkaloids Hydrochloride in 2 mL of water and loading in column for chromatography. Packaging and Storage tight containers. System suitability System performance: Dissolve 60 mg of Morphine Hydrochloride RS. Next wash with this order 5 mL of water. Column: A stainless steel column. Separately. dissolve in water to make exactly 50 mL and use this solution as the test solution. Preserve in light-resistant. calculatedon the anhydrous basis × A T2 + 0. or the rhizome or root of Notopterygium incisum Ting or Notopterygium forbesii Boissier (Umbelliferae). Ostericum Root Osterici Radix Ostericum Root is the root of Ostericum koreanum Maximowicz (Umbelliferae). 10 mg of Codeine Phosphate RS. morphine.0. Under a . AT2. 8 hours).0 and 4.1 g of Opium Alkaloids Hydrochloride. Amount (mg) of morphine (C 17 H 19 NO 3) = amount (mg) of Morphine Hydrochlor ide RS. and 2 to 5 purple periderm are attached around the crown. with sparse rootlet scars. pH Dissolve 1.20. A few remains of stem are present at the crown. papaverine and noscapine are eluted in this order with the resolution between these peaks being not less than 1. packed with octadecylsilanized silica gel for liquid chromatography (5 μm in particle diameter). (2) Meconic acid⎯Dissolve 0. Assay Weigh accurately about 0. Column temperature: A constant temperature of about 40 °C. Use the outflow solution as the test solution. of morphine. thebaine. AT5 and AT6.29A T3 + 0. To 240 mL of this solution add 70 mL of tetrahydrofuran and mix. Purity (1) Clarity⎯Dissolve 0. codeine. of morphine of the standard solution.0 g of Opium Alkaloids Hydrochloride in 50 mL of water: the pH of the solution is between 3. Loss on Drying Not more than 6. Perform the test with 20 μL each of the sample solution and the standard solution as directed under the Liquid Chromatography according to the following operating conditions and calculate the peaks area. After adding 2 mL of diluted sodium hydroxide solution and 1 drop of ferric chloride TS to the test solution: no red color develops. and 2 cm to 5 cm in diameter.5 g of Opium Alkaloids Hydrochloride in 10 mL of water: the solution is clear and determine the spectrum of the solution at 420 nm as directed under the Ultraviolet-visible Spectrophotometry: the absorption is not more than 0. System repeatability: When the test is repeated 6 times with 20 μL of the standard solution under the above operating conditions.8867 AS Operating conditions Detector: An ultraviolet absorption photometer (wavelength: 285 nm). Flow rate: Adjust the flow rate so that the retention time of morphine is about 10 minutes.20A T 4 + 0. and several branched rhizomes.36 g of aminopropylsilanized silica gel (55 μm to 105 μm in particle diameter) in polyethylene tube about 1 cm inside diameter). Description (1) Ostericum koreanum⎯Ostericum Root from Ostericum koreanum consists fusiform main root.6 mm in inside diameter and about 15 cm in length. 120 °C.5. (2) A solution of Opium Alkaloids Hydrochloride (1 in 50) responds to the Qualitative Test (2) for chloride. 5 mL of methanol.0 with sodium hydroxide TS. papaverine. 10 mg of Papaverine Hydrochloride RS and 40 mg of Noscapine Hydrochloride RS in water to make exactly 50 mL. weigh accurately about 60 mg of Morphine Hydrochloride RS.1 mol/L hydrochloric acid and pass with 2 mL of 1 mol/L hydrochloric acid. The root is 15 cm to 30 cm in length. Residue on Ignition Not more than 0. (3) and (4). External surface is yellow-brown to brown. 1068 Monographs, Part II magnifying glass, cortex of transverse section is light yellow, xylem of fracture is yellow, and brown cambium is distinct. Under a microscope, a transverse section reveals collenchyma under cork layer, and resin canal arrange on several concentric circles. Vessels develop radiating from protoxylems. Medullary rays develop in rows of 2 to 3 from pith to phloem. The whole parenchymas contain starch grains. Ostericum Root from Ostericum koreanum has characteristic odor and sweet and cooling taste at first and followed by a slight bitterness. (2) Notopterygium incisum⎯Ostericum Root from Notopterygium incisum consists of rhizome and root, somewhat curved cylindrical to conical, 3 cm to 10 cm in length, 0.5 cm to 2.0 cm in diameter. The rhizome is occasionally branched. Surface is yellow-brown to dark-brown. The top of rhizome has scars of slightly round stem, and it is occasionally founded with remains of short stem. The surface of rhizoma has outstanding nodes, and the length of internode is normally short. Scars of warty roots in nodes, coarsely longitudinal wrinkles and warty sparse root are present in external surface of root. The texture is light, slightly fragile and breakable. The transverse section has radial fissured appearance, the cortex is yellow-brown to brown, the xylem is light yellow to light grayish yellow, and the pith is grayish-white to light brown. Under a magnifying glass, the transverse section reveals brown thin oil drops in cortex and pith. Ostericum Root from Notopterygium incisum has characteristic odor, and slightly sour taste at first and followed by a slight pungent and acrid taste. (3) Notopterygium forbesii⎯Ostericum Root from Notopterygium forbesii is rhizoma or root. The rhizoma is cylindrical, the top of rhizoma has scars of stem or leaf sheath, and the root is conical, with longitudinal and fissure. Surface is brown and with dense circular pattern nearby rhizoma. The root is 4 cm to 13 cm in length, and 6 mm to 25 mm in diameter. Some rhizoma are coarse, large, irregulary knotted, and the top of rhizoma has several remains of stem bottom. The root is relatively thin and breakable. The cutted surface is slightly flat, the cortex is light grayish black-brown, and the xylem is yellowish white. Ostericum Root from Notopterygium forbesii has slightly bitter taste and relatively lightness. Identification Weigh 1 g of pulverized Ostericum Root, add 10 mL of ether, and extract this at ordinary temperature. Examine the extract solution under ultraviolet light; it has strong fluorescence. Purity Foreign matter⎯Ostericum Root contains not more than 5.0% of stem base and other foreign matters. Loss on Drying Not more than 12.0%. Ash Not more than 10.0%. Acid-insoluble Ash Not more than 2.0%. Essential Oil Content Not less than 0.2 mL (50.0 g). Extract Content Dilute ethanol-soluble extract— Not less than 20.0%. Oyster Shell Ostreae Testa Oyster Shell is the shell of Ostrea gigas Thunberg, Ostrea talienwhanensis Crosse or Ostrea rivularis Gould (Ostreidae). Description Oyster Shell of Ostrea gigas Oyster shell is the shell consisting of irregularly curved, foliaceous or lamellated broken pieces. The unbroken oyster shell forms a bivalve, 6 mm to 100 mm in length and 2 cm to 5 cm in width. The upper valve is flat and the lower one is somewhat hollow. Both the upper and lower edges of the valve are irregularly curved and bite with each other. The surface of the valve is externally light greenish gray-brown and internally milky. Oyster shell is odorless and tasteless. Oyster Shell of Ostrea talienwhanensis Oyster shell is the shell, subtriangular, dorsal and ventral edges are V-shaped. The outer surface of the right shell is pale yellow and concentric scales are arranged loosely and undulated up and down. The inner surface is white. The left shell are bering strong and thick concentric scales, with weveral distinct ribs radiated from the umbo. The inner surface is concaved in box-shaped. Hinge surface is small. Oyster Shell of Ostrea rivularis Oyster shell is the shell, rounded, oval or triangular. The outer surface of the right shell is slightly uneven, gray, purple and yellow, surrounding the concentric scales in a ring. It is thin and fragile when immature and overlapped one another after several years growth. The inner surface is white and sometimes its edge is pale purple. Identification (1) Weigh l g of pulverized Oyster Shell, dissolve in 10 mL of dilute hydrochloric acid by heating: it evolves a gas and forms a very slightly red, turbid solution in which a transparent, thin suspended matter remains. Pass the evolved gas through calcium hydroxide TS: a white precipitate is produced. (2) The solution obtained in (1) has slight, characteristic odor. Filter this solution and neutralize with ammonia TS: the solution responds to the Qualitative Tests for calcium salt. (3) Ignite l g of pulverized Oyster Shell: it turns blackish brown at first and evolves characteristic odor. Ignite it further: it becomes almost white. Purity Barium—Weigh 1 g of pulverized Oyster Shell, dissolve in 10 mL of dilute hydrochloric acid: the solution does not respond to the Qualitative Tests (1) KP VIII 1069 for barium salt. Loss on Drying Not more than 4.0% (1 g, 180 °C, 4 hours). Packaging and Storage Preserve in tight containers. Peach Kernel Persicae Semen Peach Kernel is the ripe seed of Prunus persica Batsch or Prunus davidiana Franchet (Rosaceae). Peach Kernel contains not less than 0.5% of amygdalin (C20H27NO11: 457.43). Description Peach Kernel is the seed, flattened, asymmetric ovoid seed, 12 mm to 20 mm in length, 6 mm to 12 mm in width and 3 mm to 7 mm in thickness. The shape of the seed is somewhat sharp at one end and round at the other end with chalaza. Seed coat is redbrown to pale brown and its surface is powdery by easily detachable stone cells of epidermis. Numerous vascular bundles are running and rarely branching from chalaza through the seed coat and, appearing as dented longitudinal wrinkles. When soaked in boiling water and softened, the seed coat and thin, translucent, white albumen are easily separated from the cotyledons, and the cotyledons are white. Under a microscope, the outer surface of seed coat reveals polygonal, long polygonal, or obtuse triangular stone cells on the protrusion from vascular bundles, shape of which considerably different according to the position and their membranes almost equally thickened. In lateral view, Peach Kernel appears as a square, rectangle or obtuse triangle. Peach Kernel has slightly characteristic odor tastes bitter. Identification Weigh 1 g each of pulverized Peach Kernel or Peach Kernel RMPM, add 10 mL of methanl and heat under a reflux condenser in a water bath for 10 minutes. After then, filter and use these as the test solution and Peach Kernel RMPM standard solution. Separately, weigh 2 mg of Amygdalin RS, dissolve in 1 mL of methanol and use this solution as the standard solution. Perform the test with the test solution, Peach Kernel RMPM standard solution and the standard solution as directed under Thin-layer Chromatography. Spot 10 μL each of the test solution, Peach Kernel RMPM standard solution and the standard solution on a plate of silica gel with fluorescent indicator for thin-layer chromatography. Develop the plate with a mixture of ethyl acetate, methanol and water (12 : 2 : l) to a distance of about 10 cm and air-dry the plate. Spray evenly the plate with sulfuric acid TS for spraying and heat at 105 o C for 10 minutes: the spots from the test solution and the spots from Peach Kernel RMPM standard solution show the same color and the same Rf value, and one spot among them and brown to dark brown spot from the standard solution show the same color and the same Rf value. Purity (1) Rancidity—Grind Peach Kernel with boiling water: no odor of rancid oil is perceptible. (2) Foreign matter—Peach Kernel does not contain broken pieces of endocarp or other foreign matter. Assay Weigh accurately about 2.0 g of pulverized Peach Kernel, add 50 mL of methanol, extract with a reflux condenser for 3 hours and filter. Repeat the above procedure with the residue using 50 mL of methanol. Combine the whole filtrates, evaporate to dryness in vaccum. Add 70 mL of water and 70 mL of hexane to the residue, shake well and discard the hexane layer. Add 70 mL of ether to the water layer, shake and discard the ether layer. The remaining water layer is filtered, adjust the total volume to 100 mL and use this solution as the test solution. Seperately, dry the Amygdalin RS for 24 hours in the desiccator (silica gel) and weigh accurately about 10 mg, dissolve in 100 mL of water and use this solution as standard solution. Perform the test with 10 µL each of the test solution and the standard solution as directed under the Liquid Chromatography according to the following operating conditions and determine the peak areas, AT and AS, of amygdalin for the test solution and the standard solution, respectively. Amount (mg) of amygdalin (C 20 H 27 NO 11 ) = amount (mg) of Amygdalin RS × AT AS Operating conditions Detector: An ultraviolet absorption photometer (wavelength: 214 nm). Column: A stainless steel column, 4 mm to 6 mm in inside diameter and 15 cm to 25 cm in length, packed with octadecylsilyl silica ge1 (5 　m to l0 　m in particle diameter). Column temperature: An ordinary temperature. Mobile phase: A mixture of methanol and water (20 : 80). Flow rate: 1.0 mL/minute. Peony Root Paeoniae Radix Peony Root is the root of Peonia lactiflora Pallas or allied plants (Paeoniaceae). Peony Root contains not less than 2.3% of total sum of albiflorin (C23H28O11: 480.46) and paeoniflorin (C23H28O11: 480.46), calculated on the basis of dried material. Description Peony Root is the root, cylindrical, sometimes curved, 5 cm to 20 cm in length and 10 mm 1070 Monographs, Part II to 25 mm in diameter, and large root is cut lengthwise. External surface is white or brown, with distinct longitudinal wrinkles, often with wrinkles or scars of lateral roots and with laterally elongated lenticels. The upper part of root often remains scars of stems or unremoved brown cortex. Texture is hard, difficult to fracture. The transverse section is granular and very dense. Under a magnifying glass, cambium is distinct, milky white or brown, and radial pith is observed. Peony Root has characteristic odor and taste, slightly sweet at first, followed by an astringency and a slight bitterness. and , AASA and AASp, of albiflorin for the standard solution, respectively. Identification (1) Weigh 0.5 g of pulverized Peony Root, add 30 mL of ethanol, shake for 15 minutes and filter. Shake 3 mL of the filtrate with l drop of ferric chloride TS: a blue-purple to blue-green color is produced and it changes to dark blue-purple to dark green. (2) Weigh 2 g of pulverized Peony Root, add 10 mL of methanol, warm in a water-bath for 5 minutes, cool, filter and use the filtrate as the test solution. Separately, weigh l mg of Paeoniflorin RS, add 1 mL of methanol, dissolve and use this solution as the standard solution. Perform the test with the test solution and the standard solution as directed under the Thin-layer Chromatography. Spot 10 μL each of the test solution and the standard solution on a plate of silica gel for thin-layer chromatography. Develop the plate with a mixture of acetone, ethyl acetate and acetic anhydride (10 : 10 : 1) to a distance of about 10 cm and air-dry the plate. Spray evenly p-anisaldehyde-sulfuric acid TS on the plate and heat at 105 o C for 10 minutes: one spot among the spots from the test solution and the purple spot from the standard solution show the same color and the same Rf value. Operating conditions Detector: An ultraviolet absorption photometer (wavelength: 230 nm). Column: A stainless steel column, 4 mm to 6 mm in inside diameter and 15 cm to 25 cm in length, packed with octadecylsilyl silica gel (5 μm to 10 μm in diameter). Column temperature: An ordinary temperature. Mobile phase: Control gradually or concentrationgradiently with mobile phase A and B as follows. Mobile phase A – water Mobile phase B – acetonitrile Loss on Drying Not more than 14.0% (6 hours). Flow rate: 1.0 mL/min System suitability System performance: Perform the test with the standard solution under the above operating conditions. Use a column giving elution of albiflorin and paeoniflorin in this order with the resolution between their peaks being separated completely. System repeatability: When the test is repeated 6 times with 20 μL of the standard solution under the above operating conditions: the relative standard deviation of the peak area of paeoniflorin is not more than 1.5%. Ash Not more than 6.5%. Acid-insoluble Ash Not more than 0.5%. Assay Weigh accurately about 0.5 g of pulverized Peony Root, add 50 mL of 50% methanol, heat under a reflux condenser in a water-bath for 30 minutes, cool and filter. To the residue, add 40 mL of 50% methanol and proceed in the same manner. Combine the filtrates, add 50% methanol to make exactly 100 mL and use this solution as the test solution. Separately, weigh accurately about 10 mg each of Paeoniflorin RS, previously dried in a desiccator (in vacuum, P2O5, 80 °C), and Albiflorin RS, previously dried in a desiccator (in vacuum, P2O5, 80 °C), for 8 hours, dissolve in 50% methanol to make exactly 100 mL and use this solution as the standard solution. Pipet 20 μL each of the test solution and the standard solution and perform the test as directed under the Liquid Chromatography according to the following operating conditions. Determine the peak areas, ATA and ASA, of paeoniflorin for the test solution Amount (mg) of albiflorin (C 23 H 28 O11 ) = amount (mg) of Albiflorin RS × A TA A SA Amount (mg) of paeoniflor in (C 23 H 28 O 11 ) = amount (mg) of Paeoniflor in RS × A TP A SP Time (min) Mobile phase A (%) Mobile phase B (%) 0 90 10 15 90 10 30 80 20 45 65 35 48 50 50 55 50 50 Perilla Leaf Perillae Folium Perilla Herb is the leaf and twig of Perilla frutescens Britton var. acuta Kudo or Ferilla frutescens Britton var. crispa Decaisne (Labiatae). Description Perilla Herb is leaves and twigs. Both KP VIII 1071 surfaces of the leaf are brownish purple, or the upper surface is grayish green to brownish green and the lower surface is brownish purple. When smoothed by immersion in water, the lamina is ovate to obcordate, 5 to 12 cm in length and 5 cm to 8 cm in width. The apex is acuminate and the margin is serrate. The base is broadly cuneate, and has petiole, 3 cm to 5 cm in length. Cross sections of stem and petiole are square. Under a magnifying glass, hairs are observed on both surfaces of the leaf, but abundantly on the vein and sparsely on other parts. Small glandular hairs are observed on the lower surface. Under a microscope, a transverse section of midvein reveals horn-like and nonglandular hairs, and glandular hairs, and scales in the external wall. Bundles of fibers are sparsely arranged in the center region of the ring, the phloem is small, medullary rays are clear, the pith is very large. Perilla Herb has characteristic odor and slightly bitter taste. Identification Take 0.3 mL of a mixture of essential oil and xylene, obtained in Essential oil content, add l mL of acetic anhydride, shake and add l drop of sulfuric acid: a red-purple to dark red-purple color develops. Purity (1) Stem—The amount of its stems, which are not less than 3 mm in diameter, contained in Perilla Herb is not more than 3.0%. (2) Foreign matter—The amount of foreign matter other than the stems is not more than 1.0%. Loss on Drying Not more than 13.0% (6 hours). Ash Not more than 16.0%. Acid-insoluble Ash Not more than 2.5%. Essential Oil Content Not less than 0.2 mL (50.0 g, 1 mL of silicon resin). Pharbitis Seed Pharbitidis Semen Pharbitis Seed is the ripe seed of Pharbitis nil Choisy or Pharbitis purpurea Voigt (Convolvulaceae). Description Pharbitis Seed is the seed like longitudinally quartered or sexpartite globe, 6 mm to 8 mm in length and 3 mm to 5 mm in width. One hundred seeds weigh about 4.5 g. External surface is black to grayish reddish brown or grayish-white, smooth, but slightly shrunken and coarsely wrinkled. Under a magnifying glass, the surface of the seed coat reveals dense, short hairs, dented hilum at the bottom of the ridge. The transverse section is almost fan-shaped, pale yellow- brown to pale grayish brown and dense in texture. Seed coat is thin and the outer layer is dark gray and the inner layer is pale gray. Two irregularly folded cotyledons and two thin membranes from the center of the dorsal side to the ridge separating cotyledons are present in the transverse section of the upper part, but they are not observed in the transverse section of the lower part. Dark gray secretary pits are located in the section of the cotyledon. When cracked, Pharbitis Seed has a slightly characteristic odor and oily and slightly pungent taste. Ash Not more than 6.0%. Phellodendron Bark Phellodendri Cortex Phellodendron Bark is the bark of Phellodendron amurense Ruprecht or Phellodendron chinense Schneide (Rutaceae), from which the periderm has been removed. Phellodendron Bark contains not less than 0.6% of berberine [as berberine chloride (C20H18ClNO4 : 371.81)], calculated on the dried basis. Description Phellodendron Bark is flat or rolled semi-tubular pieces of bark, 2 mm to 4 mm in thickness, 5 to 15 cm in width and 20 cm to 40 cm in length, and sometimes fragments are mixed. External surface is grayish yellowish brown to grayish brown, with numerous traces of lenticel. The internal surface is yellow to dark yellowish brown, with five vertical lines and smooth. Fractured surface is fibrous and bright yellow. Under a magnifying glass, the transverse section reveals a thin and yellow outer cortex, scattered with stone cells appearing as yellowish brown dots. Inner cortex is thick. Primary medullary rays expand its width towards the outer end. The phloem appears as a nearly triangular part between these medullary rays in secondary cortex and many secondary medullary rays radiating and gathering to the tip of the triangle. Brown phloem fiber bundles lined in tangential direction, crossed over the secondary medullary rays and then these tissues show a latticework. Phellodendron Bark has slight odor and extremely bitter taste and is mucilaginous. Phellodendron Bark colors the saliva yellow on chewing. Identification (1) Weigh 1 g of pulverized Phellodendron Bark, add 10 mL of ether, allow to stand for 10 minutes with occasional shaking and filter. Collect the powder on the filter paper, add 10 mL of ethanol, allow to stand for 10 minutes with occasional shaking and filter. To 2 to 3 drops of the filtrate, add 1 mL of hydrochloric acid, add 1 to 2 drops of hydrogen peroxide TS and shake: a red–purple color develops. (2) Use the filtrate obtained in (1) as the test solution. Separately, weigh 1 mg of Berberine Chloride RS, Develop the plate with a mixture of n-butanol. Examine under ultraviolet light (main wavelength: 365 nm): one spot among the spots from the test solution and a spot with yellow to yellow-green fluorescence from the standard solution show the same color and the same Rf value.0% (6 hours). The vessels of spring wood are up to about 150 μm in diameter. Spot 5 μL each of the test solution and the standard solution on a plate of silica gel with a fluorescent indicator for thin-layer chromatography. Perform the test with the test solution and Pinellia Tuber RMPM standard solution as directed under the Thin-layer Chromatography. Description Pinellia Tuber is the tuber. taste.5% Assay Weigh about about 0. Ash Not more than 4. Purity Foreign matter—Not more than 1. Picrasma Wood Picrasmae Lignum Picrasma Wood is the heartwood of Picrasma quassioides Bennet (Simaroubaceae).0% Packaging and Storage Preserve in tight containers.5%. the transverse section reveals distinct annual rings and thin medullary rays. usually 10 μm to 15 μm in diameter and simple grains. Vivid yellow or red-brown. Spot 5 μL each of the test solution and the standard solution on a plate of silica gel for thin-layer chromatography. but leaving a strong acrid taste. Under a microscope. completely removed the periderm. resinous substances are often present in the vessels. Perform the test with the test solution and the standard solution as directed under the Thin-layer Chromatography. 7 mm to 25 mm in diameter and 7 mm to 15 mm in height. from which periderm has been removed. Identification Weigh 1 g of pulverized Pinellia Tuber or Pinellia Tuber RMPM. Ash Not more than 7. The wood fibers are extremely thickened. and medullary rays and xylem parenchyma cells contain rosette aggregates of calcium oxalate and starch grains.5 g of Phellodendron Bark. and water (8 : 3 : l) to a distance of about 10 cm. but those of autumn wood are only one-fifth as diameter. The upper end is dented where the stem has been removed. add 10 mL of methanol. (3) Stir up pulverized Phellodendron Bark with water: the solution becomes gelatinous owing to mucilage. These vessels are all single or in groups.5%. Description Picrasma Wood the heartwood consisting of chips. Plantago Seed Plantaginis Semen . External surface is white to grayish white-yellow. acetic anhydride. The texture is pale yellow and dense. a transverse section reveals amphivasal vascular bundle scattered. proceed as described in the Assay of Coptis Rhizoma. heat under a reflux condenser for 30 minutes in a water-bath. The taphides are 25 μm to l50 μm in length. Ash Not more than 3. slightly mucous. water and glacial acetic acid (7 : 2 : 1) to a distance of about 10 cm and air-dry the plate.0%. and use the filtrate as the test solution or Pinellia Tuber RMPM standard solution. and a cross section is white and powdery. Starch grains mostly 2 to 3 compound grains. Part II dissolve in l mL of methanol and use this solution as the standard solution. the spots from the test solution and the spots Pinellia Tuber RMPM standard solution show the same color and the same Rf value. filter. 6 hours). extremely bitter and lasting. Acid-insoluble Content Not more than 1. Loss on Drying Not more than 11.1072 Monographs. slices or short pieces of wood. Pinellia Tuber is nearly odorless and tasteless at first. scattered in the xylem parenchyma. slightly flattened spherical to irregular-shaped. Under a magnifying. Acid-insoluble Contents Not more than 0. Picrasma Wood reveals medullary rays consisting of l to 5 cells wide for transverse section and 5 to 50 cells high for longitudinal section. Under a microscope.0% (105 o C . mainly tissue of parenchyma filled with starch grains and scattered with a few mucilage cells containing raphides of calcium oxalate. and air-dry the plate. usually 3 μm to 7 μm in diameter. Loss on Drying Not more than 14. Deve1op the plate with a mixture of n-buthanol. Spray evenly the plate with ninhydrin TS and heat at 105 o C for 10 minutes. Picrasma Wood is odorless. Texture is dense. Pinellia Tuber Pinelliae Tuber Pinellia Tuber is the tuber of Pinellia ternata Breitenbach (Araceae).0%. and with root scars dented as numerous small spots on the circumference. boil gently with 10 mL of dilute hydrochloric acid for 2 minutes and filter. followed by an acrid and bitter taste. Preserve in light-resistant.7 mm to 1 mm in width and 0. a transverse section reveals cambium and its neighborhood often brown. transverse section reveal a line of radiating vessels and medullary rays developing to the cortex lined alternately. add carefully 0. Platycodon Fluid Extract is miscible with water and produces slight turbidity. The cortex is slightly thinner than xylem. The greater part of the root. a vegetative layer and a pigment layer of approximately equidiameter cells. Micropyle and raphe is not observed. De Candolle (Campanulaceae). Content of the Active Principle Transfer 5 mL of Platycodon Fluid Extract. add 1 mL of Fehling's TS and warm the mixture: a red precipitate is produced. Platycodon Root Platycodonis Radix Platycodon Root is the root. accurately measured. long fusiform to conical . The xylem is white to pale brown and the tissue is slightly denser than cortex. Platycodon Fluid Extract has a mild taste at first. with the dorsal side protruding like a bow and with the ventral side somewhat dented. In the interior. Platycodon Root has slight odor and is tasteless at first.5%. Under a microscope.5 mL of sulfuric acid to make two layers: a red to redbrown color develops at the zone of contact and the upper layer acquires a blue-green to green color. An appropriate quantity of Ethanol and Purified Water may be used in place of 25% Ethanol. . (2) Weigh 1 g of Plantago Seed. with or without periderm. 0. Under a magnifying glass. Neutralize the filtrate with sodium hydroxide TS. warm with 2 mL of acetic anhydride in a water bath for 2 minutes and filter.5 mm in thickness. (2) Dissolve 1 drop of Platycodon Fluid Extract in 2 mL of acetic anhydride and add gently 0. Purity Starch Mix 1 mL of Platycodon Fluid Extract with 4 mL of water and add 1 drop of dilute iodine TS: no purple or blue color is observed. evaporate to dryness on a water-bath and dry at 105 o C for 5 hours: the residue is not less than 0.KP VIII 1073 Plantago Seed is the ripe seed of Plantago asiatica Linné or Plantago depressa Willdenow (Plantaginaceae). the surface of the seed is practically smooth.5 mm in length. is covered with coarse longitudinal wrinkles. Description Platycodon Fluid Extract is red-brown liquid. irregularly thin. 100 seeds weigh about 50 mg. External surface is brown to yellow-brown and lustrous. Description Platycodon Root is the root. To l mL of the filtrate. Plantago Seed is odorless and tastes slightly bitter and mucous. often branched. to a tared beaker.3 mm to 0.5 mL of Platycodon Fluid Extract with 10 mL of water: a lasting fine foam is produced.2 g of pulverized Platycodon Root. Acid-insoluble Ash Not more than 2. Under a magnifying glass.5 g of pulverized Platycodon Root. Identification (1) Shake vigorously 0. lateral furrows and lenticel-like lateral lines. Description Plantago Seed is flattened ellipsoidal seed. Main root is 10 to 15 cm in length and 1 to 3 cm in diameter. External surface is grayish brown. Purity Foreign matter⎯Not more than 2. Platycodon root has solitary crystals of calcium oxalate and lactiferous tubes with light yellowish latex in the cork cells. a transverse section reveals a seed coat consisting of three layers of epidermis composed of ce1ls containing mucilage.0%. endosperm is thicker than seed coat enclosing two cotyledons. of Platycodon grandiflorum A. boil with 10 mL of water for a while. almost white and with scattered cracks. later acrid and bitter. The upper end of the root has dented scars of removed stems. Packaging and Storage tight containers.5 mL of sulfuric acid: a red to red-brown color is observed at the zone of contact. Ash Not more than 5. 2 mm to 2. to 3 mL of this solution. except the crown. often with cracks.50 g Identification (1) Weigh 1 g of Plantago Seed. Under a magnifying glass. Identification (1) Weigh 0. The neighborhood of the root has fine lateral wrinkles and longitudinal furrows and also slightly constricted.0%. The texture is hard is but brittle and the fractured surface is not fibrous. pale brown or white. (2) Weigh 0. add 2 mL of warm water and allow the mixture to stand for 10 minutes: the seed coat swells to discharge mucilage. Platycodon Fluid Extract Method of preparation Weigh coarse powder of Platycodon Root and prepare the fluid extract as directed under Fluid Extracts using 25% Ethanol. allow to cool and shake the mixture vigorously: a lasting fine foam is produced. consisting of the stem and opposite leaves. Main root is 10 cm to 20 cm in length. Part II Ash Not more than 4.0%.0%.0%. To filtrates. The texture is soft and breakable and the center of fractured surface reveals pith Pogostemon Herb has characteristic odor and slightly bitter taste. Margin of the transverse section is irregularly undulate. with large cracks here and there. Deve1op the plate with a mixture of toluene. Polygonatum falcatum A. frequently branched. combine the extract and evaporate the filtrate to dryness. Stems are square. (2) Foreign matter—The amount of foreign matter other than the stems contained in Polygala Root is not more than 1. Loss on Drying Not more than 13. Dissolve the residues to 1 mL of ethylacetate. The spots from the test solution and the spots from the standard solution show the same color and the same Rf value. pale brown and often tears in a wedge-like shape.5 g of pulverized Polygala Root. add 10 mL of water and shake vigorously: a lasting fine foam is produced (2) Weigh 0. Extract Content Dilute ethanol-soluble extract— Not less than 25.1074 Monographs. 2 mm to 10 mm in diameter. heat the plate at 105 o C for 10 minutes and examine under ultraviolet light (main wavelength: 365 nm). shake well and heat for distillating. margin-irregularly serrate. respectively.0 g). Description Polygonatum Rhizome is irregular cy- .0%. Leaves are crumpled into masses. add carefully 1 mL of sulfuric acid to make two layers: a redbrown color develops at the zone of contact and changes to dark green. To the filtrate. Description Polygala Root is thin. Purity (1) Stem—Not more than 10. heat under a reflux condenser on a water bath for 30 minutes. External surface is pale grayish brown. using 20 mL of dichloromethane. and filter. Spray diluted sulfuric acid TS to the plate. Pogostemon Herb Pogostemonis Herba Pogostemon Herb is the aerial part of Pogostemon cablin Bentham (Labiatae). Gray. Take 2 mL of distillate and add 0. Ash Not more than 6. Cortex is comparatively thick. Xylem is usually globular to elliptical. 50 cm to 60 cm in length. After shaking well. Polygala Root has slight odor and slightly acrid taste. ethyl acetate and formic acid (14 : 4 : 0. 2 cm to 5 cm in length. Identification (1) Weigh 0. cylindrical or tubular root. (3) Weigh 1 g each of pulverized Polygala Root and Polygala Root RS.0%. 2 mm to 7 mm in diameter and externally pubescent. Petioles are slender. filter. when whole ovate or elliptical. sometimes with several lateral roots. (Liliaceae). Polygonatum Rhizome Polygonati Rhizoma Polygonatum Rhizome is the steamed rhizome of Polygonatum sibiricum Redoute. Ash Not more than 13.5) to a distance of about 10 cm and air-dry the plate. Spot 5 μL each of the test solution and the standard solution on a plate of silica gel with fluorescent indicator for thin-layer chromatography. Polygonatum kingianum Coll.5 g of pulverized Polygala Root. with coarse longitudinal wrinkles and with deep lateral furrows cracked to some degree here and there: It is brittle and fractured surface is not fibrous. Identification Add 20 mL of water to the 2 mg of pulverized Pogostemon Herb.3 mL (50. Perform the test with the test solution and the standard solution as directed under the Thin-layer Chromatography. 4 cm to 9 cm in length and 3 cm to 7 cm in width. Pogostemon Herb is grayish white pubescent on both surfaces apex short-acute or obtuse-rounded. add 30 mL of water and 20 mL of dichloromethane. add 30 mL of a solution of hydrochloric acid in ethanol (1 in 10). add 2 mL of acetic anhydride.5 mL of dinitrophenylhydrazine solution and shake well: it becomes turbid brown. Polygala Root Polygalae Radix Polygala Root is the root of Polygala tenuifolia Willdenow (Polygalaceae).0%. Essential Oil Content Not less than 0.0% (6 hours). long and curved. coated with soft hairs. allow to stand for 2 minutes and filter. and use each of the filtrates as the test solution and the standard solution. shake and separate the dichloromethane layer. et Hemsley or Polygonatum cyrtonema Hua. Repeat this procedure with the water layer. Description Pogostemon Herb is the aerial part. fractured surface is pale brown.5% Extract Content Dilute ethanol-soluble extract— Not less than 17.0% Ash Nor more than 5. Add 1 mL of Fehling’s TS to 3 mL of this solution and heat: red precipate appears Ponciri Fructus Immaturus Ash Not more than 5.5 g of pulverized Poncirus Immature Fruit. Under a microscope. Identification 1) Drop the ammonia TS to the pulverized Polygonum Multiflorum Root: a deep red color Loss on Drying Not more than 14. Poncirus Immature Fruit has characteristic odor and bitter taste. Vascular bundles are collateral or amphivasal bundles. weigh 10 mg of Poncirin RS. appears. heat and filter. A transverse section is pale milky yellow to pale brown. allow to stand for 30 minutes and filter. shake well. a transverse section reveals phloem broadly is scattered.5 g each of pulverized Poncirus Immature Fruit and Poncirus Immature Fruit RMPM.0% Polygonum Multiflorum Root Polygoni Multiflori Radix Polygonum Multiflorum Root is the tuber of Polygonum multiflorum Thunberg (Polygonaceae). respectively.0% Acid-insoluble Ash Not more than 1. methanol and water (30 : 10. heat on a water bath for 2 minutes and filter.KP VIII 1075 linder or tubercle-shaped rhizome. dissolve in 10 mL of methanol and use this solution as the standard solution. The lower part bears prominent root scars. 3 cm to 10 cm in length and 5 mm to 30 mm in diameter. Poncirus Immature Fruit. and numerous vascular bundles and mucilage cells are scattered in parenchyma tissue. Epidermal side of the transverse section is yellowish brown. 3 cm to 10 cm in diameter. with ring shaped transverse nodes. Texture is hard and tenacious. Mucilage cells contain raphides of calcium oxalate. External surface is brown to deep brown. Deve1op the plate with a mixture of dichloromethane. Acid-insoluble Ash Not more than 1. Use the filterates as the test solution and the standard solution of Poncirus Immature Fruit RMPM. add sodium hydroxide TS to neutralize. 5 cm to 15 cm in length. semi-translucent and horny with numerous yellowish white small spots. Spray the vanillin sulfuric acid TS to the plate.5 : 1) to a distance of about 10 cm and air-dry the plate. Description Poncirus Immature Fruit is almost ballshaped. Separately. To 1 mL of the filtrate. inner side is pale grayish-brown and the center is composed of about 8 small cells.0% Poncirus Immature Fruit Poncirus Immature Fruit is the unripe whole fruit or halved fruit of Poncirus trifoliata Rafinesque (Rutaceae). add 2 mL of acetic anhydride. add 10 mL of water.5 mL of sulfuric acid:a reddish brown color appears at the zone of contact. Identification 1) Weigh 0. Vessels in xylem is almostly round and parenchymatous cells contain cluster of calcium oxalate.0%. with thich horizontal wrinkles and thin longitudinal wrinkles. add carefully 0. 2) Weigh about 2 g of Polygonum Multiflorum Root. the standard solution of Poncirus Immature Fruit RMPM and the standard solution as directed under the Thin-layer Chromatography. cambium is in a ring. The upper part of the node shows stem scar orbiculate with a sunken circumference. when dried. with subrounded abnormal vascular bundles forming brocaded patterns. 2) Weigh 0. sometimes unriped seed is contained. sometimes furcated. several scale nodes and thin longitudinal wrinkles. External surface is reddish brown to blackish brown. 2) Weigh 1 g of pulverized Polygonatum Rhizome. unripe fruit. the standard solution of Poncirus Immature Fruit RMPM and the standard solution on a plate of silica gel for thin-layer chromatography.28). Perform the test with the test solution. heat gently for 2 minutes and filter. each cell is yellowish brown and dented. Under a microscope. Add 0. To the filtrate. . Polygonum Multiflorum Root is odorless and tastes slightly bitter and astringent.1g of magnesium powder and 1 mL of hydrochloric acid to the 5 mL of the filtrate: the liquid becomes reddish purple.5 g of pulverized Polygonatum Rhizome. contains not less than 2. Add 1 to 2 droplets of the ferric chloride TS to 1 mL of the filtrate: a purple to blue color develops Identification 1) Weigh 0. heat carefully for 2 minutes and filter. a transverse section reveals epidermis is covered with cuticle. Spot 10 μL each of the test solution. Description Polygonum Multiflorum Root is fusiform or massive tuber. heat the plate at 105 o C for 10 minutes. add 10 mL of dilute hydrochloric acid. add 10 mL of ethanol.0% of poncirin (C28H34O14: 594. Polygonatum Rhizome has slight burning smell and tastes sweet and viscous on chewing. coarse and has a number of dented spots due to the oil cavity. 1 cm to 2 cm in diameter. External surface is yellowish brown-dark brown. add 10 mL of the methanol. parenchyma tissue lies inside of epidermis. 5 mL of acetic anhydride and add 1 drop of sulfuric acid: a pale red color develops.3 cm in thickness. Paikbupyun⎯Select the large and uniform Yibuja. (2) Jebuja (Processed Aconite)-Heuksoonpyun⎯ Select the large and uniform Yibuja. Ash Not more than 1. Poria Poria Sclerotium Poria is the sclerotium of Poria cocos Wolf (Polyporaceae). Mobile phase: From a mixture of methanol and water at the ratio of 30 : 70.0%. Stain the slices dark brown by immersing in caramel solution and steam until the slices turn to be oily and lustrous. packed with octadecylsilyl silica ge1 (5 μm to 10 μm in particle diameter). Select the large and uniform Yibuja. peel the bark and cut longitudinally into slices about 0. Amount (mg) of poncirin (C28H34O14) A = amount (mg) of Poncirin RS × T AS Operating conditions Detector: An ultraviolet absorption photometer (wavelength: 313 nm). but brittle. Boil the Yibuja in edible brine thoroughly. One spots among those spots from the test solution and a yellowish brown spot from the standard solution show the same color and the same Rf value. Bake the slices to half-dryness and then sundry or bake to complete dryness. about 10 cm to 30 cm in diameter and up to 0. they are classified into the following varieties: Yumbuja (Salted Aconite). (3) Pobuja (Boiled Aconite)⎯Take Yumbuja and immerse in water. Jebuja (Processed Aconite) and Pobuja (Boiled Aconite). Method of preparation (1) Yumbuja (Salted Aconite)⎯Collect daughter root of Aconitum carmichaeli in late June to early August and remove parent root. cut longitudinally into slices about 0.6%. warm in a water-bath for 2 minutes with shaking and filter. wash with water and immerse overnight in brine. add diluted methanol (7 in 10) to make 100 mL and use this solution as the test solution.0%. After immersing and rinsing in water. It is known as Heuksoonpyun. wash with water and immerse for several days in edible brine. 4 mm to 6 mm in inside diameter and 15 cm to 25 cm in length. Replace the water 2 to 3 times a day . Poria is nearly odorless. which fissures. add 60 mL of diluted methanol (7 in 10). Remaining outer layer is dark brown to dark reddish brown. coarse. Part II The spots from the test solution and the spots from the standard solution of Poncirus Immature Fruit RMPM show the same color and the same Rf value. usually as broken or chipped pieces. It is known as Yumbuja. increase the methanol content 1% per minute up to 20 minutes. Add salt. slightly tasteless and slightly mucous. Column temperature: A room temperature. Acid-insoluble Ash Not more than 0. Prepared Aconite Aconiti Lateralis Radix Preparata Prepared Aconite is the prepared daughter root of Aconitum carmichaeli (Ranunculaceae). According to the method of preparation. rinse in water completely. Repeat the above process and gradually prolong the time for dryness until a lot of salt is crystallized on the surface of the drug and its texture becomes hard. Take out. of poncirin for the test solution and the standard solution.1 kg to 2 kg in mass. Identification (1) Weigh 1 g of pulverized Poria. wash with water and immerse for several days in edible brine. weigh accurately about 20 mg of Poncirin RS. It is known as Yibuja. then increase the methanol content 2% per minutes until the ratio reaches 70 : 30. sun-dry to halfdryness and sun-dry completely. The inside is white or slightly reddish white. Flow rate: 1. The texture is hard. add 5 mL of acetone. extract under a reflux condenser in a water-bath for 2 hours and filter. take out. Assay Weigh accurately about 0.1076 Monographs. Description Poria is mass. rootlet and soil. Combine the whole filtrates. (2) Take a section or powder of Poria and add 1 drop of iodine TS: a deep red-brown color is produced. Take out. Column: A stainless steel column. Perform the test with l0 μL each of the test solution and the standard solution as directed under the Liquid Chromatography according to the following operating conditions and determine the peak areas. Immerse and rinse in water once again. respectively. It is known as Paikbupyun. steam thoroughly.5 cm in thickness. dissolve the residue in 0. immerse and take out and sun-dry. Evaporate the filtrate to dryness. AT and AS.5 g of pulverized Poncirus Fruit. Ash Not more than 7. which changes immediately to dark green. Separately. dissolve in diluted methanol (7 in 10) to make 100 mL and use this solution as the standard solution. Repeat the above procedure with the residue using 30 mL of diluted methanol (7 in 10). Boil the Yibuja in edible brine thoroughly.0 mL/minute. 25 mol/L sulfuric acid solution. and semi-translucent. when dried. Transversely cut surface is grayishbrown. Acid-insoluble Ash Not more than 2. Description (1) Yumbuja (Salted Aconite)⎯ Yumbuja is the processed daughter root. Repeat the above process with the residue. ammomum fruit and citrus unshiu peel. Weigh accurately about 10 mg of 5Hydroxymethyl-2-furaldehyde RS. Boil the desalted Yumbuja with the Licorice Root and black bean until the slice becomes numbless to a tongue. cut longitudinally. 2 mm to 5 mm in thickness. 17 mm to 50 mm in length. Take it out and sun-dry. Repeat the above process until the inside and outside of the root becomes blackish and shiny and until the texture becomes soft and flexible. yellowish-white. Separate the acid solution and determine the spectrum of the solution as directed under the Ultraviolet-visible Spectrophotometry: the spectrum exhibits maximum between 231 nm and 274 nm. add 30 mL of ether and 5 mL of ammonia TS. Prepared Rehmannia Root has slightly characteristic odor and the sweet taste. The texture is soft and flexible. Description Prepared Rehmannia Root is the steamed root as an irregular mass. shake for 10 minutes. with irregular shape and size of 3 mm to 5 mm in thickness or logitudinally sliced in 2 to 3 pieces. lustrous and sticky. dissolve in 100 mL of methanol and use this solution as the standard solution. Add 10 mL of Fehling’s TS to the filtrate and heat for a while: reddish purple-reddish brown precipitate is developed. It has slight odor and tastes salty. add 20 mL of water or dilute ethanol. (3) Pobuja (Boiled Aconite)⎯Pobuja is the processed Yumbuja.5%. Extract the water layer twice with 100 mL volumes of ethylacetate. topped with depressed bud scars and encircled with tuberculated short rootlets or rootlet scars. Perform the test with the test solution and the standard solution as directed under the Thin-layer Chromatography. Prepared Rehmannia Root Rehmanniae Radix Preparata Prepared Rehmannia Root is the root of Rehmannia glutinosa Liboschitz ex Steudel (Scrophulariaceae). External surface is pale brown to dark brown or black. 4 cm to 7 cm in length and 3 cm to 5 cm in diameter. Identification Weigh 4 g of the pulverized Prepared Aconite. steam with wine. External surface is grayish-black. covered with fine powder of salt. contains not less than 0. shake for 20 minutes and filter. add 150 mL of ether.0%. Combine the filtrate. Purity Aconitine—Weigh 20 g of the pulvarized Prepared Aconite to a stoppered Erlenmeyer flask. Method of preparation Select well cleaned rehmannia root. add 20 mL of 0. Develop the plate with a mixture of hexane and ethylacetate (1 : 1) to a distance of about 10 cm and air-dry the plate. oily and lustrous. uneasily broken and the fracture is black and lustrous. extract twice with 200 mL volumes of hexane and discard the hexane layer. with various size. with the application of steaming. Ash Not more than 6. Assay Weigh accurately about 2 g of finely cut Prepared Rehmannia Root. about 3 mm in thickness. Spray evenly Dragendorff’s TS on the plate: the spot of the test solution is not more dense than that of the standard solution. Evaporate the ether layer to dryness. Fractured surface is horn-like. The outer bark is blackish-brown and the cut surface is darkish yellow. Identification Weigh 1 g of the Prepared Rehmannia Root. Paikbupyun⎯Paikbupyun is the processed daughter root. Dissolve the residue in 2 mL of dehydrated ethanol and use this solution as the test solution. showing small clefts filled with fine powder of salt and a polyangular cambium ring and vascular bundles are arranged irregularly inside the ring. Remaining water layer is evaporated under reduced pressure until the volume is less than half of the initial volume. translucent and shows longitudinal vascular bundles. Take out. shake and stand. Steamed Rehmannia Root. Perform the test with 10 μL each of the test solution and the standard solution as directed under the . Transfer the filtrate to a separatory funnel.11). (2) Jebuja (Processed Aconite)-Heuksoonpyun⎯ Heuksoonpyun is the processed daughter root. 9 mm to 30 mm in width.1% of 5hydroxymethyl-2-puraldehyde (C6H6O3: 126. dissolve in 10 mL of ethanol and use this solution as the standard solution. conical. wide in the upper part and narrow in the lower part. Texture is hard and semi-translucent and it is slightly lustrous. extract with a reflux condenser for 3 hours and filter. add 100 mL of diluted methanol (1 in 2). Spot 5 μL each of the test solution and the standard solution on a plate of silica gel for thin-layer chromatography. It is known as Pobuja. shake for 30 minutes and allow to stand for 1 to 2 hours.KP VIII 1077 until the salt is completely rinsed out from the Yumbuja. External surface is black. Texture is heavy and hard. It has slight odor and its taste is weak. Separately weigh 20 mg of Aconitine RS. shake well and filter. the extract is combined and is evaporated under reduced pressure. remove the periderm and make slices or cut into 2 to 3 pieces and sun-dry. Texture is hard and fragile. numb and pungent. add 10 mL of ammonia TS. The residue is dissolved in methanol to make 20 mL and use this solution as the test solution. The former are irregular hexagons of about 0. 3 cm to 6 cm in length and 10 mm to 15 mm in diameter. Prunella Spike Prunellae Spica Prunella Spike is the spike of Prunella vulgaris Linné var. Pueraria Root Pueraria Radix Pueraria Root is the root. The phloem shows light grayish yellow.0%. a transverse section reveals fiber bundles accompanied by crystal cells in phloem.0%. And starch grains numerous in parenchyma is mainly composed of 9 to 12 μm polygonal simple grains. for the test solution and the standard solution. rarely 2 to 3compound grains with hilum or cleft in the center. Description Pueraria Root is the root and is usually cut into small pieces or cut into long rectangle-like pieces. ethyl acetate and acetic anhydride (20 : 6 : 8. 5 cm to 10 cm in width. Separately. add 20 mL of ethanol.38). Identification Weigh 2 g of pulverized Pueraria Root or Pueraria Root RMPM. the transverse section shows concentric annulate ring or part of it formed by abnormal growth of cambium.5 : 0. and shake for 2 minutes. Column: A stainless steel column. calculated on the dried basis. dissolve in 1 ml of methanol and use this solution as the standard solution. Perform the test with the test solution. Spot 2 μL each of the test solution and the standard solution on a plate of silica gel for thin-layer chromagraphy. Pueraria Root contains not less than 2. weigh 1 mg of Puerarin RS. lilacina Nakai or Prunella vulgaris Linné (Labiatae).0%. Column temperature: 25 o C . Acid-insoluble Ash Not more than 5. and use the filtrate as the test solution or Pueraria Root RMPM standard solution.1078 Monographs.0 mL/minute. and texture is light.Hydroxymethyl . of Pueraria lobata Ohwi (Leguminosae). take 1 mg of Ursolic acid RS.0% of puerarin (C21H20O9: 416. Mobile phase: A mixture of water and acetonitrile (95 : 5). Pueraria has slight odor and it tastes slightly sweet. Identification Weigh 1 g of pulverized Prunella Spike. Separately. heat on a water bath for 1 hour under a reflux condenser and filter. (2) Foreign matter—The amount of foreign matter other than the stems contained in Prunella Spike is not more than 1. Prunella Spike is almost odorless and tasteless. External surface is grayish brown to reddish brown. packed with octadecylsilyl silica ge1 for liquid chromatography (5 μm to l0 μm in particle diameter). Medullary rays are slightly dented. Spray evenly diluted sulfuric acid TS on the plate and heat at 105 o C for l0 minutes: One spot of the several spots from the test solution and the reddish spot spot from the standard solution show the same color and the same Rf value.0%. Develop the plate with a mixture of cyclohexane. and vertical section shows longitudinal patterns formed alternately by fibrous xylem and parenchyma. 20 cm to 30 cm in length.5) to a distance of about 10 cm and airdry the plate.hydroxymethyl . dissolve the residue to 1 mL of ethanol and use the solution as the test solution. Purity (1) Stem—The amount of the stems contained in Prunella Spike is not more than 5. respectively. Under a microscope.2 . Under a magnifying glass. add 10 mL of methanol. Amount (mg) of 5 . It is easily breakable lengthwise. and the latter are plate-like pieces. Evaporate the filtrate to dryness. filter. shake for 3 minutes. dissolve the residue to 15 mL of petroleum ether. Flow rate: 1. and its section extremely fibrous.2 . Part II Liquid Chromatography according to the following operating conditions and determine the peak areas. and the xylem shows numerous vessels appearing as small dots. 4 mm to 6 mm in inside diameter and 15 cm to 25 cm in length. Ash Not more than 13. Pueraria Root RMPM standard solution and the standard solu- . Spikes are composed of a floral axis having numerous bracts and calyxes. AT and AS. External surface is grayish white to pale brown. longitudinal wrinkled and coarse. as on the calyx. distinct vessels and xylem fibers in xylem. Bract is cordate to eccentric and exhibiting white hairs on the vein. and about l cm in thickness. Remove the petroleum ether layer. and also with striae. Corollas are often remained on the upper part. Perform the test with the test solution and the standard solution as directed under Thin-layer Chromatography.5 cm cube. Description Prunella Spike is spike in nearly cylindrical and wheat ear-like shape. dichloromethane. add 1 mL of ethanol and use the solution as the standard solution. with or without periderm.furaldehyde RS A 1 × T× AS 5 Operating conditions Detector: An ultraviolet absorption photometer (wavelength: 280 nm).furaldehyde (C 6 H 6 O 3 ) = amount (mg) of 5 . A calyx usually enclosed four mericarps. cool. Crown is somewhat constricted and sometimes with short remains of stem. respectively. Amount (mg) of puerarin (C 21 H 20 O 9 ) = amount (mg) of Puerarin RS × AT × 10 AS Operating conditions Detector: An ultraviolet absorption photometer (wavelength: 254 nm). Ether-soluble extract—Not less Red Ginseng Ginseng Radix Rubra Red Ginseng is the root of Panax ginseng C. and 2 mm to 3 mm in width. of puerarin of the test solution and the standard solution. Column temperature: An ordinary temperature. External surface is yellowish brown to reddish brown. Take 10 mL of this solution. AT and AS.01) and not less than 0. Loss on Drying Not less than 13. Fractured surface is flat. boil gently under a reflux condenser in a water-bath for 15 minutes. Raphanus Seed is odorless and the taste is weak. add 30 mL of methanol. Ash Not more than 6. the spots from the test solution and the spots from Pueraria Root RMPM standard solution show the same color and the same Rf value. Description Red Ginseng is thin and long cylindrical to fusiform root. Spot 2 μL each of the test solution. dissolve 1 mg of Ginsenoside Rg1 RS in 1 mL of methanol and use this . Raphanus Seed Raphani Semen Raphanus Seed is the ripe seed of Raphanus sativus Extract Content than 31.0% (6 hours). (2) Weigh 2 g of pulverized Red Ginseng.0%. Assay Weigh accurately 2 g of pulverized Pueraria Radix. with a deep brown round hilum at one end and several longitudinal furrows on one side under a magnifying glass. Separately. with reddish brown substance inside and endosperm flattened in a line. Red Ginseng has characteristic odor and taste. External surface is pale yellow-brown to red-brown and semitranslucent and with longitudinal wrinkles and with thin scars. and filter. coryledons is 2. Testa is thin and brittle. Loss on Drying Not more than 8. Examine under ultraviolet light (main wavelength: 365 nm). Flow rate: 1. Texture is horny and hard. extract under a reflux condensor for 2 hours. A. slightly flattened. and water (12 : 2 : l) to a distance of about 10 cm. calculated on the basis of dried material.0%. To the residue. subovoid or ellipsoidal. often branching out into 2 to 3 lateral roots from the middle. Meyer (Araliaceae). and air-dry the plate. add gently 0.20% of ginsenoside Rb1 (C54H92O23: 1109. Pipet 10 μL each of the test solution and the standard solution.5 mL of sulfuric acid to make two layers: a red–brown color develops at the zone of contact.10% of ginsenoside Rg1 (C42H72O14: 801. Pueraria Root RMPM standard solution and the standard solution on a plate of silica gel with fluorescent indicator for thinlayer chromatography. add 2 mL of acetic anhydride. with starch grains inside. methanol. 2. and use this solution as the test solution. add 20 mL of methanol.5 mm to 4 mm in length. Mobile phase: A mixture of methanol and water (25:75).2 g of pulverized Red Ginseng. Column: A stainless column. add 60 mL of methanol. yellowish white and oily.0%. Description Raphanus Seed is theseed. Red Ginseng is 5 cm to 25 cm in length. add methanol to make exactly 100 mL. transverse section reveals a pigment layer adhering to palisade layer and atrophying. Deve1op the plate with a mixture of ethyl acetate. and perform the test as directed under the Liquid Chromatography according to the following operating conditions.of root. Under a microscope. warm in a water-bath for 2 minutes and filter. at first slightly sweet. followed by a slight bitterness. main root is 5 to 30 mm in diameter.0%.KP VIII 1079 Linné (Cruciferae). slightly bitter and pungent. after being steamed. Acid-insoluble Ash Not more than 1.0%. filter and use the filtrate as the test solution.29). dissolve in methanol to make exactly 100 mL. 4 to 6 mm in inside diameter and 15 to 25 cm in length. It contains not less than 0. and one spot among the spots from the test solution and a fluorescent bluish white spot from the standard solution show the same color and the same Rf value. To 1 mL of the filtrate. and use this solution as the standard solution. Separately. packed with octadecylsilyl silica gel for liquid chromatography (5 to 10 μm in particle diameter). Combine all the filtrates and add methanol to make exactly 100 mL. and proceed in the same manner. or grayish brown. tion as directed under the Thin-layer Chromatography. Identification (1) Weigh 0. weigh accurately 10 mg of Puerarin RS. Ash Not more than 7.0 mL/min. Determine the peak areas. Part II solution as the standard solution. Loss on Drying Not more than 15. calculated on the dried basis. 1 mm to 3 mm in diameter and arranged in a ring or scattered irregularly. the patterns is often radiate and pith consists of whirls of tissues radiated from the center of a small brown circle.5%. with deep. externally dark brown or blackish-red and with coarse wrinkles. Under a magnifying glass. respectively. fine reticulations. methanol and water (14 : 6 : 1) to a distance of about 10 cm and air-dry the plate. In the case of Rhubarb with cork layer. cortex composed entirely of parenchyma cells and scattered cells containing brown secretes in outer region of cortex.0%. a transverse section reveals yellowish brown to blackish brown. and often broken or markedly deformed in shape. 5 mm to 15 mm in diameter. In the case of Rhubarb without most part of cortex. Xylem practically filled with parenchyma cells and vessels are radially lined. often cut crosswise or longitudinally.72). and perform the test as directed under the assay of [Ginseng] Rehmannia Root Rehmanniae Radix Rehmannia Root is the root of Rehmannia glutinosa Liboschitz ex Steudel (Scrophulariaceae). having patterns of dark brown tissue complicated with white and pale brown tissues. 4 cm to 10 cm in diameter and 5 cm to 15 cm in length.0%.0%. Ash Not more than 6. add 20 mL Purity Foreign matter⎯Rehmannia Root does not contain stems. and lenticel. and texture is rough and brittle. Description Rehmannia Root is conical to fusiform root. heat the plate at 105 o C for 10 minutes. from which periderm has been removed. Perform the test with the test solution and the standard solution of Rehmannia Root RMPM as directed under Thin-layer Chromatography. Rhubarb contains not less than 0. and perform the test as directed under the assay of [Ginseng] 2) Ginsenodise Rb1—Use the solution of 1) as the test solution. External surface is yellow-brown to blackbrown. Under a microscope. The texture is soft and breakable. and slightly sweet taste at first and followed by a slight bitterness. Rheum tanguticum Maximowicz ex Balf. Concentrate the filtrate to 5 mL by evaporationg and use these solutions as the test solution and the standard solution of Rehmannia Root RMPM. and texture is thick and hard. the cambium-rings produce phloem inside and xylem outside. Identification Weigh 2 g each of pulverized Rehmannia Root and Rehmannia Root RMPM. The fractured surface is not fibrous. Spray the anisaldehyde TS to the plate. sand and other foreign matters. Purity Foreign matter—The amount of stems and other foreign matter contained in Red Ginseng is not more than 2. the outer surface is flat and smooth. of methanol. yellowbrown to pale brown and sometimes exhibiting white. ovoid. Develop the plate with the lower layer of a mixture of chloroform. Extract Content Dilute ethanol-soluble extract— Not less than 18. oblong-ovoid or cylindrical. Perform the test with the test solution and the standard solution as directed under the Thin-layer Chromatography. Rehmannia Root has characteristic odor. Spot 10 μL of the test solution and the standard solution of Rehmannia Root RMPM on a plate of silica gel for thin-layer chromatography. spray evenly sulfuric acid TS for spray on the plate and heat at 110 o C for 5 minutes: one spot among the spots from the test solution and a red-purple spot from the standard solution show the same color and the same Rf value. small cambium-rings scattered here and there in the pith.25% of sennoside A(C42H38O20 : 862. Several spots from the test solution and the spots from the standard solution of Rehmannia Root RMPM show the same color and the same Rf value. Near the cambium. A transverse section is grayish brown. accompanied with 2 to 4 rows of medullary rays containing brown-colored substances and the . laterally scars of lateral roots. pale grayish brown or brown. 5 cm to 15 cm in length. mainly reticulate vessels. Assay 1) Ginsenoside Rg1—Weigh 1 g of pulverized Red ginseng. Acid-insoluble Ash Not more than 2. and Rheum officinale Baillon (Polygonaceae) ). Spot 10 μL each of the test solution and the standard solution on a plate of silica gel for thin-layer chromatography. Rhubarb Rhei Radix et Rhizoma Rhubarb is usually the root and rhizome of Rheum palmatum Linné. a transverse section reveals 7 to 15 layers of cork. heat on a water bath for 1 hour under a reflux condenser and filter. Develop the plate with a mixture of dichloromethane. methanol and water (13 : 7 : 2) to a distance of about 10 cm.5% (6 hours) Ash Not more than 4.0%. longitudinal wrinkles. Under a microscope. hardly observable pith. the transverse section reveals mostly parenchyma cells. cortex darker than xylem in color.1080 Monographs. Description Rhubarb is the root and rhizome. 3 and 0. sennoside A and naringin are eluted in this order with the resolution between their peaks being not less than 3. brown-colored substances or crystal druses of calcium oxalate. sinica Rehder et Wilson (Anacardiaceae).5 g of pulverized Rhubarb.KP VIII 1081 rays run radially from the center of the ring towards the outside forming whirls of tissues. respectively.0 mL of this solution. Amount (mg) of sennoside A (C 42 H 38 O 20 ) = amount (mg) of Sennoside A RS × AT × 0. When the procedure is run with 20 μL of this solution under the above operating conditions.5 g of pulverized Rhubarb.0%. shake for 30 minetes. though a bluish white fluorescence may appear. n-butanol and methanol (26 : 7 : 7) to a distance of about 10 cm and air-dry the plate. Develop the plate with a mixture of isopropyl ether. Var.0. Assay Weigh accurately about 0. Rhubarb has characteristic odor and slightly astringent and bitter taste. water and acetic anhydride (40 : 40 : 30 : 1) to a distance of about 15 cm and air-dry the plate. Rhus Galls Galla Rhois Rhus Galls is the gall produced mainly by parasitic aphids of Schlechtendalia chinensis Bell (Pemphigidae). Perform the test with the test solution and the standard solution as directed under the Thin-layer Chromatography. not more than 0. Develop the plate with a mixture of ethyl acetate. heat in a water-bath with a reflux condenser for 10 minutes and filter. dissolve in sodium bicarbonate solution (1 in 1000) to make exactly 50 mL. Flow rate: Adjust the flow rate so that the retention time of sennoside is about 15 minutes. dissolve 1 mg of Sennoside A RS in 4 mL of a mixture of tetrahydrofuran and water (7 : 3).67 kPa.5 by adding l mol/L hydrochloric acid TS. add 30 mL of tetrahydrofuran. Loss on Drying Not more than 13. Perform the test as directed under the Thin-layer Chromatography. it is gritty between the teeth and coloring the saliva yellow. on the leaf of Rhus javanica Linné. Medullary rays are linear with 1 to 2 rows in Rheum palmatum. According to its from the drug is divided into Dubai and Gagbai. The parenchyma cells contain starch grains. Rhus potaninii Maximowicz or Rhus punjabensis Stew. 4 mm to 6 mm in inside diameter and 15 cm to 25 cm in length. Column: A stainlee steel column. Column temperature: A constant temperature of about 40 o C . System suitability System performance: Dissolve 1 mg each of Sennoside A RS and Naringin RS in sodium bicarbonate solution (1 in 1000) to make 10 mL. Separately. Transfer this solution to another separatory funnel.0% (6 hours). add 50 mL of sodium bicarbonate TS (1 in 1000). packed with octadecylsilyl silica gel for liquid chromatography (5 μm to 10 μm in particle diameter).0%. add 13 g of sodium chloride and shake for 30 minutes. curved with 2 to 4 rows in Rheum tanguticum. npropanol. separate the tetrahydrofuran layer and use this solution as the test solution.6. P2O5). When chewed. Ash Not more than 13. weigh accurately 10 mg of Sennoside A RS. Acid-insoluble Ash Not more than 2. shake for 30 minutes and centrifuge. Pipet 5. dry Sennoside A RS for more than 12 hours in the desiccator (in vacuum. Determine the peak areas. add 10 mL of ethanol. Examine under ultraviolet light (main wavelength: 365 nm): one of the spots from the test solution and a red fluorescent spot from the standard solution show the same color and the same Rf value.25 AS Operating conditions Detector: An ultraviolet absorption photometer (wavelength: 340 nm). Description (1) Dubai-Rhus Galls from Dubai is the . of sennoside A of the test solution and the standard solution. Separately. Purity Raponticin—Weigh 0. using the filtrate as the test solution. Spot 10 μL of the test solution on a plate of silica gel with fluorescent indicator for thin-layer chromatography. filter and use the filtrate as the test solution. Transfer the supernatant liquid to a separatory funnel. System repeatability: When the test is repeated 6 times with the standard solution under the above operating conditions: the relative standard deviation of the peak area of sennoside A is not more than 1. and use this solution as the standard solution. Examine under ultraviolet light (main wavelength: 365 nm): no spot with blue-purple fluorescence is observed at an Rf value between 0. Mobile phase: A mixture of diluted acetic acid (1 in 80) and acetonitrile (4 : 1). Spot 40 μL each of the test solution and the standard solution on a plate of silica gel with fluorescent indicator for thin-layer chromatography.5%. shake for 10 minutes. Identification Weigh 2 g of pulverized Rhubarb. Separate the water layer with undissolved sodium chloride and adjust the pH to 1. Perform the test with 10 μL each of the test solution and the standard solution as directed under the Liquid Chromatography according to the following operating conditions. and linear with 1 to 2 rows in Rheum officinale around pith. add sodium bicarbonate solution (1 in 1000) to make exactly 20 mL and use this solution as the standard solution. AT and AS. add 40 mL of a mixture of tetrahydrofuran and water (7 : 3). 4 mL (50. . Gall walls are relatively thin. the wall of calyx is 1 mm to 2 mm in thickness. sometimes purplish brown. Under a magnifying glass. the seed coat reveals fine wrinkles and is covered with membranous aril. with brown small scars of the fallen bristles. A dish like calyx is remained at the apex.0%. Add ferricchloride solution into the filtrate: a bluish-black precipitate is produced. 15 mm to 40 mm in diameter. Description Rosa Fruit is the fruit. each loculus containins 3 to 7 seeds joining by aril. Loss on Drying Not more than 17. pale grayish brown to dark brown. nearly ellipsoidal. Pericarp is relatively thin and seeds are thin and blighted.5 mm in width. Round Amomum Fruit Amomi Fructus Rotundus Round Amomum Fruit is the ripe fruit of Amomum kravanh Pierre ex Gagnep. Calyx is 5 lobed. Pericarp is thin. Seed is irregularly angular ovoid. To 5 mL of the filtrate. 2 mm to 3 mm in length and 1 mm to 1. Acid-insoluble Ash Not more than 5. The seed of Round Amomum Fruit has strong aroma and extremely hot. Rubus Fruit is odorless. Purity Foreign matter⎯ Round Amomum Fruit contains not more than 2. Essential Oil Content 0. Rosa Fruit has slight odor and sweet and slightly astringent taste. fruit stalk and other foreign matter.Round Amomum Fruit is the fruit. Extract Content Dilute ethanol-soluble extract— Not less than 34.0 g) (seed). light and fibrous. Loss on Drying Not more than 12. Identification Weigh 0. Interior is longitudinally divided into three loculi by thin membranes. 5 mm to 10 mm in diameter. like camphor. with numerous small achenes inside with yellow tomenta. obovoid.0% (seed). 20 mm to 35 mm in length and 1 cm to 2 cm in diameter. External surface is yellowish red to reddish brown. Ash Not more than 5. with a scar of fruit stalk.0% of fruit stalk and bristle. External surface is yellowish gray. remaining a scar of stigma. slightly pubescent. Inner surface of gall is smooth and contains black-brown killed aphids and gray excreta. and the dorsal side of seed protrudes in arc shape. Rhus Galls from dubai has characteristic odor and astringent taste (2) Gagbai-Rhus Galls from Gagbai is the rhombic gall with irregular obtuse branchings and distinct pubescences. On cutting. Rubus Fruit Rubi Fructus Rubus Fruit is the unripe fruit of Rubus coreanus Miquel (Rosaceae). Drupelets are easily fallen. lustrous with 2 mm to 3mm thick of gall wall. and filter. brown. Purity Fruit stalk—Rosa Fruit contains less than 2.0%. lunate. covered with numerous. add a little of magnecium powder and 2 to 3 drops of hydrochloric acid: the color develops deep red.0% Rosa Fruit Rosae Laevigatae Fructus Rosa Fruit is the ripe fruit of Rosa laevigata Michaux (Rosaceae). Texture is hard and fragile. The upper part is protrudent and the lower part has a dented scar of fruit stalk.5 g of pulverized Rubus Fruit. Fractured surface is hornylike. (2) Amomum compactum . Identification Weigh 0.0%. and the taste is slightly sour and astringent. External surface is pale yellow-white to yellow-brown with three blunt ridges and many longitudinal lines. external surface of drupe is yellowish green to yellowish brown. macerate with 10 mL of water. One end is sharped. Ash Not more than 5. with a yellow stalk base in the middle and the lower part is gradually tapered.Round Amomum Fruit is the fruit. Round Amomum Fruit has week odor and taste. or Amomum compactum Solander ex Maton (Zingiberaceae). easily broken. External surface is grayish brown. Under a magnifying glass. Description (1) Amomum kravanh . Description Rubus Fruit is the fruit as aggregate consisting of numerous small drupes. smaller than Amomum kravanh. mostly round and 7 mm to 9 mm in diameter. small and dented dots with netty and prominent ridges. Part II oblong or spindle-globular gall. 25 mm to 90 mm in length. light and hard. add 10 mL of ethanol. Texture is hard.0% of the capsule.0% (seed). 1 cm to 2 cm in length. 3 mm to 4 mm in diameter. External surface is dark brown or greenish brown.1082 Monographs. heat for about 2 minutes and filter.5 g of pulverized Rhus Gallas. Examine the plate under ultraviolet light (wavelength: 365 nm). The pressed slab is about 5 mm in thickness. add 5 mL of 80% solution of acetone. (2) Glycerol. pale red. Total length is about 1 cm. containing 3 mL of water and allow the paper to soak up the water for 1 hour: most of the upper part of the paper is colored pale yellow and the lower volume. Packaging and Storage well-closed containers. Use these solutions as the test solution and the standard solution of Safflower RMPM. stems. with the end of partite part widened and the other end narrowed gradually. Packaging and Storage well-closed containers. Extract Content Dilute ethanol-soluble extract— Not less than 20. It is dark yellowish red to reddish brown. respectively. shake for 15 minutes and filter.4) to a distance of about 10 cm and air-dry the plate. To 1. add 150 mL of warm water. boil with 10 mL of dilute ethanol under a reflux condenser for 15 minutes and after cooling. Under a microscope. Saffron has strong and characteristic odor. Pollen grains are yellow and approximately spherical. (2) Crocin—Dry Saffron in a desiccator (silica gel) for 24 hours and powder. consists of a collection of numerous corollas. sugar or honey—Saffron has no sweet taste.0%.0 mL of the filtrate. Deve1op the plate with a mixture of ethyl acetate. Ash Not more than 8. Salvia Miltiorrhiza Root Salviae Miltiorrhizae Radix . The several spots from the test solution and the spots from the standard solution of Safflower RMPM show the same color and the same Rf value. about 50 μm in diameter. Ash Not more than 7.1 g of pulverized Saffron. tripartite or separate. Transfer and immediately hang the paper in another glass vessel of the same type. thin cord-like shaped. Loss on Drying Not more than 12. Press it between two pieces of paper: no spot is left on the paper.0% (6 hours). when softened by immersion in water. Preserve in light-resistant.5 g each of pulverized Safflower and Safflower RMPM. with fine protrusions on the surface. 20 mm to 35 mm in length. (3) Yellow style—The yellow style in Saffron is not more than 10. water and methanol (7 : 2 : 3 : 0. Safflower Preserve in light-resistant. leaves and other foreign matter is not more than Saffron is the stigma of Crocus sativus Linné (Iridaceae). Description Saffron is the stigma. Spot 5 μL each of the test solution and the standard solution of Safflower RMPM on a plate with fluorescent indicator for thin-layer chromatography.0%. Purity Foreign matter—The amount of ovaries. Corolla is tubular and with 5 lobes and 5 stamens surround long pistil. Weigh 0.KP VIII 1083 2. bitter taste and the color of saliva becomes yellow. Description Safflower is the tubulous flower.0%. yellow style and stamen. Safflower has characteristic odor and slightly bitter taste.0%. warm the mixture between 60 °C and 70 °C for 30 minutes with frequent shaking and filter. Purity (1) Aniline dyes—Shake 50 mg of Saffron with 10 mL of chloroform: the solution is colorless or only slightly yellow. dissolve it in water to make exactly l0 mL. the upper end has numerous tubular protrusions about 150 μm in length. Control solution— Weigh 5 mg of potassium bichromate. hang a piece of filter paper. with a small number of pollen grains. 2 cm in width and 30 cm in length. formic acid.0%. Identification (1) Add l drop of sulfuric acid to Saffron: The color changes to dark blue which gradually turns red–brown through purple.2 g of Safflower. Ash Not more than 18. so that one end of the filter paper reaches the bottom of the vessel and allow the paper to soak up the liquid for 1 hour. 2) Weigh 0. Perform the test with the test solution and the standard solution of Safflower RMPM as directed under the Thin-layer Chromatography. filter.5%. rarely mixed with immature ovary. add water to make 10 mL: the solution is not more intense than the following control solution. Place 3 mL of the filtrate in a small glass vessel about 30 mm in both inside diameter and height. Saffron Carthami Flos Crocus Safflower is the tubulous flower of Carthamus tinctorius Linné (Compositae). Identification 1) Weigh 0. red to red-brown corolla. 5 g of pulverized Sappan Wood. Sappan Wood Sappan Lignum Sappan Wood is the heartwood of Caesalpinia sappan Linné (Leguminosae). shake and filter.0%.0%. Extract Content Dilute ethanol-soluble extract— Not less than 25. transverse section reveals 1 or 2 to 4 xylary vessels aligned in the center and containing yellowish brown to reddish brown substances. Identification (1) Weigh 1 g of pulverized Salvia Miltiorrhiza Root. elliptical-shaped. The vessels of xylem are aligned radiately around pith and surrounded with fibers.0%. Texture is hard and fragile. Salvia miltiorrhiza Root has slight characteristic odor and slightly bitter and astringent taste. Salviae Miltiorrhizae Root is the root of Salvia miltiorrhiza Bunge (Labiatae). add 10 mL of ethanol. add 10 mL of diluted ethanol. and full of yellow secretion. Description Sappan Wood is the heartwood. In a cross section. Xylary parenchymatous cells are lignified and thickwalled. conical. mostly purplish-brown. some branched and with rootlets. fracture is loosened. long cylindrical. with the short and stout rhizome. External surface is pale brown.0%. The root reveals many longitudina1 wrinkles and scars of rootlets. The Root is long cylindrical. Extract Content Dilute ethanol-soluble extract— Not less than 20. transverse section reveals the cork cell with yellow or red pigment. sometimes with remain of a stem at the apex. Saposhnikovia Root Saposhnikoviae Radix Saposhnikovia Root is the root of Saposhnikovia diva- Description Saposhnikovia Root is the root. transverse section reveals numerous lactiferous tubes. semicylindrical or stick-like in shape. Under a microscope. Ash Not more than 7. Under a microscope. To 5 mL of filtrate. Acid-insoluble Ash Not more than 1. Saposhnikovia Root has characteristic odor and slightly sweet taste.0%. (2) Put a small piece of Sappan Wood in calcium hy- . It is often cut transversely or longitudinally. boil shortly and filter: the filtrate shows brownish yellow. The bark of old roots is loosened. Spot 20 μL each of the test solution and the standard solution on a plate of silica gel with fluorescent indicator for thin-layer chromatography. filter and use the fitrate as the test solution. usually scaling off. (2) Weigh 2 g of pulverized Salvia Miltiorrhiza Root. containing solitary crystal of calcium oxalate. 15 cm to 20 cm in length and 7 mm to 15 mm in diameter.3 cm to 1 cm in width. Phloem has large intercellular space. External surface is yellowish red to grayish brown. Ash Not more than 7. Examine under ultraviolet light (main wavelength: 254 nm) or spray evenly the plate with sulfuric acid TS for spray and heat: one spot among the spots from the test solution and a spot from the standard solution show the same color and the same Rf value. with sometimes traces of sapwood in pale brown to grayish brown. Medullary rays are composed of 1 to 2 rows in long round shape and sometimes forming lacuna on breaking.5 g of zinc powder: the filtrate turn to yellow. Part II ricata Schischkin (Umbelliferae). sonicate for 1 hour. dissolve 1 mg of tansinone II A RS in 1 mL of methanol and use this solution as the standard solution. Perform the test with the test solution and the standard solution as directed under the Thin-layer Chromatography. Under a microscope. Develop the plate with a mixture of hexane and ethyl acetate (4 : 1) to a distance of about 10 cm and air-dry the plate. showing bundles of yellowish-white vessels arranged radially. add 10 mL of methanol. Separately. Texture is hard but longitudinally cut texture is easy to be broken. Sappan Wood is nearly odorless and slightly astringent. longitudinally wrinkled. Description Salvia Miltiorrhiza Root is the root. rough. Loss on Drying Not more than 12. The upper part of rhizome reveals dense crosswise wrinkles like ring nodes and sometimes reveals brown and hair-like remains of leaf sheath. cleft or slightly even and dense. add 2 to 3 drops of sodium hydroxide TS: dark red color develops. distributed in the parenchyma cells of phloem. and the lower part is slightly thin. 8 cm to 25 cm in length and 0. with brownish-red bark and grayish-yellow or purplish-brown wood. Medullary rays is curved and developed. Add 1 mL of diluted sulfuric acid and 0. slightly curved.0% . Transversely cut surface has distinct annual rings.5%.1084 Monographs. cortex is grayish brown and reveals many lacunae and xylem is yellow. Identification (1) Weigh 0. The external surface is brownish red or dark brownish-red. Purity Foreign matter—The amount of stems and other foreign matter contained in Saposhnikovia Root is not more than 2. Loss on Drying Not more than 13. with wrinkles and occasionally with white powder. ASGA and ASGN. Flow rate: 0. the standard solution (2) and the standard solution (3) show the same color and the same Rf value. Purity Foreign matter—The amount of receptacle.0% of sapwood other than heartwood. Amount (mg) of schisandri n (C 24H32O7) = amount (mg) of Schisandri n RS × A TS 1 × A SS 5 Amount (mg) of gomisin A (C23H28O7) A 1 = amount (mg) of Gomisin A RS × TGA × ASGA 5 Amount (mg) of gomisin N (C 23H28O6) = amount (mg) of Gomisin N RS × ATGN 1 × ASGN 5 Operating conditions Detector: An ultraviolet absorption photometer (wavelength: 254 nm). heat the plate at 105 o C for 10 minutes and detect the spots from the test solution and the standard solution on the plate: the spots from the test solution and the spots from the standard solution of Schisandra Fruit RMPM show the Assay Weigh accurately about 0. of the standard solution.0%. sonicate for 20 minutes and filter. of the test solution and ASS. Perform the test with the test solution as directed under the Thinlayer Chromatography. 1 or 2 seeds are present. respectively. the standard solution (2) and the standard solution (3).5 g of the fine powder of Schisandra Fruit. externally yellow-brown to dark red-brown. External surface is dark red to blackish brown. heat on a water bath for 30 minutes under a reflux condenser.6 mL/min. same color and the same Rf value. 4 to 6 mm in inner diameter and 15 to 25 cm in length. Combine all the filtrates and add methanol to make exactly 50 mL and use this solution as the test solution. packed with octadecylsilyl silica gel for liquid chromatography (5 to 10 μm in particle diameter). The seeds are 2 mm to 5mm in length. peduncle and other foreign matter contained in Schisandra Fruit is not more than 1. kidney-shaped. ethyl acetate and formic acid (7 : 3 : 0. Determine the peak areas. add 1 mL of dichloromethane respectively and use each of this solution as the standard solution (1).1).51). Take exactly 2 mL of this solution. When removed the sarcocarp.0% Ash Not more than 5.47). External seed coat is easily peeled but internal seed coat adheres closely to the albumen. System suitability System performance: Proceed with 10 μL of the standard solution under the above operating conditions. respectively. Identification Weigh 1.KP VIII 1085 droxide TS: no purplish blue color develops. add 20 mL of methanol and proceed in the same manner. weigh accurately 10 mg of schisandrin RS.46) and gomisin N (C23H28O6: 400. Mobile phase: A mixture of acetonitrile. Spray the dilute sulfuric acid TS to the plate. Ash Not more than 2. Spot 2 μL each of the test solution and the standard solution on a plate of silica gel for thin-layer chromatography. Extract Content Dilute ethanol–soluble extract— Not less than 5. Schisandra Fruit Schisandrae Fructus Schisandra Fruit is the well ripe fruit of Schisandra chinensis Baillon (Schisandraceae). 1 mg of gomisin A RS and 1 mg of gomisin N RS. gomisin A (C23H28O7: 416.0 g each of pulverized Schisandra Fruit and Schisandra Fruit RMPM. 10 mg of gomisin A RS and 10 mg of gomisin N RS. Pipet 10 μL each of the test solution and the standard solution. add 20 mL of dichloromethane. Three spots among those spots and each spot of the standard solution (1).0% (6 hours).5) to a distance of about 10 cm and air-dry the plate. dissolve to make exactly 25 mL of methanol.0%. water and formic acid (70:30:0. Purity Sapwood – Sappan Wood contains less than 3. add exactly 20 mL of methanol and use this solution as the standard solution. add 20 mL of methanol. Description Schisandra Fruit is sap fruit of irregular sphere or spheroid. gomisin A . filter and evaporate the filterate to dryness.7% of total sum of the contents of schisandrin (C24H32O7: 432. lustrous. Schisandra Fruit has slightly odor and acidic. about 6 mm in diameter. with distinct raphe on the dorsal side. Add 1 mL of methanol to each of the residue and use these solutions as the test solution and the standard solution of Schisandra Fruit RMPM. Weigh 1 mg of schisandrin RS. and perform the test as directed under the Liquid Chromatography according to the following operating conditions. Deve1op the plate with a mixture of toluene. Separately. Column: A stainless column. Column temperature: An ordinary temperature. To residue. Schisandra Fruit contains not less than 0. later astringent and bitter taste.5%. respectively. ATGA and ATGN. ATS. Use a column giving elution of schisandrin. add 2 or 3 drops of 2.37) and scopolamine . stopper tightly. Internal standard solution—A solution of brucine in the mobile phase (1 in 2500). shake for 1 hour. add 8 mL of ammonia TS and 80 mL of ether. add 20 mL of water. Shake the mixture with 40 mL of chloroform and 1 mL of ammonia TS immediately for 2 minutes and. add Packaging and Storage Preserve in light-resistant tight containers. add 25 mL of ether. shake for 15 minutes. 5 cm to 10 cm in length. dissolve the residue with 1 mL of ethanol and proceed as directed in the Identification (2) under Scopolia Rhizome using this solution as the test solution. shake and filter after the chloroform becomes clear. water. allow to stand for 5 minutes and separate the ether layer into a porcelain dish. add 3. Dissolve the residue in 5 mL of the mobile phase.4dinitrophenylhydrazine-ethanol TS: an orange-red precipitate is formed. with calyx-tubes containing small labiate flower or often fruits and with short milky white hairs at the whole root.5 g of powdered tragacanth.4 g of Scopolia Extract.8551 Q SA 5 Scopolia Extract Amount (mg) of scopolamin e (C 17 H 21 NO 4 ) Scopolia Extract contains not less than 0. Part II and gomisin N in this order and clearly dividing each peak with the resolution between their peaks being not less than 1.0%. after standing for 4 minutes. The spike is purple-greenish brown to greenish brown. shake vigorously. Q 1 calculated on the dried basis × TS × × 0 . Scopolia Extract dissolves in water with a slight turbid. System repeatability: When the test is repeated six times with 10 μL of the standard solution under the above operating conditions: the relative standard deviation of the peak area of schisandrin.0%. = amount (mg) of Scopolamin e Hydrobromi de RS. shake well and distill. dissolve in 10 mL of water. stopper tightly. Rinse the flask with 2 mL of water and add the rising to the separatory funnel.N-dimethylformamide and add 5 to 6 drops of tetraethylammonium hydroxide TS: a redpurple to purple color is observed.5%. mix with 4 mL of water in a flask and transfer the mixture to a separatory funnel. gomisin A and gomisin N is not more than 1. add the mobile phase to the internal standard solution and add the mobile phase to make 25 mL. and has characteristic odor and bitter taste. Add 3 g of anhydrous sodium sulfate to the chloroform. (2) Weigh 0. 2.11% of total alkaloids [as hyoscyamine (C17H23NO3: 289. Ash Not more than 11. Acid-insoluble Ash Not more than 3.1086 Monographs. add 15 mL of ammonia TS and shake. centrifuge and separate the ether layer.09% and not more than 0.7894 Q SS 25 Method of preparation Extract the coarse powder of Scopolia Rhizome with 35% ethanol. Evaporate the ether on a water-bath. Identification (1) Weigh 4 g of Scopolia Extract. Schizonepeta Spike has characteristic aroma and slightly cool feeling on keeping in the mouth. place in a glass-stoppered centrifuge tube. Q 1 calculated on the dried basis × TA × × 0. Repeat this procedure twice with the water layer. add 5 drops of fuming nitric acid and evaporate on a water-bath to dryness.0 μL of the internal standard solution. drain off the chloroform layer.37) and scopolamine(C17 H21NO4: 303.6. 10% Scopolia Extract Powder 10% Scopolia extract powder contains not less than 0. Store in a cold place. To this solution. dissolve the residue in 1 mL of N. long spike.90% and not more than 1.0%. Proceed as directed under Scopolia Rhizome. Schizonepeta Spike Schizonepetae Spica Schizonepeta Spike is the spike of Schizonepeta tenuifolia Briquet (Labiatae).09% of total alkaloid [as hyoscyamine (C17H23NO3: 289. using the ether on a water-bath. After cooling. Amount (mg) of hyoscyamin e (C 17 H 23 NO 3 ) = amount (mg) of Atropine Sulfate RS. Evaporate 30 mL of the filtrate of dryness. Extract Content Dilute ethanol-soluble extract— Not less than 8. Description Scopolia Extract is brown to dark brown.35)]. Assay Weigh accurately about 0. To 3 mL of the distillate.5 g of Scopolia Extract. Description Schizonepeta Spike is a thin. or purified water and prepare the viscous extract as directed under Extracts. Identification Weigh 2 g of pulverized Schizonepeta Spike. Constrictions make the rhizome appear nodular. allow to stand for 2 minutes. Combine the extracts and evaporate the ether on a water-bath. transfer the filtrate and the washing to a separatory funnel. Method of preparation Scopolia Extract 100 g Starch. stir to mix well . (2) Weigh 2 g of pulverized Scopolia Rhizome. add 20 mL of diluted sulfuric acid (l in 50). shake for 1 hour.0 g of 10% Scopolia Extract powder. add 100 mL of ether and 7 g of sodium chloride. Filter the mixture. External surface is grayish brown to blackish brown. dissolve the residue in 1 mL of ether and use this solution as the test solution. Fractured surface is grayish white to pale brown. transverse sectioin reveals xylem with groups of vessels arranged stepwise and accompanied with xylem sieve tubes in medullary rays. using 25 mL volumes of ether.35)].KP VIII 1087 (C17H21NO4: 303. add 10 mL of ammonia TS and shake. Rarely. Scars of stem are present at upper side of each node. shake the extract with 3 g of anhydrous sodium sulfate and filter through a dry filter paper. slightly curved. Dissolve the residue in 5 mL of the mobile phase. Scopolia Rhizome Scopoliae Rhizoma Description 10% Scopolia Extract powder is a brownish yellow to grayish yellowish brown powder. add 10 mL of ether. Evaporate 30 mL of the filtrate to dryness. Cool. stopper tightly and shake thoroughly for 5 minutes. granular and compact. contains not less than 0. Assay Weigh accurately about 4. lactose or their mixture little by little and mix well. Under a microscope. and has faint. After cooling. Description Scopolia Rhizome is the rhizome. add 5 g of powdered tragacanth and shake vigorously. (2) Weigh 5 g of Scopolia Extract Powder 10%. Scopolia Rhizome has characteristic odor and sweet taste. or Scopolia carniolica Jacquin (Solanaceae). Amount (mg) of scopolamin e (C 17 H 21 NO 4 ) = amount (mg) of Scopolamin e Hydrobromi de RS.8551 Q SA 5 Identification (1) Weigh 1 g of pulverized Scopolia Rhizome.3% of total alkaloids [as hyoscyamine (C17H23 NO3: 289.7894 Q SS 25 Packaging and Storage Preserve in tight containers. dissolve the residue in 1 mL of dimethylformamide and add 5 to 6 drops of tetraethylammonium hydroxide TS: a redpurple to purple color develops. stopper tightly. Lactose or their mixture a sufficient quantity ⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯ To make 1000 g Take Scopolia Extract. with lighter colored cortex. Dry preferably at a low temperature and dilute with a sufficient additional quantity of starch. stopper tightly. chiefly irregularly branched. add 20 mL of methanol in a flask and boil the mixture in a water-bath for 30 minutes under a reflux condenser. Repeat this procedure three times with the water layer. add 25 mL of diluted sulfuric acid (1 in 50). Allow to stand for 5 minutes. Proceed as directed in the Identification (2) under Scopolia Rhizome using this solution as the test solution. shake for 30 minutes and filter. Parenchyma cells contain starch grains and sometimes sand crystals of calcium oxalate. later slightly bitter. about 5 cm to l5 cm in length and 1 cm to 3 cm in diameter. add 10 mL of ether and 0. characteristic odor and slightly bitter taste. add 100 mL of purified water. To the residue. Q 1 calculated on the dried basis × TA × × 0.37) and scopolamine (C17H21NO4: 303. shake well and drain off the acid extract into another separatory funnel. when dried. Wash the residue with l0 mL of ether.. Render the solution slightly alkaline with ammonia TS.35 )]. and scars of roots or root are on lower surface of rhizome. add 5 mL of water and 2 mL of ammonia TS and mix well. with wrinkles. separate the ether extract.5 mL of ammonia TS. Amount (mg) of hyoscyamin e (C17 H 23 NO 3 ) = amount (mg) of Atropine Sulfate RS. add exactly 3 mL of the internal standard solution and add the mobile phase to make exactly 25 mL. combine the filtrate with the washings and evaporate the methanol. lactose or their mixture to make 1000 g of homogeneous powder. wash the residue twice with l0 mL volumes of methanol. shake well. mix homogeneously. take the clearly separated ether layer and filter. To the residue. add 5 drops of fuming nitric acid and evaporate the mixture on a water-bath to dryness. Add 25 mL of ether. stem base is present at one end. Scopolia Rhizome. place in a glass-stoppered centrifuge tube. warm and soften the mixture with stirring. Proceed with the filtrate as directed in the identification (1) under Scopolia Extract. transfer the ether layer to a porcelain dish and evaporate the ether on a water-bath. shake for 15 minutes and centrifuge to take the ether layer. add 800 g of starch. Immediately add 50 mL of ether and 5 g of sodium chloride. Proceed as directed under Scopolia Rhizome. Scopolia Rhizome is the rhizome of Scopolia japonica Max. Q 1 calculated on the dried basis × TS × × 0 . Identification (1) Weigh 20 g of 10% Scopolia Extract powder add 15 mL of water and 8 mL of ammonia TS. Scrophularia Root Scrophulariae Radix Scrophularia Root is the root of Scrophularia buergeriana Miquel or Scrophularia ningpoensis Hemsley (Scrophulariaceae). transverse lenticels and sparse rootlet scars. weigh accurately about 25 mg of Atropine Sulfate RS (determined the loss on drying before use). Repeat this procedure twice with the residue using 25 mL volumes of ether. about 4 mm in inside diameter and about 15 cm in length. spray evenly Dragendorff’s TS on the plate: two principal spots from the test solution and each yellow-red spot from the standard solutions (1) and (2) show the same color and the same Rf value. add 3. add 10 mL of triethylamine adjust with phosphoric acid to make a pH of 3.1088 Monographs. Ash Not more than 7. add water to make 1000 mL and mix this solution with acetonitrile (9 : 1). Description Scrophularia Root is irregularly curved. of the peak area of hyoscyamine (atropine) and the ratios. After cooling.5.8551 Q SA 5 Amount (mg) of scopolamin e (C 17 H 21 NO 4 ) = amount (mg) of Scopolamin e Hydrobromi de RS. Determine the ratios. respectively. Texture is compact and flexible. add 2 g of anhydrous sodium sulfate to the chloroform solution. atropine and the internal standard are eluted in this order with. long cylindrical or spindle-shaped root. To this. water and strong ammonia water (90 : 7 : 3) to a distance of about 10 cm and dry the plate at 80 °C for 10 minutes. Filter this solution through a filter having a porosity of not more than 0. Combine all the extracts and evaporate the ether on a water-bath. Perform the test with 10 μL each of the test solution and the standard solution as directed under the Liquid Chromatography according to the following operating conditions. QTA and QSA. Selection of column: When the procedure is run with 10 μL of the standard solution under the above operating conditions and determine the resolution: scopolamine. Q 1 calculated on the dried basis × TA × × 0. for the test solution and the standard solution. add immediately 30 mL of chloroform and shake to mix. QTS and QSS.0 mL of the internal standard solution and add the mobile phase to make 25 mL. add 25 mL of ether. dissolve in the mobile phase to make exactly 25 mL and use this solution as the standard stock solution B.0%. Operating conditions Detector: An ultraviolet absorption photometer (wavelength: 210 nm). Transfer 20 mL of the filtrate to a separatory funnel and shake thoroughly with 10 mL of ether. Pipet 5 mL of standard stock solution A and 1 mL of standard stock solution B. Separate the aqueous layer. discard the first 2 mL of the filtrate and use the subsequent filtrate as the test solution. Dissolve the residue in 5 mL of the mobile phase. develop the plate with a mixture of acetone. in a glass-stoppered centrifuge tube and moisten with l5 mL of ammonia TS. hard to be fractured. previously dried at 60°C for 8 hours. shake and filter when the chloroform layer becomes clear. Column temperature: A room temperature. Q 1 calculated on the dried basis × TS × × 0 . respectively. Separate the chloroform layer. for the test solution and the standard solution.7894 Q SS 25 Internal standard solution⎯A solution of brucine in the mobile phase (1 in 2500). dissolve the residue in 1 mL of ethanol and use this solution as the test solution. External surface is yellowish brown-brown. Perform the test with the test solution and the standard solutions (1) and (2) as directed under the Thin-layer Chromatography. calculate the amounts of hyoscyamine and scopolamine by the following equations and designate the total as the amount of tota1 alkaloids. centrifuge and separate the ether layer. Assay Weigh accurately about 0.0 mL of the internal standard solution. with rough longitudinal wrinkles. packed with octadecylsilyl silica gel for liquid chromatography (5 μm in particle diameter). and the fractured surface is dark brown. Spot 5 μL each of the test solution and the standard solutions (1) and (2) on a plate of silica gel for thin-layer chromatography. Separately. render slightly alkaline with ammonia TS. dissolve each in 10 mL of ethanol and use these solutions as standard solutions (l) and (2).8 μm. clearly dividing each peak. weigh 20 mg of Atropine Sulfate RS and 10 mg of Scopolamine Hydrobromide RS. Evaporate 20 mL of the solution to dryness. shake for 15 minutes. Weigh accurately about 25 mg of Scopolamine Hydrobromide RS (determined the loss on drying before use). stopper the centrifuge tube tightly. add 3. Part II and filter. Amount (mg) of hyoscyamin e (C 17 H 23 NO 3 ) = amount (mg) of Atropine Sulfate RS.7 g of pulverized Scopolia Rhizome. of the peak area of scopolamine to that of the internal standard. Column: A stainless steel column. then add 25 mL of the mobile phase and use this solution as the standard solution.8 g of monobasic potassium phosphate in 900 mL of water. Separately. 4 cm to 15 cm in length and 1 cm to 3 cm in diameter. Mobile phase: Dissolve 6. dissolve in the mobile phase to make exactly 25 mL and use this solution as the standard stock solution A. Flow rate: Adjust the flow rate so that the retention time of scopolamine is about 8 minutes. Scrophularia Root has characteristic odor and tastes . semitubular or flattened root. Pipet 10 μL each of the test solution 1. Scutellaria Root is the root or the root from which the periderm has been removed of Scutellaria baicalensis Georgi (Labiatae).5 g of pulverized Scrophularia Root.0%. Combine all the extracts. with coarse and marked longitudinal wrinkles and with scattered scars of lateral root and remains of brown periderm. heat on a water Acid-insoluble Ash Not more than 1.0% of total sum of baicalin (C21H18-O11: 446. add 10 mL of methanol. add carefully 1 mL of sulfuric acid to the filtrate: a reddish brown color develops at the zone of contact.0 mL of the test solution 1.0%. Extract Content Dilute ethanol-soluble extract— Not less than 24. Fractured surface is fibrous and yellow. 2 and the standard solution and perform the test as directed under the Liquid Chromatography according to the following operating conditions. (2) Weigh 1 g each of pulverized Scutellaria Root and Scutellaria Root RMPM.0 mL of the solution. Pipet 2. the standard solution of Scutellaria Root RMPM and the standard solution (1). add 30 mL of a mixture of ethyl acetate and methanol (3 : 1). respectively. Deve1op the plate with a mixture of toluene. the standard solution of Scutellaria Root RMPM and the standard solution (1). respectively. dissolve in methanol to make exactly 20 mL. heat for 2 minutes and filter. Texture is hard and easily broken. methanol and formic acid (10 : 3 : 1 : 2) to a distance of about 10 cm and airdry the plate.5 g of pulverized Scutellaria Root. To the residue. Determine the peak areas. often forming a hollow. boil gently with 20 mL of ether under a reflux condenser in a water-bath for 5 minutes. Perform the test with the test solution. Xylem is rotted in old roots.37). add 1 mL of methanol and use these solutions as the standard solution (1) and the standard solution (2). cool and filter.5 mg each of baicalin TS and woogonin TS. add 20 mL of 70% solution of ethanol to make exactly 100 mL and use this solution as the test solution 1. add 40 mL of 70 % solution of ethanol and proceed in the same manner. of bai- . Separately. Add 2 mL of Fehling TS to 4 mL of the filtrate and heat in a water-bath: a red precipitate is produced. Pipet 2.1 g of pulverized Scrophularia Root. ATB. Assay Weigh accurately about 0.KP VIII 1089 sweet at first and slightly bitter later.0%. add 40 mL of 70% solution of ethanol. Loss on Drying Not more than 17.28). weigh 0. add 1 to 2 drops of dilute ferric chloride TS: a grayish green color develops and changes to purple-brown. The several spots from the test solution and the spots from the standard solution of Scutellaria Root RMPM show the same color and the same Rf value. The filtrate is evaporated to dryness. Evaporate the filtrates to dryness. External surface is yellowbrown. Examine the plate under ultraviolet light (wavelength: 254 nm). Scutellaria Root contains not less than 10. dissolve the residues to 5 mL of methanol and use these solutions as the test solution and the standard solution of Scutellaria Root RMPM.0%. Description Scutellaria Root is cone-shaped. Separately.67 kPa (silica gel) for not less than 24 hours) and about 10 mg of Woogonin RS (previously dried in a desicator in vacuum at a pressure not exceeding 0. add 10 mL of water. Ash Not more than 6. (2) as directed under the Thin-layer Chromatography. (2) Weigh 0. Identification (1) Weigh 0. of baicalein and woogonin for the test solution 1.0%. Scutellaria Root is almost odorless and it has slightly bitter taste.67 kPa (silica gel) for not less than 24 hours). Scutellaria Root Scutellari Radix bath for 30 minutes under a reflux condenser and filter.24) and woogonin (C16H12-O5: 284. calculated on the dried basis. Spot 2 μL each of the test solution. heat for 2 to 3 minutes in a water-bath and filter. dissolve the residue in 10 mL of ethanol and to 3 mL of the solution. about 10 mg of Baicalein RS (previously dried in a desicator in vacuum at a pressure not exceeding 0. Ash Not more than 6.5 g of pulverized Scutellaria Root. baicalein (C15H10O5: 270. Evaporate the filtrate. add 70% solution of ethanol to make exactly 20 mL and use this solution as the standard solution. Loss on Drying Not more than 15. Scars of stem or remains of stem are present at the crown.0% (6 hours). weigh accurately each of about 10 mg of Baicalin RS (previously dried in a desicator in vacuum at a pressure not exceeding 0. 5 cm to 25 cm in length and 5 mm to 30 mm in diameter. (2) on a plate with fluorescent indicator for thin-layer chromatography. The two spots of the several spots from the test solution and the each spot of the standard solution (1) and the standard solution (2) show the same color and the same Rf value. ATBH and ATW. Acid-insoluble Ash Not more than 2. add 70% solution of ethanol to make exactly 20 mL and use this solution as the test solution 2.0%. heat for 2 to 3 minutes in a water-bath and filter. ethyl acetate. add 4 mL of acetic anhydride to the residue.67 kPa (silica gel) for not less than 24 hours). Identification (1) Weigh 0. After cooling. heat under a reflux condenser in a water-bath for 1 hour and filter. Senega Senegae Radix Senega is the root of Polygala senega Linné or Polygala senega Linné var. and the fractured surface is not fibrous. Mobile phase: Control the mobile phase A and B stepwise or gradient as the following conditions.1090 Monographs. Description Senega is the root. conical and slightly twisted. (2) Weigh 0. Cortex on the opposite side is thickened. Ash Not more than 5. Medullary rays on xylem are not distinct. Baiclein RS. packed with octadecylsilyl silica gel for liquid chromatography (5 to 10 μm in particle diameter). Mobile phase A: A mixture of water and acetic acid (99 : 1) Mobile phase B: A mixture of acetonitrile. a transverse section of the main root reveals a cork layer consisting of several rows of pale brown cork cells.0%. It is tuberously enlarged crown.5%. and ASB. a transverse section reveals grayish brown cortex and yellowish white xylem. transversed by medullary rays. of baicalin. add 30 mL of water. resembling the aroma of methyl salicylate. Amount (mg) of baicalin (C 21 H 18 O 11 ) A = amount (mg) of Baicalin RS × TB × 5 A SB Amount (mg) of baicalein (C 15 H 10 O 5 ) = amount (mg) of Baicalein RS × A TBH 1 × A SBH 2 Amount (mg) of woogonin (C 16 H 12 O 5 ) = amount (mg) of Woogonin RS × A TW 1 × A SW 2 Operating conditions Detector: An ultraviolet absorption photometer (wavelength: 277 nm). 1 to 3 cells wide. baicalein and woogonin for the standard solution. Part II calin for the test solution 2. slender.0% . latifolia Torrey et Gray (Polygalaceae). Acid-insoluble Ash Not more than 2. System suitability System performance: Dissolve 2 mg each of Baicalin RS.5 g of pulverized Senega. It is usually round and sometimes cuneate to semicircular. Its parenchyma cells contain oil droplets. Branched rootlets are twisted and curved. Senega is breakable. add 30 mL of water and shake vigorously: a lasting fine foam is produced. shake for 15 minutes and filter.5 g of pulverized Senega. (2) Foreign matter—Senega contains less than 1. Secondary cortex is composed of parenchyma cells and sieve tubes.0% of stems. mix with 50 mL of water and determine the absorption spectrum of the solution as directed under the Ultraviolet-visible Spectrophotometry: it exhibits a maximum at about 317 nm. Column temperature: 40 o C . Extract Content Dilute ethanol–soluble extract— Not less than 30. Loss on Drying Not more than l3. The taste is sweet at first but leaving an acrid taste.0% (6 hours). ASBH and ASW. Purity (1) Stem—Senega contains lessthan 2. the margin is irregulary waved. Under a microscope. System repeatability: When the test is repeated 6 times with 10 μL of the standard solution under the above operating conditions. Senega has characteristic odor.0 mL/min. Woogonin RS and methyl phydroxybenzoate in methanol to make 100 mL. Under a magnifying glass. the relative standard deviation of the peak area of baicalin. The main root is 3 cm to 10 cm in length and 5 mm to 15 mm in diameter. When the procedure is run with 10 μL of this solution under the above operating conditions. External surface is pale grayish brown to grayish brown with many longitudinal wrinkles and sometimes with twisted protruding lines. baicalein and woogonin is not more than 1. Take 1 mL of the filtrate. Identification (1) Weigh 0. use a column giving elution of baicalin.01) to Time (min) 0 10 20 24 35 40 45 Mobile Mobile phase A(%) phase B(%) 75 25 68 32 55 45 55 45 52 48 75 25 75 25 Flow rate: 1. methanol and acetic acid (7 : 3 : 0. methyl phydroxybenzoate and woogonin in this order and clearly dividing each peak.0% of foreign matter other than stems. with remains of stems and red buds. but starch grains and calcium oxalate crystals are absent.0%. Column: A stainless steel column. 4 mm to 6 mm in inside diameter and 15 cm to 25 cm in length. baicalein. Purity (1) Rachis and fruit—Senna Leaf contains less than 5. pale grayish yellow to pale grayish yellow-green. Examine under ultraviolet light (main wavelength: 365 nm): one spot among the spots from the test solution and a red fluorescent spot from the standard solution show the same color and Rf value. calculated on the basis of dried material. centrifuge and separate the supernatant liquid. previously dried in a desiccator (in vacuum at a pressure not exceeding 0. dissolve in diluted sodium bicarbonate (1 in 100) to make exactly 20 mL and use this solution as the standard stock solution (2). separate the tetrahydrofuran layer and use this solution as the test solution. Identification (1) Weigh 0. (2) Weigh 2 g of pulverized Senna Leaf. Determine the peak areas. of sennoside B for the test solution and the standard solution. shake for 30 minutes and centrifuge. add 10 mL of water and macerate for 2 minutes. Spot 10 μL each of the test solution and the standard solution on a plate of silica gel with fluorescent indicator for thin-layer chromatography. add 25 mL of diluted methanol (7 in 10). the lower surface has slight hairs. Ash Not more than 12. Amount (mg) of sennoside A (C 42 H 38 O 20 ) = amount (mg) of Sennoside A RS × ATA 1 × ASA 4 Amount (mg) of sennoside B (C 42 H 38 O 20 ) = amount (mg) of Sennoside B RS × ATB 1 × ASB 2 .67 kPa. weigh accurately about 10 mg of Sennoside A RS. Assay Weigh accurately about 0. Acid-insoluble Ash Not more than 2.5 g of pulverized Senna Leaf in a glass-stoppered centrifuge tube.0%. Under a microscope. warty unicellular hairs. Weigh accurately about 10 mg of Sennoside B RS previously dried in a desiccator (in vacuum at a pressure not exceeding 0. Separately.0% of petiols and fruits. 15 mm to 50 mm in length and 4 mm to 20 mm in width. Add 5 mL of ammonia TS to the filtrate: a yellow-red color is produced in the water layer.0% of total sennosides [as sennoside A (C42H38O20: 862. respectively. add twice 10 mL of diluted methanol (7 in l0). add methanol to make exactly 50 mL and use this solution as the standard solution. Senna Leaf contains not less than 1. shake each for 10 minutes.74) and sennoside B (C42H38O20: 862. Margin is entire and apex is acute. ATA and ASA. The upper surface is flat. centrifuge and separate the supernatant liquid. P2O5) for not less than 12 hours.5 g of pulverized Senna Leaf. Description Senna Leaf is the leaflet. Pipet 5..5 by adding 1 mol/L hydrochloric acid TS. Epidermal cells are often separated into two loculi by a septum which is in parallel with the surface of the leaf and contain mucilage in the inner loculus. Loss on Drying Not more than 12. dissolve in 1 mL of a mixture of tetrahydrofuran and water (7 : 3) and use this solution as the standard solution. Transfer the supernatant liquid to a separatory funnel. add 10 mL of ether for 2 minutes and filter. Transfer this solution to another separatory funnel. Develop the plate with a mixture of n–propanol. of sennoside A.67 kPa. Spongy tissue is consisted of 3 to 4 layers and contains clustered or solitary crystals of calcium oxalate. ATB and ASB. respectively and the peak areas.0% of foreign matter other than petiols and fruits. Perform the test as directed under the Thin-layer Chromatography with the test solution and the standard solution. Palisade of a single layer is under each epidermis. To the residue. weigh 1 mg of Sennoside A RS. vein of lower surface is marked and petiole of leaflet is short. add diluted methanol (7 in l0) to make exactly 50 mL and use this solution as the test solution. Senna Leaf has slight odor and bitter taste. To the residue of maceration. ethyl acetate. Cells adjacent to vascular bundle forms crystal cell rows. The base is asymmetric and primary lateral veins are running toward the apex along the margin and joining together. a transverse section reveals epidermis with thick cuticle. add 13 g of sodium chloride and shake for 30 minutes. P2O5) for not less than 12 hours. shake with 30 mL of tetrahydrofuran for 10 minutes.KP VIII 1091 Senna Leaf Sennae Folium Senna Leaf is the leaflets of Cassia angustifolia Vahl or Cassia acutifolia Delile (Leguminosae). Separate the water layer with undissolved sodium chloride and adjust the pH to 1.0% (6 hours). dissolve in diluted sodium bicarbonate (1 in 100) to make exactly 20 mL and use this solution as the standard stock solution (1).74)]. elongated ovate to lanceolate. Combine all the extracts. respectively. water and acetic anhydride (40 : 40 : 30 : 1) to a distance of about 15 cm and air-dry the plate. Separately. Filter and add 5 mL of ammonia TS: a yellow-red color is produced in the water layer. shake for 30 minutes.0 mL of the standard stock solution (2). (2) Foreign matter— Senna Leaf contains less than 1.0%. Pipet 10 μL of the test solution and the standard solution and perform the test as directed under the Liquid Chromatography according to the following operating conditions. for the test solution and the standard solution.0 mL of the standard stock solution (1) and 10. calculate the amounts of sennoside A and sennoside B by the following equations and designate the total as the amount of total sennosides. add 40 mL of a mixture of tetrahydrofuran and water (7 : 3). with numerous stomata and with thick-walled. 5%. Separately. wrinkled and rolled. with apex hollowed slightly. System repeatability: When the test is repeated 6 times with the standard solution under the above operating conditions: the relative standard deviation of the peak area of sennoside A is not more than 1. The others are long round. Column temperature: A constant temperature of about 50 °C. (i) Take 2. 4 mm to 6 mm in inside diameter and 15 cm to 20 cm in length.45 g of tetra-nheptylammonium bromide in l00 mL of a mixture of diluted 1 mo1/L acetic acid-sodium acetate buffer solution. Spot 5 μL each of the test solution and the standard solution on a plate of silica gel with fluorescent indicator for thin-layer chromatography. Medullary rays contain starch grains. Flow rate: Adjust the flow rate so that the retention time of sennoside A is about 26 minutes. Examine under ultraviolet light (main wavelength: 254 nm) or spray evenly aluminum chloride TS and examine under ultraviolet light (main wavelength: 365 nm): one spot among the spots from the test solution and a spot from the standard solution do not show the same color and the same Rf value. Pistil is cylindrical and curved.Sophora Flower is the flower bud. cool and filter. Flank is dark grayish brown. Calyx is campanulate and yellowish-green. Description Sinomenium Stem and Rhizome is the stem and rhizome. The stalk of stamen is thin and long.0 mL of the filtrate. Cortex is pale brown to dark brown. yellow to yellowish white.0 (1 in 10) and acetonitrile (17 : 8). an orange- Sophora Flower Sophorae Flos Sophora Flower is the flower bud and flower of Sophora japonica Linné (Leguminosae). Mobile phase: Dissolve 2. ovoid or elliptical. 3 μm to 10 μm in diameter and small needle crystals of calcium oxalate. Sophora Flower has slightly characteristic odor and tastes slightly bitter and astringent. heat for 2 minutes in a water-bath with frequent shaking. Identification (1) Weigh 0. Primary cortex contains needle crystals of calcium oxalate. Sinomenium Stem and Rhizome Sinomeni Caulis et Rhizoma Sinomenium Stem and Rhizome is the climbing stem and rhizome of Sinomenium acutum Rehder et Wilson (Menispermaceae). packed with octadecylsilyl silica gel for liquid chromatography (5 μm to l0 μm in particle diameter). clearly dividing each peak. accreted at the base of 9 stamens. add 25 mL of ethanol. grayish brown vessel volumes and dark brown medullary rays lined alternately and radially. Evaporate the filtrate. nearly round. The stalk is thin and small. with round or elliptical sections. 2 mm to 6 mm in length. Acid-insoluble Ash Not more than 0. Irregular-sized vessels lined nearly stepwise in the vessel volume.5%. The lower part of calyx has several longitudinal scars. and the latter Koehwa. Sinomenium Stem and Rhizome is nearly odorless and as bitter taste. sonicate for 1 hour and filter. The former is known as Koemi. add a small amount of . Perform the following test with the filtrate. dissolve it in 1 mL of ethanol. Identification Weigh 0. to lobed at the apex. add 10 mL of methanol and extract and filter.0%. Purity Weigh 2 g of pulverized Sinomenium Stem and Rhizome. Sophora Flower has slightly characteristic odor and tastes slightly bitter. Description (1) Koemi . yellow precipitate is produced. Under a microscope. Numbers of stamens are 10. The upper part of calyx has yellowish white petals. To 5 mL of the filtrate. Ash Not more than 6.Sophora Flower is the flower. add 2 drops of Dragendorff’s TS: immediately.1092 Monographs. System suitability System performance: When the procedure is run with 10 μL of the standard solution under the above operating conditions: sennoside B and sennoside A are eluted in this order.5 g of the pulverized Sophora Flower. a transverse section reveals extremely thick-walled stone cells in primary cortex and pericycle. Part II Operating conditions Detector: An ultraviolet absorption photometer (wavelength : 340 nm). Perform the test with the test solution and the standard solution as directed under the Thin-layer Chromatography. (2) Koehwa . Texture is easy to break. In xylem. pH 5. ethyl acetate. methanol and formic acid (20 : 10 : 1 : 1) to a distance of about 10 cm and air-dry the plate. Column: A stainless steel column. weigh 1 mg of Aristolokinic acid RS. with longitudinal wrinkles and warty protrusions. dissolve 1 mL of ethanol and use this solution as the test solution.5 g of pulverized Sinomenium Stem and Rhizome add 10 mL of dilute acetic acid. Develop the plate with a mixture of toluene. and use this solution as the standard solution. simple grain. One of petal is relatively large. 2 mm to 4 mm in thickness and 10 mm to 45 mm in diameter. about 2 mm in diameter. Cells of medullary ray mostly not lignified and extremely thick-walled and large stone cells scattered here and there. Numbers of petals are 5. collect the aqueous layer. Ash Not more than 6. (2) Weigh 0. respectively. cool and filter. Add potassium carbonate to aqueous layer to adjust pH to 10.5%. Purity (1) Foreign matter— Sophora Flower contains not more than 10% of flower stalk and other foreign matter. Purity (1) Stem—Not more than 10. let stand for 2 hours: the yellow color of the solution is more intense than that of 0. And examine under ultraviolet light: test solution produces yellowish-brown and the zone of two liquids produces yellow fluorescence. add methanol to make exactly 10 mL. Pipet 10 μL each of the test solution and the standard solutions. Combine all the extracts and evaporate to dryness in vacuum.0% of the sum of oxymatrine (C15H24N2O2: 264. add 1 ml of methanol and use this solution as the standard solution. Develop the plate with a mixture of ethyl acetate. add 3. Weigh 8 mg of rutin RS. Acid-insoluble Ash Not more than 1. add 5 mL of methanol. add 50 mL of dichloromethane. Description Sophora Root is cylindrical root. and proceed in the same manner. add 10 mL of dilute acetic acid. filter and use the filtrate as the test solution. Identification Weigh 0. Spot 10 μL each of the test solution and the standard solution on a plate of silica gel with fluorescent indicator for thin-layer chromatography. with or without periderm. and use this solution as the standard solutions. To the residue. with somewhat fibrous surface.0%. slightly tinged with dark color near cambium.36). The transverse section is pale yellow-brown. add 40 mL of ether and proceed three times in the same manner. Combine all the filtrates. Ash Not more than 9. Determine the peak areas.0 mL of this solution.0 mL of potassium acetate solution. followed by addition of 10% hydrochloride solution to adjust to pH 2. To 5 mL of the filtrate. Sophora Root has slight odor and tastes extremely bitter and lasting. heat for 2 hours with reflux condenser and filter.04% of the potassium chromate solution.0 mL of aluminum chloride solution and 5. add 100 mL of methanol. Perform the test with the test solution and the standard solution as directed under the Thinlayer Chromatography. Preserve in light-resistant. and filter. extract with occasional.0%.2 g of pulverized Sophora Flower. sonicate for 20 minutes. 5 cm to 20 cm in length and 2 cm to 3 cm in diameter. and add water to dissolve completely. (ii) Drop 2 to 3 drops of the filtrate on the filter paper and drop 1% of alum solution onto the filtrate: at the zone of two liquids yellow color is produced. shake for 10 minutes. Sophora Root Sophorae Radix Sophora Root is the root of Sophora flavescens Solander ex Aiton (Leguminosae).5 g of pulverized Sophora Root. and matrine (C15H24N2O: 248. ATO and ATM of the test solution and the standard solutions. and perform the test as directed under the Liquid Chromatography according to the following operating conditions. The cortex is 1 mm to 2 mm in thickness. External surface of root without periderm is yellowish white. add 2 drops of Dragendorff’s TS: an orange-yellow precipitate is produced immediately. Amount(mg) of oxymatrine(C15 H 24 N 2 O 2 ) = amount(mg) of OxymatrineRS × A TO ASO . add 50 mL of 75% ethanol .36). External surface is dark brown to yellow-brown. and proceed in the same manner. weigh accurately 20 mg of Oxymatrine RS and 10mg of Matrine RS. Separately. (2) Foreign matter—The amount of foreign matter other than stems contained in Sophora Root is not more than 1. dissolve in methanol to make exactly 10 mL. Spray evenly aluminum chloride TS on the plate and examine under ultraviolet light (main wavelength: 365 nm): one spot among the spots from the test solution and a spot from the standard solution show the same color and the same Rf value. Packaging and Storage tight containers. and use this solution as the test solution. add 50mL of dichloromethane and proceed in the same manner. with distinct longitudinal wrinkles and with laterally extended lenticels. forming a crack between xylem. heat in a waterbath for 3 minutes with occasional shaking. (2) Rutin—Weigh accurately 1 g of Sophora Flower.KP VIII 1093 magnesium powder and 2 to 3 drops of hydrochloric acid: a red color is produced. shake well. Add 50 mL of dichloromethane to wash. Filtrate is concentrated in waterbath. stand. shake well. Assay Weigh accurately about 4 g of pulverized Sophora Root. formic acid and water (8 : 1 : l) to a distance of about 10 cm and air-dry the plate. Sophora Root contains not less than 1. evaporate to dryness in vacuum. To the residue. take 1.0 mL of this solution and make 20 mL. add 10 mL of water and 60 mL of ether. discard ether layer. add 50 mL of 75% ethanol.0%. Add 50mL dichloromethane to aqueous layer. Add methanol to make 100 mL. Take 2.0%. 50 g purified water a sufficient quantity ⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯ To make 100 mL Pulverize the above crude drugs to coarse powder. add 30 mL of ethanol. packed with octadecylsilyl silica gel for liquid chromatography (5 μm in particle diameter). Under a microscope. Extract Content Dilute ethanol-soluble extract— Not less than 11.93) in Licorice for a dose (one bottle). shake for 1 hour. 4. Cinnamon Bark 0. External surface is yellowish white or graysh yellow. dissolve to make 1000 mL.Take equivalent to 1 g of Peony Root.13 g Angelica Gigas Root. Ssanghwatang Solution is prepared as directed under Solutions. Separately. gel for thin-layer chromatography. heat under a reflux condensor for 10 minutes on a water-bath. The cortex and stele contain secretory cells filled with yellow substance. The texture is heave and compact. slightly ringed-arranged transversely. weigh each crude drugs. To the each residue. Develop the plate with a lower layer of the mixture of chloroform.1 mg of paeoniflorin (C23H28O11: 480. transverse section reveals vascular bundles scattered and vessels without lignification. Potassium phosphate buffer solution (pH 6.0% . conical. Perform the test with the test solution and Sparganium Rhizome RMPM standard solution as directed under the Thin-layer Chromatography. put into the extractor. add 2 mL of ethanol and use each solution as the test solution or Sparganium Rhizome RMPM standard solution. Sparganium Rhizome is odorless and taste is week. add eight to ten fold of water.0%.1094 Monographs.6 mg of glycyrrhizic acid (C42H62 O16: 822. Prepared Rehmannia Root.0%. Part II Amount (mg) of matrine (C 15 H 24 N 2 O) = amount (mg) of Matrine RS × A TO A SO Operating conditions Detector: An ultraviolet absorption photometer (wavelength: 205 nm). Flow rate: 1.6 mm in inside diameter and 25 cm in length. Develop the plate with a mixture of cyclohexane and ethyl acetate (4 : 1) to a distance of about 10 cm and air-dry the plate. slightly flattened.25 g Licorice. Cndium Rhizome. add 100 mL of methanol. methanol and water (26 : 14 : 5) to a distance of about 10 cm and air-dry the . evaporate the filtrate to dryness in vacuum until the filtrate becomes 20 mL and use this solution as the test solution.0) : Add 0. extract with a reflux condenser for 1 hour and filter. Column: A stainless column. Astragalus Root Sparganium Rhizome Sparganni Rhizoma Description Sparganium Rhizome is the tuber. filter and evaporate to dryness. Column temperature: An ordinary temperature.0 mL/min.0) (9 :91). add 100 mL of water. Identification Weigh 2 g each of pulverized Sparganium Rhizome or Sparganium Rhizome RMPM. and adjust to pH 6 with 0.5%. Evaporate the filtrate to dryness in vacuum until the filtrate becomes 20 mL and use this solution as the standard solution.94 g Jujube 0. Spot 10 μL each of the test solution and Sparganium Rhizome RMPM standard solution on a plate of silica 1. Identification (1) Peony Root . Mobile phase: A mixture of acetonitrol and potassium phosphate buffer solution (pH 6.46) in Peony Root and 5. weigh 1 g of Peony Root. Spot 20 μL each of the test solution and the standard solution on a plate of silica gel with fluorescent indicator for thin-layer chromatography. Acid-insoluble Ash Not more than 1. Ash Not more than 5. 2 cm to 6 cm in length and 2 cm to 4 cm in diameter.65 g of dibasic potassium phosphate to water. Method of preparation for a dose (one bottle) Peony Root 3. Ssanghwatang Solution Ssanghwatang Solution contains not less than 17.0%. Use a column giving elution of oxymatrine and matrine in this order and clearly dividing each peak.67 g Ginger 0. System repeatability: When the test is repeated six times with 10 μL of the standard solutions under the above operating conditions: the relative standard deviation of the peak area of oxymatrine and matrine is not more than 1. with marks pared with a knife and fibrous root scars spotted. System suitability System performance: Proceed with 10 μL of the standard solutions under the above operating conditions. Spray evenly diluted sulfuric acid TS and heat at 105 o C for 10 minutes: the spots from the test solution and the spots from Sparganium Rhizome RMPM standard solution show the same colors and the same Rf values Loss on Drying Not more than 10.1% of potassium carbonate solution. extract for 2 to 3 hours at 80 o ~ 100 C and filter. Perform the test with the test solution and the standard solution as directed under the Thin-layer Chromatography. slightly numb on chewing. Develop the plate with a mixture of toluene and methanol (93 : 7) to a distance of about 10 cm and airdry the plate. shake for 1 hour. Separately. add 100 mL of water. vacuum-concentrate the filtrate until the filtrate becomes 20 mL and use this solution as the test solution. (2) Angelica Gigas Root . Separately. shake for 5 minutes. weigh 1 g of Prepared Rehmannia Root. Examine under ultraviolet light (main wavelength: 365 nm): one spot among the spots from the test solution and a spot from the standard solution show the same color and the same Rf value. Examine under ultraviolet light (main wavelength: 254 nm): one spot among the spots from the test solution and a spot from the standard solution show the same color and the same Rf value. extract with a reflux condenser for 1 hour and filter. Perform the test with the test solution . extract with a reflux condenser for 1 hour and filter. Develop the plate with a mixture of toluene. extract with a reflux condenser for 1 hour and filter. Perform the test with the test solution and the standard solution as directed under the Thinlayer Chromatography. add 100 mL of methanol. shake for 1 hour. (6) Licorice . extract with a reflux condenser for 1 hour and filter. add 100 mL of water. Spray evenly the plate with vanillino sulfuric acid TS and heat at 105 C for 10 minutes. Spot 20 μL each of the test solution and the standard solution on a plate of silica gel for thin-layer chromatography. Spot 20 μL each of the test solution and the standard solution on a plate of silica gel with fluorescent indicator for thin-layer chromatography. vacuum-concentrate the filtrate until the filtrate becomes 20 mL and use this solution as the test solution. Vacuum-concentrate the filtrate until the filtrate becomes 20 mL and use this solution as the standard solution. (4) Cnidium Rhizome . Vacuumconcentrate the filtrate until the filtrate becomes 20 mL and use this solution as the standard solution. extract with a reflux condenser for 1 hour and filter.Take equivalent to 1 g of Cinnamon Bark. add 100 mL of methanol. add 100 mL of methanol. Vacuumconcentrate the filtrate until the filtrate becomes 10 mL and use this solution as the standard solution. Separately.4-dinitrophenylhydrazine TS. (3) Prepared Rehmannia Root .Take equivalent to 1 g of Licorice. Perform the test with the test solution and the standard solution as directed under the Thin-layer Chromatography.Take equivalent to 1 g of Prepared Rehmannia Root. Vacuum-concentrate the filtrate until the filtrate becomes 20 mL and use this solution as the standard solution. Vacuum-concentrate the filtrate until the filtrate becomes 20 mL and use this solution as the standard solution. vacuum-concentrate the filtrate until the filtrate becomes 20 mL and use this solution as the test solution. Develop the plate with a mixture of cyclohexane and ethyl acetate (9 : 1) to a distance of about 10 cm and air-dry the plate. add 100 mL of methanol. extract with a reflux condenser for 1 hour and filter. Spray evenly the plate with po anisaldehyde-sulfuric acid TS and heat at 105 C for 10 minutes: one spot among the spots from the test solution and a spot from the standard solution show the same color and the same Rf value. ether. Develop the plate with a mixture of chloroform and methanol (95 : 5) to a distance of about 10 cm and air-dry the plate. shake for 1 hour. Perform the test with the test solution and the standard solution as directed under the Thinlayer Chromatography. weigh 1 g of Astragalus Root. add 100 mL of water. water and acetic acid (500 : 500 : 5 : 2) to a distance of about 10 cm and air-dry the plate. weigh 1 g of Cnidium Rhizome. Perform the test with the test solution and the standard solution as directed under the Thin-layer Chromatography. Vacuum-concentrate the filtrate until the filtrate becomes 20 mL and use this solution as the standard solution. vacuum-concentrate the filtrate until the filtrate becomes 20 mL and use this solution as the test solution. Separately. Perform the test with the test solution and the standard solution as directed under the Thin-layer Chromatography. shake for 1 hour. (7) Cinnamon Bark . vacuum-concentrate the filtrate until the filtrate becomes 20 mL and use this solution as the test solution.KP VIII 1095 plate. Spray evenly the plate with vanillin-sulfuric acid TS: one spot among the spots from the test solution and a spot from the standard solution show the same color and the same Rf value. (5) Astragalus Root . Spray evenly the plate with sulo furic acid TS for spray and heat at 105 C for 10 minutes. add 100 mL of water. add 100 mL of methanol. add 100 mL of water. weigh 1 g of Cinnamon Bark. weigh 1 g of Licorice. Spot 20 μL each of the test solution and the standard solution on a plate of silica gel with fluorescent indicator for thin-layer chromatography.sulo furic acid TS and heat at 105 C for 10 minutes: one spot among the spots from the test solution and a spot from the standard solution show the same color and the same Rf value.Take equivalent to 1 g of Astragalus Root. weigh 1 g of Angelica Gigas Root. Examine under ultraviolet light (main wavelength: 365 nm): one spot among the spots from the test solution and a spot from the standard solution show the same color and the same Rf value. Spray evenly the plate with p-anisaldehyde. shake for 1 hour. add 100 mL of water. Spray evenly the plate with 2. vacuumconcentrate the filtrate until the filtrate becomes 10 mL and use this solution as the test solution.Take equivalent to 1 g of Angelica Gigas Root. Separately. add 100 mL of methanol. Spot 20 μL each of the test solution and the standard solution on a plate of silica gel with fluorescent indicator for thin-layer chromatography.Take equivalent to 1 g of Cnidium Rhizome. Develop the plate with a mixture of chloroform and methanol (20 : 1) to a distance of about 10 cm and air-dry the plate. Spot 20 μL each of the test solution and the standard solution on a plate of silica gel with fluorescent indicator for thin-layer chromatography. Separately. extract with a reflux condenser for 1 hour and filter. add 50 mL of chloroform. and use this solution as the standard solution. (2) Glycyrrhizic acid of Licorice . Develop the plate with a mixture of hexane and ethyl acetate (85 : 15) to a distance of about 10 cm and air-dry the plate. take the chloroform layer in separatory funnel. add 50 mL of 3 mol/L of sulfuric acid TS and hydrolyze in a water bath for 1 hour. Separately. Column: A stainless steel column. Perform the test with the test solution and the standard solution as directed under the Thin-layer Chromatography. extract twice repetitively.0 mL/min Packaging and Storage Preserve in tight containers. Spot 20 μL each of the test solution and the standard solution on a plate of silica gel for thin-layer chromatography. Perform the test as directed under Assay for Peony Root. prepared in the same manner as the test solution. Separatly. vacuum-concentrate the filtrate until the filtrate becomes 20 mL and use this solution as the test solution. Develop the plate with a mixture of chloroform and methanol (6 : 1) to a distance of about 10 cm and air-dry the plate. pH Between 3. (9) Ginger . (8) Jujube . Vacuum-concentrate the filtrate until the filtrate becomes 20 mL and use this solution as the standard solution.Take equivalent to 1 g of Ginger. extract with a reflux condenser for 1 hour and filter. vacuum-concentrate the filtrate until the filtrate becomes 50 mL and use this solution as the test solution. Develop the plate with a mixture of hexane and ethyl acetate (85 : 15) to a distance of about 10 cm and air-dry the plate. prepare the solution. shake for 5 minutes. .1096 Monographs. add 100 mL of water. 4 mm to 6 mm in inside diameter and 15 cm to 25 cm in length. extract three times repetitively. Pipet 10 μL each of the test solution and the standard solution and perform the test as directed under the Liquid Chromatography according to the following operating conditions. A calculated on the anhydrous basis × T AS Operating conditions Detector: An ultraviolet absorption photometer (wavelength: 254 nm). Perform the test with the test solution and the standard solution as directed under the Thin-layer Chromatography. Spray evenly the plate with vanillin-sulfuric acid TS o and heat at 105 C for 10 min: one spot among the spots from the test solution and a spot from the standard solution show the same color and the same Rf value. weigh accurately about 10 mg of Paeoniflorin RS (separately determined the water content). extract with a reflux condenser for 1 hour and filter. add 100 mL of methanol. add 100 mL of methanol. of the test solution and the standard solution. combine the filtrates. add 10 mL of water. add 30 mL of chloroform. add 100 mL of water. dissolve the residue in methanol to make exactly 50 mL. Spray evenly the plate with p-anisaldehyde sulfuric aco id TS and heat at 105 C for 10 min: one spot among the spots from the test solution and a spot from the standard solution show the same color and the same Rf value. After cooling. Mobile phase: A mixture of methanol.Take equivalent to 1 g of Jujube. weigh accurately about 10 mg of Glycyrrhizic acid RS (separately determined the water content). add 100 mL of methanol. After cooling. Spot 20 μL each of the test solution and the standard solution on a plate of silica gel for thin-layer chromatography. To the residue. shake for 1 hour. heat and extract with a reflux condenser in a water bath for 30 minutes. vacuum-concentrate the filtrate until the filtrate becomes 20 mL and use this solution as the test solution. and use this solution as the test solution. weigh accurately and pulverize. respectively.980 and 1.Take accurately equivalent to 1 g of glycyrrhizic acid. weigh 1 g of Ginger. Amount (mg) of glycyrrhizic acid (C 42 H 62 O16 ) = amount (mg) of Glycyrrhizic Acid RS. Separately. Part II and the standard solution as directed under the Thinlayer Chromatography. Spot 20 μL each of the test solution and the standard solution on a plate of silica gel for thin-layer chromatography. water and acetic anhydride (78 : 19 : 3) Flow rate: 1. dissolve in methanol to make exactly 50 mL and use this solution as the standard solution.080 Assay (1) Paeoniflorin of Peony Root .Take not less than about 20 sachets of Ssanghwatang Solution. packed with octadecylsilyl silica gel for liquid chromatography (5 μm in particle diameter). heat and extract with a reflux condenser in a water bath for 3 hours. Determine the peak areas. Vacuum-concentrate the filtrate. Vacuum-concentrate the filtrate until the filtrate becomes 20 mL and use this solution as the standard solution. add 100 mL of methanol. combine chloroform layers and filter through anhydrous sodium sulfurate.0 and 5. Column temperature: A room temperature. Weigh accurately equivalent to about 10 mg of paeoniflorin. Separately. shake for 1 hour.0 Specific Gravity [α ] 20 D : Between 0. Spray evenly the plate with a saturated solution of o-dianisidineacetic anhydride(make when used): one spot among the spots from the test solution and a spot from the standard solution show the same color and the same Rf value. weigh 1 g of Jujube. AT and AS . add 100 mL of methanol. Vacuum-concentrate the filtrate until the filtrate becomes 10 mL and use this solution as the standard solution. Spray evenly the plate with 2. Develop the plate with a lower layer of the mixture of chloroform.13 g Angelica Gigas Root. shake for 5 minutes. vacuum-concentrate the filtrate until the filtrate becomes 10 mL and use this solution as the test solution. add 10 mL of water. shake for 5 minutes. Develop the plate with a mixture of chloroform and methanol (20 : 1) to a distance of about 10 cm and air-dry the plate. Method of preparation for a dose (one sachet) Peony Root 3. Develop the plate with a mixture of toluene.4dinitrophenylhydrazine TS.KP VIII 1097 Ssanghwatang Extract Granules Ssanghwatang Extract Granules contains not less than 12. ether. add eight to ten fold of water. weigh 1 g of Angelica Gigas Root. add 100 mL of methanol. Perform the test with the test solution and the standard solution as directed under the Thinlayer Chromatography. (3) Prepared Rehmannia Root . shake for 5 minutes.46) in Peony Root and 4. Examine under ultraviolet light (main wavelength: 365 nm): one spot among the spots from the test solution and a spot from the standard solution show the same color and the same Rf . Perform the test with the test solution and the standard solution as directed under the Thin-layer Chromatography. extract with a reflux condenser for 1 hour and filter. put into the extractor.Pulverize Ssanghwatang Extract Granules. vacuumconcentrate the filtrate until the filtrate becomes 10 mL and use this solution as the test solution. weigh equivalent to 1 g of Peony Root.25 g dium Rhizome. weigh equivalent to 1 g of Angelica Gigas Root. extract for 2 to 3 hours at 80 ~ 100 o C and filter.37 g to 5. add 100 mL of methanol. Ssanghwatang Extract Granules is prepared as directed under Granules. Vacuum-concentrate the filtrate until the filtrate becomes 10 mL and use this solution as the standard solution. water and acetic acid (500 : 500 : 5 : 2) to a distance of about 10 cm and air-dry the plate.98 g of Dry extract. Perform the test with the test solution and the standard solution as directed under the Thin-layer Chromatography.7 mg of glycyrrhizic acid (C42H62 O16: 822. Cni1.05 g of Viscous extract or concentrate in a suitable method until it becomes 1. Spot 20 μL each of the test solution and the standard solution on a plate of silica gel with fluorescent indicator for thin-layer chromatography.Pulverize Ssanghwatang Extract Granules. (2) Angelica Gigas Root . Vacuum-concentrate the filtrate under 60 o C until it becomes 3. add 10 mL of water. extract with a reflux condenser for 1 hour and filter. add 100 mL of methanol. Identification (1) Peony Root . add 100 mL of methanol. Separately. weigh 1 g of Peony Root.94 g Jujube 0.Pulverize Ssanghwatang Extract Granules. (4) Cnidium Rhizome . Spray evenly the plate with p-anisaldehydesulfuric acid o TS and heat at 105 C for 10 minutes: one spot among the spots from the test solution and a spot from the standard solution show the same color and the same Rf value. Vacuum-concentrate the filtrate until the filtrate becomes 10 mL and use this solution as the standard solution.2 mg of paeoniflorin (C23H28O11: 480. Spray evenly the plate with sulfuric acid TS for spray and heat at o 105 C for 10 minutes. Vacuum-concentrate the filtrate until the filtrate becomes 10 mL and use this solution as the test solution. Develop the plate with a mixture of cyclohexane and ethyl acetate (9 : 1) to a distance of about 10 cm and air-dry the plate. Spray evenly the plate with vanillin-sulfuric acid TS: one spot among the spots from the test solution and a spot from the standard solution show the same color and the same Rf value. Vacuum-concentrate the filtrate until the filtrate becomes 10 mL and use this solution as the standard solution. Perform the test with the test solution and the standard solution as directed under the Thin-layer Chromatography. add 100 mL of methanol. Spot 20 μL each of the test solution and the standard solution on a plate of silica gel with fluorescent indicator for thin-layer chromatography.50 g Pulverize the above crude drugs to coarse powder. Spot 20 μL each of the test solution and the standard solution on a plate of silica gel with fluorescent indicator for thin-layer chromatography. Separately. methanol and water (26 : 14 : 5) to a distance of about 10 cm and air-dry the plate. weigh equivalent to 1 g of Cnidium Rhizome. weigh each crude drugs. Separately. Cinnamon Bark 0. Spot 20 μL each of the test solution and the standard solution on a plate of silica gel with fluorescent indicator for thin-layer chromatography. extract with a reflux condenser for 1 hour and filter. add 100 mL of methanol.67 g Ginger 0. weigh 1 g of Cnidium Rhizome. add 10 mL of water. Examine under ultraviolet light (main wavelength: 254 nm): one spot among the spots from the test solution and a spot from the standard solution show the same color and the same Rf value.Pulverize Ssanghwatang Extract Granules.93) in Licorice for a dose (one sachet). weigh equivalent to 1 g of Prepared Rehmannia Root. Astragalus Root Licorice.32 g to 1. weigh 1 g of Prepared Rehmannia Root. Prepared Rehmannia Root. shake for 5 minutes. extract with a reflux condenser for 1 hour and filter. add 10 mL of water. extract with a reflux condenser for 1 hour and filter. add 100 mL of methanol. vacuum-concentrate the filtrate until the filtrate becomes 10 mL and use this solution as the test solution. Separately. (5) Astragalus Root . Particle Size Distribution Test It meets the requirement. Vacuum-concentrate the filtrate until the filtrate becomes 10 mL and use this solution as the standard solution. Weigh accurately equivalent to about 10 mg of paeoniflorin. Disintegration Test It meets the requirement. add 10 mL of water. Vacuumconcentrate the filtrate until the filtrate becomes 10 mL and use this solution as the standard solution. Assay (1) Paeoniflorin of Peony Root . Separately. Vacuum-concentrate the filtrate until the filtrate becomes 20 mL and use this solution as the standard solution. add 10 mL of water. Develop the plate with a mixture of toluene and methanol (93 : 7) to a distance of about 10 cm and air-dry the plate. shake for 5 minutes. weigh 1 g of Ginger. add 100 mL of methanol.Pulverize Ssanghwatang Extract Granules. Separately. Spray evenly the plate with po anisaldehyde-sulfuric acid TS and heat at 105 C for 10 min: one spot among the spots from the test solution and a spot from the standard solution show the same color and the same Rf value. weigh equivalent to 1 g of Cinnamon Bark. Develop the plate with a mixture of hexane and ethyl acetate (85 : 15) to a distance of about 10 cm and air-dry the plate. Develop the plate with a mixture of chloroform and methanol (95 : 5) to a distance of about 10 cm and air-dry the plate. Perform the test with the test solution and the standard solution as directed under the Thin-layer Chromatography. shake for 5 minutes. Spot 20 μL each of the test solution and the standard solution on a plate of silica gel for thin-layer chromatography. Part II value. add 100 mL of methanol.1098 Monographs. weigh 1 g of Jujube. shake for 5 minutes. vacuum-concentrate the filtrate until the filtrate becomes 10 mL and use this solution as the test solution. add 100 mL of me- . Vacuumconcentrate the filtrate until the filtrate becomes 10 mL and use this solution as the standard solution. extract with a reflux condenser for 1 hour and filter. Separately. Develop the plate with a mixture of hexane and ethyl acetate (85 : 15) to a distance of about 10 cm and air-dry the plate. (9) Ginger .Take not less than about 20 sachets of Ssanghwatang Extract Granules. shake for 5 minutes. Perform the test with the test solution and the standard solution as directed under the Thin-layer Chromatography. Vacuum-concentrate the filtrate until the filtrate becomes 10 mL and use this solution as the standard solution. add 100 mL of methanol. weigh equivalent to 1 g of Licorice. weigh 1 g of Cinnamon Bark. Spot 20 μL each of the test solution and the standard solution on a plate of silica gel for thin-layer chromatography. extract with a reflux condenser for 1 hour and filter.Pulverize Ssanghwatang Extract Granules. Perform the test with the test solution and the standard solution as directed under the Thin-layer Chromatography. Spray evenly the plate with vanillino sulfuric acid TS and heat at 105 C for 10 min: one spot among the spots from the test solution and a spot from the standard solution show the same color and the same Rf value.Pulverize Ssanghwatang Extract Granules. add 100 mL of methanol. Develop the plate with a mixture of chloroform and methanol (6 : 1) to a distance of about 10 cm and air-dry the plate. extract with a reflux condenser for 1 hour and filter. extract with a reflux condenser for 1 hour and filter. vacuum-concentrate the filtrate until the filtrate becomes 10 mL and use this solution as the test solution. Spot 20 μL each of the test solution and the standard solution on a plate of silica gel with fluorescent indicator for thin-layer chromatography. (6) Licorice . add 100 mL of methanol. add 10 mL of water. vacuumconcentrate the filtrate until the filtrate becomes 10 mL and use this solution as the test solution. vacuum-concentrate the filtrate until the filtrate becomes 10 mL and use this solution as the test solution. weigh 1 g of Astragalus Root. Examine under ultraviolet light (main wavelength: 365 nm): one spot among the spots from the test solution and a spot from the standard solution show the same color and the same Rf value. add 100 mL of methanol. shake for 5 minutes. Spray evenly the plate with vanillino sulfuric acid TS and heat at 105 C for 10 minutes. add 100 mL of methanol. Spot 20 μL each of the test solution and the standard solution on a plate of silica gel for thin-layer chromatography. Spot 20 μL each of the test solution and the standard solution on a plate of silica gel for thin-layer chromatography. (7) Cinnamon Bark . add 100 mL of methanol. add 10 mL of water. shake for 5 minutes.Pulverize Ssanghwatang Extract Granules. extract with a reflux condenser for 1 hour and filter. weigh equivalent to 1 g of Jujube. add 10 mL of water. weigh accurately and pulverize. add 100 mL of methanol. Spray evenly the plate with p-anisaldehydesulfuric acid TS and o heat at 105 C for 10 minutes: one spot among the spots from the test solution and a spot from the standard solution show the same color and the same Rf value. add 100 mL of methanol. Separately. vacuumconcentrate the filtrate until the filtrate becomes 10 mL and use this solution as the test solution. Perform the test with the test solution and the standard solution as directed under the Thin-layer Chromatography. (8) Jujube . Spray evenly the plate with a saturated solution of odianisidine-acetic anhydride freshly prepared: one spot among the spots from the test solution and a spot from the standard solution show the same color and the same Rf value. weigh 1 g of Licorice. Separately. add 10 mL of water. weigh equivalent to 1 g of Ginger. Perform the test with the test solution and the standard solution as directed under the Thin-layer Chromatography. weigh equivalent to 1 g of Astragalus Root.Pulverize Ssanghwatang Extract Granules. Examine the plate under ultraviolet (main wavelength: 254 nm): Two spots among the several spots from star anis fruit and the each spot from the standard standard (1) and (2) show the same color and the same Rf value.Take not less than about 20 sachets of Ssanghwatang Extract Granules. prepared in the same manner as the test solution. Fruit stalk is 3 cm to 4 cm in length. add 50 mL of chloroform. Loss on Drying Not more than 11. vacuumconcentrate the filtrate until the filtrate becomes 50 mL and use this solution as the test solution. and use this solution as the standard solution. Separately. lustrous. connected to the base of the fruit. Column temperature: An ordinary temperature. and 6 mm to 10 mm in height. Each follicle is 1 cm to 2 cm in length. Star Anis Fruit Illici Veri Fructus Star Anis Fruit is the dried fruit or the dried fruit passed through hot water of Illicium verum Hook. Identification Weigh 1 g of pulverized star anis fruit. extract with a reflux condenser for 1 hour and filter. packed with octadecylsilyl silica gel for liquid chromatography (5 μm in particle diameter). Swertia Herb contains not less than 2. and use this solution as the test solution. Pipet 10 μL each of the test solution and the standard solution and perform the test as directed under the Liquid Chromatography according to the following operating conditions. Star Anis Fruit is aromatic and taste is pungent and sweet. respectively. After cooling. Weigh accurately equivalent to 10 mg of glycyrrhizic acid. of the test solution and the standard solution. Develop the plater with a mixture of hexane and ethyl acetate (20 : 1) to a distance of about 10 cm and air-dry the plate. Mobile phase: A mixture of methanol. weigh accurately and pulverize. Separately. curved. A calculated on the anhydrous basis × T AS Operating conditions Detector: An ultraviolet absorption photometer (wavelength: 254 nm). dissolve 1 mg each of Anetole RS and Anesaldehyde RS to 1 mL of ethanol and use these solutions as the standard solution (1) and the standard solution (2). allow to stand for 5 minutes and filter. add 10 mL of hexane.0% of swertiamarin (C16H22O10: 374.34). with summit beaked and upper part mostly dehiscent. reddish brown. add 50 mL of 3 mol/L of sulfuric acid TS and hydrolyze in a water bath for 1 hour. with a hilum at the acute end. smooth and lustrous. extract twice repetitively. add 50 mL of water. 3 mm to 5 mm in width. To the residue. Inner surface is pale brown. dissolve the residue in methanol to make exactly 50 mL. add 100 mL of methanol. combine chloroform layers and filter through anhydrous sodium sulfurate. AT and AS . shake to mix. (2) as directed under Thin-layer Chromatography. irregularly wrinkled. extract three times repetitively. fil.KP VIII 1099 thanol. respectively Amount (mg) of glycyrrhiz ic acid (C 42 H 62 O 16 ) = amount (mg) of Glycyrrhiz ic Acid RS. Determine the peak areas. External surface is reddish brown. Vacuumconcentrate the filtrate. After cooling. calculated on the . Column: A stainless steel column.0% Swertia Herb Swertia Herba Swertia Herb is the whole herb of Swertia japonica Makino (Gentianaceae) collected during the blooming season. (2) on a plate of silica gel with a fluorescent indicator for thin-layer chromatography. Perform the test as directed under Assay for Peony Root. heat and extract with a reflux condenser in a water bath for 30 minutes. Separately. combine the filtrates. Description Star Anis Fruit is mostly aggregate fruit of 8 follicles radiated from the central axis.0 mL/min Packaging and Storage Preserve in tight containers. dissolve in methanol to make exactly 50 mL and use this solution as the standard solution. Each follicle contains a compressed-ovoid seed which is about 6 mm in length. heat and extract with a reflux condenser in a water bath for 3 hours. Use this solution as the test solution. 4 mm to 6 mm in inside diameter and 15 cm to 25 cm in length. water and acetic anhydride (78 : 19 : 3) Flow rate: 1. (2) Glycyrrhizic acid of Licorice .. weigh accurately about 10 mg of Glycyrrhizic acid RS (separately determined the water content). take the chloroform layer in separatory funnel. Spot 5 μ each of the test solution and the standard solution (1). and usually deciduous. Endosperm is white and oily.0% Ash Not more than 4. weigh accurately about 10 mg of Paeoniflorin RS (separately determined the water content). add 30 mL of chloroform. use the solution. prepared prepare the solution. Perform the test with the test solution and the standard solution (1). Texture is hard and brittle.0% Extract Content Dilute ethanol-soluble extract Not less than 15. Terminalia Fruit Terminaliae Fructus Terminalia Fruit is the ripe fruit of Terminalia chebula Retzins or Terminalia chebula Retzins var. overlapped and rolled. Column: A stainless steel column. pungent. add the mobile phase to make exactly 20 mL. Peduncle is distincted. Under a magnifying glass. weigh 2 mg of Swertiamarin RS. dissolve in 1 mL of ethanol. Seed coat is yellowish brown and 2 cotyledons are white. Column temperature: A constant temperature of about 50 o C . Identification Weigh 2 g of pulverized Swertia Herb. tomentella Kurt. and the margin of lobe resembles eyelashes. about 4. . shake for 5 minutes. Examine under ultraviolet light (broad spectrum wavelength): one spot among the several spots from the test solution and a red spot from the standard solution show the same color and the same Rf value. entire and sessile. of the peak area of swertiamarin of each solution. calculated on the anhydrous basis × AT ×5 AS Operating conditions Detector: An ultraviolet absorption photometer (wavelength: 238 nm). Combine the extracts. Separately. Perform the test with 10 μL each of the test solution and the standard solution as directed under the Liquid Chromatography according to the following operating conditions. and clearly dividing each peak. and the root is yellow-brown. Use a column giving elution of theophylline and swertiamarin in this order. and determine AT and AS. oblong. coarse and hard. and use this solution as the standard solution. Loss on Drying Not more than 12. 10 mm to 15 mm in diameter. 2 cm to 4 cm in length. Terminalia Fruit has slight characteristic order and sour. 20 cm to 25 cm in diameter. The stems are cylindrical. and extremely bitter and lasting taste.0% (6 hours). Swertia Herb has slight odor. 1 cm to 4 cm in length. and 20 cm in length. the flowers are white to whitish. add the mobile phase to make exactly 20 mL. Separately. Then develop the plate with a mixture of ethyl acetate. Kernel is narrow. centrifuge. about 2 mm in diameter. add 40 mL of methanol.0%.5%. the lobes are narrow. Spot 10 μL each of the test solution and the standard solution on a plate of silica gel with fluorescent indicator for thin-layer chromatography. pale yellow. Mobile phase: A mixture of acetonitrile and water (9:91).5%. To the residue add 40 mL of methanol and proceed in the same manner. and use this solution as the standard solution. opposite leaves.0 mL of this solution. 1 mm 5 mm in width. Purity Foreign matter⎯The amount of straw and other foreign matters contained in Swertia Herb is not more than 1. The leaves and stems are dark green to dark purple or yellow-brown. with 5 to 6 ridgeline and irregular wrinkles. the relative standard deviation of the peak area of swertiamarin is not more than 1. The five stamens grow on the tube of the corolla and stand alternately in a row with corolla-lobes. and use the filtrate as the test solution.0 mL of this solution. and 2 mm to 4 mm in diameter. System suitability System performance: Dissolve 1 mg each of Swertiamarin RS and theophylline in the mobile phase to make 10 mL.6 mm in inside diameter and about 15 cm in length. External surface is yellowish-brown to dark brown.1100 Monographs. n-propanol and water (6 : 4 : 3) to a distance of about 10 cm. Amount (mg) of swertiamarin (C16 H 22 O 10 ) = amount (mg) of Swertiamarin RS. stems. and basal scar of peduncle. (Combretaceae). lignified roots. oblong or ovoid. Assay Weigh accurately about 1 g of pulverized Swertia Herb in a glass-stoppered centrifuge tube. filter. shake for 15 minutes. Texture is hard. and air-dry the plate. and add methanol to make exactly 100 mL. When smoothed by immersion in water. The corolla is split deeply as five lobes. Description Terminalia Fruit is the fruit. add methanol to make exactly 20 mL. usually short. packed with octadecylsilyl silica gel for liquid chromatography (5 μm in particle diameter). Ash Not more than 6. add 10 mL of ethanol. about 10 mm in length. Part II dried basis. Sarcocarp is 2 mm to 4 mm in thickness. weigh accurately about 10 mg of Swertiamarin RS (previously dertermine the water content). Perform the test with the test solution and the standard solution as directed under Thin-layer Chromatography. and separate the supernatant liquid. ofter lustrous. consisted of flowers. and use this solution as the test solution. Pipet 5. Perform the test with 10 μL of this solution according to the above operating conditions and calculate the resolution. and occasionally with branches. the leaves are linear to narrow lanceolate. and later sweet taste. System repeatability: When the test is repeated six times with 10 μL of the standard solution under the above operating conditions. Flow rate: Adjust the flow rate so that the retention time of swertiamarin is about 12 minutes. ellipsoidal. Pipet exactly 5. Description Swertia Herb is the whole herb. at the base of the inner surface is with two elliptical nectarines juxtaposed. Acid-insoluble Ash Not more than 0.5 g of pulverized Terminalia Fruit.0 mL of this solution. hard in texture and difficult to break. Pipet 10. long ovoid or long elliptical. about 20 mg of Cinobufagin RS (previously dried in a desiccator of silica gel for 24 hours). Separately. 3 mm to 5 mm in length and 2 mm to 3 mm in diameter. (ii) Evaporate 1 mL of the test solution in a waterbath to dryness.1 g of pulverized Toad Venom with 5 mL of a solution of tartaric acid (1 in 100) in a waterbath for 10 minutes and filter.0%. the mass of one disk being about 8 g. Wash the residue with 30 mL of methanol. combine the washing and filtrate. add carefully 1 mL of p-dimethylaminobenzaldehyde TS. add methanol to make exactly 25 mL and use this solution as the test solution. External surface is pale yellow or yellowish white. heat for l0 minutes in a waterbath and add l0 mL of water: a blue color develops.8% of bufosteroid. somewhat lustrous.0%. covered with membranous tegmen. Thuja Seed has characteristic odor and weak taste. (i) Take 1 mL of the test solution and add carefully 1 mL of sulfuric acid to make two layers: a yellow color develops at the zone of contact. Apex is slightly acute. (2) Warm 0. and dissolve each in methanol to make exactly 100 mL. cool and filter. Thuja Seed Thujae Semen Thuja Seed is the seed of Thuja orientalis Linné (Cupressaceae ). previously dried in a desiccator (silica gel) for 24 hours. add methanol to make exactly l00 mL. filter and perform the following tests using the filtrate as the test solution. shake and mix well. about 8 cm in diameter and about 15 mm in thickness. add 5. and about 20 mg of Redibufogenin RS (previously dried in a desiccator of silica gel for 24 hours).0%. Acid-insoluble Ash Not more than 2. and filter. from which seed coat is removed. weigh accurately about 10 mg of Bufalin RS (previously dried in a desiccator of silica gel for 24 hours). Purity Seed coat – Thuja Seed contains not more than 1. followed a little later by a lasting sensation of numbness.0%.KP VIII 1101 Identification Weigh 0. warm under a reflux condenser in a water-bath for l0 minutes. Description Thuja Seed is the seed. To 1 mL of the filtrate. Acid-insoluble Ash Not more than 1. about 3 cm in diameter and about 5 mm in thickness. dissolve the residue in 25 mL of methanol and determine the absorption spectrum of the solution as directed under the Ultraviolet-visible Spectrophotometry: it exhibits a maximum at about 300 nm.5 g of pulverized Toad Venom. transverse section is white to yellowish white.l g of pulverized Toad Venom. approximately uniform and horny.0%. External surface is red-brown to blackish brown. Toad Venom contains not less than 5. Loss on Drying Not more than 7. Extract Content than 50. Description Toad Venom is the secretion.0% of penduncle and other foreign matter.0% (6 hours). Ash Not more than 5.0% of the endocarp and other foreign matter. Identification (1) Weigh 0. Texture is soft and oily. add 50 mL of methanol.0%. To this solution. Assay Weigh accurately about 0. Under a microscope. add 5 mL of chloroform. Add 1 to 2 drops of ferric chloride TS to the filtrate: a dark purple color develops Purity Foreign matter—Terminalia Fruit contains less than 2. with much albumen and oil. Perform the test with 10 μL each of the test solution and the standard solutions . Ash Not more than 6. Ether-soluble extract—Not less Toad Venom Bufonis Venenum Toad Venom is the venomous secretion of Bufo bufo gargarizans Cantor or Bufo melanostictus Schneider (Bufonidae). Fractured surface is nearly flat and edges of broken pieces red-brown and translucent. heat under a reflux condenser in a water-bath for 1 hour. add 10 mL of water. Loss on Drying Not more than 12.0%. Ash Not more than 2. When dried. in round disk with slightly dented bottom and protuberant sur- face.0 mL of the internal standard solution. the mass of one disk being about 80 g to 90 g or it is a round disk with almost flattened surfaces on both sides.4% Extract Content Dilute ethanol-soluble extract— Not less than 35. with a small deep brown spot and bast obtusely rounded. Toad Venom is odorless and it has bitter and irritating taste.0%. proceed in the same manner as the test solution and use these solutions as the standard solution. then changes to red after standing for l5 to 20 minutes and the chloroform layer acquires a pale red color. Pipet 10 mL of this solution. A single-layer of cell between mesocarp and endocarp contains solitary crystals of calcium oxalate. Determine the ratios. Ash Not more than 4. heat on a water bath for 2 minutes and filter. from which the cortex has been removed. bufalin.0% Ash Not more than 13. followed by bitterness. Tribulus Fruit Tribulus Fruit Tribulus Fruit is the ripe fruit of Tribulus terrestris Linné. QTC and QSC.0% of fruit stalk. External surface is pale yellowish white and with irregular pattern of vascular bundles appearing as brownish yellow lines. of the peak area of bufalin. to that of the internal standard in each solution and designate the total amount as an amount of bufosteroid.0% Acid-insoluble Ash Not more than 2. Selection of column: When the procedure is run with 10 μL of the standard solution under the above operating conditions.0%. External surface is grayish green to grayish brown. a bluish purple or green color at the upper layer. the transverse section reveals the wide medullary rays and yellowish brown spots or small holes formed by vessels. The pericarp is hard in texture and a fractured surface is pale yellow. Description Trichosanthes Root is irregular cylinder root. Cotyledons of seed contain oil droplets. Trichosanthes Root has slightly characteristic odor and slightly bitter taste. Mobile phase: A mixture of diluted phosphoric acid (1 in 1000) and acetonitrile (11 : 9).1102 Monographs. Each mericarp is often separated. Identification Weigh 0. Each mericarp contains 1 – 3 seeds. Add carefully 1 mL of sulfuric acid to 1 mL of the filtrate: a reddish brown color appears at the zone of contact. QTB and QSB.0%. Amount (mg) of bufalin (C 24 H 34 O 4 ) = amount (mg) of Bufalin RS × Q TB Q SB Amount (mg) of cinobufagin (C26 H 34 O 6 ) Q = amount (mg) of Cinobufagin RS × TC QSC Amount (mg) of redibufogenin (C 24 H 32 O 4 ) = amount (mg) of Redibufogenin RS × Q TB Q SB Internal standard solution⎯A solution of indometacin in methanol (1 in 4000). packed with octadecylsilyl silica gel for liquid chromatography (5 μm to 10 μm in particle diameter).2 g of pulverized Tribulus Fruitm. 7 mm to 12 mm in diameter. 4 mm to 6 mm in inside diameter and 15 cm to 30cm in length. Operating conditions Detector: An ultraviolet absorption photometer (wavelength: 300 nm). respectively. of the peak area of resibufogenin. numerous small processes on midrib. a transverse section reveals epicarp composed of a single-layered epidermis. for the test solution and the standard solution. Purity (1) Fruit stalk —Tribulus Fruit has Less than 4.5% Extract Content Water-soluble extract Not less than 12. Fractured surface of the root is light yellow and somewhat fibrous. Part II as directed under the Liquid Chromatography according to the following operating conditions. mesocarp composed of parenchyma and sclerenchyma layer and endocarp composed of several-layered fiber cells. the shorter one is 2 mm to 5 mm in length. resibufogenin and the internal standard are eluted in this order and clearly dividing each peak. aleurone grains and occasionally starch grains. . Under magnifying glass. respectively and QTR and QSR. Description Tribulus Fruit is pentagonal star shaped fruit composed of five mericarps.0% Trichosanthes Root Trichosanthis Radix Trichosanthes Root is the root of Trichosanthes kirilowii Maximowicz or Trichosanthes rosthornii Harms (Cucurbitaceae). for the test solution and the standard solution. Loss on Drying Not more than 7. add 3 mL acetic anhydride. 5 cm to 10 cm in length and 3 cm to 5 cm in diameter. cinobufagin. Under a microscope. Column temperature: A constant temperature of about 40 °C. respectively. often cut lengthwise. Column: A stainless steel column. of the peak area of cinobufagin. Tribulus Fruit has almost odorless and mild taste at first. a protrusion and a pair of longer and shorter spines on reverse surface of each mericarp: the longer spine is 3 mm to 7 mm in length. for the test solution and the standard solution. Flow rate: Adjust the flow rate so that the retention time of the internal standard is 16 to 19 minutes. (2) Foreign matter—The amount of foreign matter other than fruit stalk contained in Tribulus Fruit is not more than 1. The upper side is relatively sharp. and 1 mm to 3 mm in diameter. 6 mm to 10 mm in width and about 3.1 mL (50.3 mL of hydrochloric acid to 5 mL of the fitrate: a pale red .KP VIII 1103 Trichosanthes Seed Trichosanthis Semen Trichosanthes Seed is the ripe seed of Trichosanthes kirilowii Maximowicz or Trichosanthes rosthornii Harms (Cucurbitaceae). External surface is deep brown. scaly leaves. Description Vitex Fruit is the fruit. spheroidal and 4 mm to 6 mm in diameter. Add 0. Ash Not more than 9. Ash Not more than 4. the transverse section reveals a thick. and about 2.0 g). Acid-insoluble Ash Not more than 3. and a grayish brown stele. with hilum and the base is obtusely round or relatively narrow.0%. The inner seed coat is membranous and grayish green. and 1 cm to 2 cm in diameter. Valerianae Radix et Rhizoma Loss on Drying Not more than 12.0%. add 2 mL of acetic anhydride.Trichosanthes Seed from Trichosanthes kirilowii is flat elliptical. short rhizome with numerous.3 mL (50. 8 mm to 10 mm in width. distinctly dented scars. each with a white seed. of which 2 is relatively deep. Texuture is light. add 10 mL of ethanol.0% Description Valerian Root is obovoid.0%. flat. External surface is grayish brown to blackish brown. Add 0. . or Vitex trifolia Linné (Verbenaceae). The seed coat is tough and hard. Acid–insoluble ash Not more than 5.0% of fragments of unriped seed coat. Purity (1) fruit stalk—Less than 4.Trichosanthes Seed from Trichosanthes rosthornii is a relatively large and flat seed. light grayish brown cortical layer. about 12 mm to 15 mm in length. slippery.1 g of magnesium and 0. Water-soluble extract—Not less Valerian Root and Rhizome thick and short or thin. Apex is slightly concave.0%. and densely pubescent. The upper side is cutting flat. Description Trichosanthes kirlowii . Identification Weigh 0. 1 mL of silicon resin).0% (6 hours). bearing 4 longitudinal shallow furrows. Flank of rhizome is sometimes accompanied with stolons having Essential Oil Content Not less than 0.5 mm in thickness.1 g of powdered Trichosanthes Seed.5 mm in thickness. and with buds and remains of stem at the crown. (2) Trichosanthes rosthornii . shake well and filter. The root is 10 cm to 15 cm in length. Calyx is 1/3 to 2/3 length of the fruit.0 g. Extract Content than 6.5 g of pulverized Vitex Fruit. Transverse section is showing 4 loculi. Identification Weigh 0. fine and long roots. Two grayish cotyledons are largely oily. External surface has fine longituidinal wrinkles and it is brittle. with dented scar along the margin of the seed. The rhizome is 1 cm to 2 cm in length. Ash Not more than 10. with 5 crenatures. Under a magnifying glass. Tricosanthes Seed has the characteristic odor and a slightly bitter taste. Vitex Fruit Viticis Fructus Vitex Fruit is the ripe fruit of Vitex rotundifolia Linné fil.5%. Packaging and Storage Preserve in tight containers. Purity Foreign matter—Not more than 1.0%. The edge surrounding like ring shape is relatively wide. rough and uneasily broken. (2) Foreign matter—Vitex Fruit contains other foreign matter less than 1. and extremely small. 15 mm to 19 mm in length.0%. Essential Oil Content Not less than 0. Valerian Root is the root and rhizome of Valerianae faurei Briquet or other species of the same genus (Valerianaceae). The texture of the root is hard and difficult to break. External surface is pale brown to deep brown. shake well and heat for 2 minutes in a water-bath and filter.5 mL of sulfuric acid to the fitrate: a reddish brownred color is produced at the zone of the two liquids. Extract Content Dilute ethanol-soluble extract— Not less than 8. Valerian Root has strong and characteristic odor and slightly bitter taste. long. Vitex Fruit has characteristic odor and the taste is weak and slightly pungent. with grayish white persistent calyx and short peduncle at base.reddish purple color appears. covered with grayish white frost-like hairs.0%. 34 g of Viscous extract or concentrate in a suitable method until it becomes 0. Vacuum- .57 g to 2. weigh equivalent to 1 g of pulverized Moutan Root Bark. Poria. proceeding in the same manner as the test solution. weigh accurately about 1 g of pulverized Prepared Rehmannia Root and use this solution.Pulverize Youkmijihwang Extract Granules. Cornus Fruit. add water to the residue and dissolve. Alisma Rhizome 1. add 100 mL of methanol. weigh equivalent to 1 g of Prepared Rehmannia Root. Vacuum-concentrate the filtrate under 60 C until it becomes 1. shake for 5 minutes.0% Ash Not more than 7.00g ___________________________________________ Pulverize the above crude drugs to coarse powder. Develop the plate with a mixture of ethyl formate.1104 Monographs. as the standard solution. Identification Weigh 0. Add 30 mL of ethyl acetate and extract in separatory funnel.Pulvarize Youmijiwhang Extract Granules. Evaporate the filtrate to dryness in vacuum. Evaporate the layer of ethyl acetate to dryness.0% Youkmijihwang Extract Granules Youkmijihwang Extract Granules contains no less than 1. add 100 mL of methanol. Spray evenly the plate with po anisaldehyde-sulfuric acid TS and heat at 105 C for 10 minutes: one spot among the spots from the test solution and a spot from the standard solution show the same color and the same Rf value. relatively even at the one side.00 g Moutan Root Bark. grayish black with longitudinal wrinkles and the seet coat is membranous. To the filtrate.22 g of Dry extract. extract with a reflux condenser for 1 hour. 10 mm to 15 mm in length. weigh accurately about 1 g of Moutan Root Bark RMPM. Hyunggeyungyo Extract Granules is prepared as directed under Granules. add eight to ten fold of water.0% Acid-insoluble Ash Not more than 1. shake for 5 minutes. extract with a reflux condenser for 1 hour and filter. Vacuum-concentrate the filtrate until the filtrate becomes 10 mL and use this solution as the standard solution. weigh each crude drugs. Dioscorea Rhizome. macerate with 10 mL of water and filter. extract with a reflux condenser for 1 hour and filter.4 mg of paenioflorin (C23H28 O11: 480. The apex has two relatively thick spines. External surface is yellowish brown to yellowish green with hooked spines throughout. Loss on Drying Not more than 7. pale gray and oily with two cotyledons. Spot 20 μL each of the test solution and the standard solution on a plate of silica gel for thin-layer chromatography. add 100 mL of methanol. Description Xanthium Fruit is the fusiform or ovoid fruit. (3) Poria . each having an achene. Separately. Separately. add 100 mL of methanol. Perform the test with the test solution and the standard solution as directed under the Thinlayer Chromatography. extract with a reflux condenser for 1 hour and filter. put into the extractor.5 g of pulverized Xanthium Fruit. add 2 mL of ethanol and use this solution as the test solution. 4dinitrophenylhydrazine TS and examine under ultraviolet light (main wavelength: 254 nm): one spot among the spots from the test solution and a spot from the standard solution show the same color and the same Rf value. toluene and formic acid (6 : 6 : 5 : 3) to a distance of about 10 cm and air-dry the plate. Spot 20 μL each of the test solution and the standard solution on a plate of silica gel with a fluorescent indicator for thin-layer chromatography.46) in Moutan Root Bark for a dose (a sachet) Method of preparation for a dose (one sachet) Prepared Rehmannia Root 2. The pericarp is thin. Spray evenly the plate with 2. The center of a transverse section show a septum and two loculi. Develop the plate with a mixture of chloroform and methanol (20 : 1) to a distance of about 10 cm and air-dry the plate. (2) Moutan Root Bark .Pulvarize Youkmijiwhang Extract Granules. chloroform. Vacuum-concentrate the filtrate until the filtrate becomes 10 mL and use this solution as the test solution. Part II o Xanthium Fruit Xanthii Fructus Xanthium Fruit is the ripe fruit of Xanthium strumarium Linné (Compositae).82 g to 1. Perform the test with the test solution and the standard solution as directed under the Thinlayer Chromatography. extract for 2 to 3 hours at 80 ~ 100 o C and filter. An achene is slightly fusiform. Texture is hard and rigid. 4 mm to 7 mm in diameter.0% Extract Content Dilute ethanol-soluble extract Not less than 10. add 10 mL of water. The apex of an achene has protruding remains of style. add one droplet of ferric chloride TS: a grayish green color appears. Indentification (1) Prepared Rehmannia Root . add 10 mL of water. cool and filter. Xanthium Fruit has characteristic odor and bitter taste. weigh equivalent to 1 g of Poria. sperated or linked up and the base has a fruit stalk scar. proceed in the same manner as the test solution and use this solution as the standard solution. Extract the residue with chloroform. Spray evenly the plate with p-anisaldehyde-sulfuric acid TS and heat at o 105 C for 10 minutes: one spot among the spots from the test solution and a spot from the standard solution show the same color and the same Rf value. Spot 20 μL each of the test solution and the standard solution on a plate of silica gel with fluorescent indicator for thin-layer chromatography. Perform the test with the test solution and the standard solution as directed under the Thinlayer Chromatography. Vacuum-concentrate the filtrate until the filtrate becomes 10 mL and use this solution as the standard solution. remove the layer of chloroform. Perform the test with the test solution and the standard solution as directed under the Thin-layer Chromatography. weigh accurately about 1 g of pulverized Poria. extract with a sonicator for 30 minutes and filter. (6) Alisma Rhizome . Particle Size Distribution Test It meets the requirement. Develop the plate with a mixture of cyclohexane and ethyl acetate (3 : 1) to a distance of about 10 cm and air-dry the plate. cool and filter. Assay (1) Paenioflorin of Moutan Root Bark . cool and filter. Develop the plate with a mixture of chloroform and acetone (1 : 1) to a distance of about 10 cm and air-dry the plate. proceed in the same manner as the test solution and use this solution as the standard solution. calculated on the anhydrous basis × AT AS Operating conditions Detector: An ultraviolet absorption photometer (wavelength: 254 nm). Spray evenly the plate with sulfuric acid TS for spray and heat at 105 o C for 10 minutes: one spot among the spots from the test solution and a spot from the stan- dard solution show the same color and the same Rf value. packed with octadecylsilyl silica gel for liquid chromatography . weigh and pulverize. add 100 mL of methanol. weigh equivalent to 1 g of Alisma Rhizome. add water in the layer of water to make exactly 50 mL and use this solution as the test solution Separately. Spray evenly the plate with p-anisaldehydeo sulfuric acid TS and heat at 105 C for 10 minutes: one spot among the spots from the test solution and a spot from the standard solution show the same color and the same Rf value.Pulverize Youkmijiwhang Extract Granules. Determine the peak areas. add 40 mL of water. methanol and water (60 : 35 : 15) to a distance of about 10 cm and air-dry the plate. extract with a reflux condenser for 1 hour and filter. add 2 mL of ethanol. shake thoroughly and filter. weigh accurately about 5 mg of Paenioflorin RS (separately determined the water content). add water to make exactly 50 mL and use the solution as the standard solution. Spray evenly the plate with p-anisaldehydeo sulfuric acid TS and heat at 105 C for 10 minutes. add 100 mL of ether. Perform the test with the test solution and the standard solution as directed under the Thin-layer Chromatography.KP VIII 1105 concentrate the filtrate until the filtrate becomes 10 mL and use this solution as the test solution. Spot 20 μL each of the test solution and the standard solution on a plate of silica gel with a fluorescent indicator for thin-layer chromatography. Evaporate the filtrate to dryness in vacuum. AT and AS . add 100 mL of methanol. Separately. Separately.Pulverize Youkmijiwhang Extract Granuels. Examine under ultraviolet light (main wavelength: 254 nm): one spot among the spots from the test solution and a spot from the standard solution show the same color and the same Rf value. 4 mm to 6 mm in inside diameter and 15 cm to 25 cm in length. dissolve and use this solution as the test solution. Develop the plate with a mixture of hexane and acetone (7 : 3) to a distance of about 10 cm and air-dry the plate. (4) Cornus Fruit .Pulverize Youkmijiwhang Extract Granules. Separately. Perform the test with the test solution and the standard solution as directed under the Thin-layer Chromatography. weigh accurately about 1 g of pulverized Cornus Fruit RMPM. Evaporate the filtrate to concentrate until the filtrate becomes about 2 mL and use this solution as the test solution. add 50 mL of ethanol and 5 mL of acetic acid. weigh accurately about 1 g of pulverized Dioscorea Rhizome RMPM. Disintegration Test It meets the requirement. Column: A stainless steel column. of the test solution and the standard solution. proceed in the same manner as the test solution and use this solution as the standard solution. Develop the plate with a mixture of dichloromethane. respectively Amount (mg) of paenioflorin (C 42 H 62 O16 ) = amount (mg) of Paenoiflorin RS.Take not less than about 20 sachets of Youkmijiwhang Extract Granules. Separately. (5) Dioscorea Rhizome . weigh accurately about 1 g of pulverized Alisma Rhizome. Evaporate the filtrate to concentrate until the filtrate becomes about 2 mL and use this solution as the test solution. extract with a reflux condenser for 1 hour. extract with a reflux condenser for 1 hour. Pipet 10 μL each of the test solution and the standard solution and perform the test as directed under the Liquid Chromatography according to the following operating conditions. weigh equivalent to 1 g of Dioscorea Rhizome. Weigh accurately equivalent to about 5 mg of paenioflorin. Spot 20 μL each of the test solution and the standard solution on a plate of silica gel for thin-layer chromatography. Spot 20 μL each of the test solution and the standard solution on a plate of silica gel for thin-layer chromatography. weigh equivalent to 1 g of Cornus Fruit. and the base. consisting of follicles. scattered with numerous oil dots and fine reticulated and raised wrinkles. transverse section is waxy. Lee et C. grayish brown to bluish brown.5 g of pulverized Zanthox- ylum Peel. Acid-insoluble Ash Not more than 1. Ling (Zingiberaceae).Zanthoxylum Peel is pericarp. Endodermal ring is yellowish white. Description (1) Rhizome of Curcuma phaeocaulis Zedoary is the rhizome.0 mL/min Packaging and Storage Preserve in tight containers. (3) Foreign matter—The amount of foreign matter other than fruit stalk and twigs contained in Zanthoxylum Peel is not more than 1. (2) Fruit stalk and twig—Less than 5. consisting of 2 to 3 follicles. Develop the plate with a mixture of ethyl acetate. dehiscent in 2 pieces and about 5 mm in diameter. (3) Rhizome of Curcuma wenyujin . Purity (1) Seed—Less than 20. The upper part is conspicuously raised-annulated and with rounded and slightly dented rootlet scars. Zanthoxylum Peel has characteristic odor and slight sweet and pungent taste.0 g). with commonly pale yellow . 0. Follicles are spherical. usually dried after steamed.Zedoary is the rhizome and its fractured surface is commonly yellowish brown to dark brown. (4) Fruit of the twigs—The mass of tannins in Zanthoxylum Peel shows red when vanillin–hydrochloric acid TS added. translucent when observed against light. Part II (5 μm to 10 μm in particle diameter). Zedoary has slightly characteristic odor and slightly bitter and pungent taste. Essential Oil Content Not less than 1. add 10 mL of diluted ethanol (7 in l0). Inner surface is yellowish. slightly raised-annulated. Ash Not more than 6. with numerous dented spots originated from oil sacs: the inner surface is pale yellowish white. Under a microscope. G. Description (1) Pericarp of Zanthoxylum piperitum .Zedoary is the rhizome. Chen et C. Inner surface is almost white and smooth.. ovoid. splitting along the ventral suture and 3 mm to 4 mm in diameter. Curcuma kwangsiensis S. Remains of seed are ovoid.0%. The cortex and stele are easily detachable and endodermal ring is deep brown. Zanthoxylum Fruit has characteristic odor and purgent taste with a sensation of numbness on the tongue. (2) Rhizome of Curcuma kwangsiensis .0%.5 mm to 1 mm in diameter.0%. (2) Pericarp of Zanthoxylum schinifolium .0 mL (30. or remaining rootlets. consisting of 2 to 3 small follicles which is apocarpous at the upper part and grouped on a fruit stalk. External surface is grayish green to dark green. External surface is grayish yellow to grayish brown. The outer surface of pericarp is dark yellow-red to dark red-brown. Identification Weigh 0. 2 cm to 3 cm in diameter.Zanthoxylum Peel is pericarp. Zanthoxylum Peel Zanthoxyli Pericarpium Zanthoxylum Peel is the pericarps of the ripe fruit of Zanthoxylum piperitum De Candolle. Exernal surface is reddish purple to reddish brown. The texture is hard and heavy.0%. 2 cm to 8 cm in length. filter and use this filtrate as the test solution. conical or elongated fusiform. Fractured surface is yellowish brown to brown. Perform the test with the test solution as directed under the Thin-layer Chromatography. F. obtuse and round. Examine under ultraviolet light (main wavelength: 365 nm): one spot showing a grayish red to red color at the Rf value of about 0. mostly singly and 4 mm to 5 mm in diameter. Zanthoxylum schinifolium Siebold et Zuccarini or Zanthoxylum bungeanum Maximowicz (Rutaceae).1106 Monographs. Zedoary Curcumae Rhizoma Zedoary is the rhizome of Curcuma phaeocaulis Val. Spot 10 μL of the test solution on a plate of silica gel with fluorescent indicator for thinlayer chromatography. ethanol and water (8 : 2 : 1) to a distance of about 10 cm and air-dry the plate.Zanthoxylum Peel is pericarp. with black and lustrous surface. with the upper part. Zanthoxylum Peel has strong and characteristic odor and taste lastingly pungent and numb. 3 mm to 4 mm in length.. with commonly pale yellow powder. shake for 30 minutes. elongated ovoid. acetonitrile and acetic acid (86 : 14 : 1) Flow rate: 1. 15 mm to 40 mm in diameter. (3) Pericarp of Zanthoxylum bungeanum . Mobile phase: A mixture of water. Column temperature: An ordinary temperature.7 appears. Endocarp is commonly separated from exocarp at the base. transverse section reveals the external epidermis and the adjoined unicellular layer containing red-brown tannin: the pericarp holds oil sacs being up to approximately 500 μm in diameter and sporadically vascular bundles consisting mainly of spiral vessels: the endocarp consists of stone cell layers: inner epidermal cells very small. Liang or Curcuma wenyujin Y. Each mericarp is flattened spheroidal. stopper the vessel tightly.5%. with grayish brown powder. H. frequently acute and obtuse. scattered with numerous warty oil dots. ovoid. Zizyphus Seed Zizyphi Semen Zizyphus Seed is the ripe seed of Zizyphus jujuba Miller var. shake for 2 minutes and filter. the other end shows a finely raised chalaza. One end shows a linear hilum.KP VIII 1107 or yellowish brown powder. Identification Weigh 0. 1 mL of silicon resin). smooth and lustrous.0%.0 g. add 5 mL of ether. 6 mm to 9 mm in length and 4 to 6 mm in width. Ash Not more than 7. Zizyphus Seed has slight oily odor and taste is weak and soft. Purity Foreign matter—Zizyphus Seed contains not more than 3% of endocarp and other foreign matter. F. spinosa Hu ex H.5 mL of acetic anhydride to the residue and add 1 drop of sulfuric acid: a pale red color is developed at first and it slowly change to reddish purple.5 mL (50. Zedoary has slight characteristic odor. Testa is fragile and covers grayish endosperm and 2 pale yellow cotyledons. External surface is yellowish brown-reddish brown. 2 to 3 mm in thickness. add 0. Description Zizyphus Seed is the seed. Chou (Rhamnaceae). One raised longitudinal line is along with margin from the hilum. Essential Oil Content Not less than 0. The filtrate is removed.5 g of Zizyphus Seed.0%. . Ash Not more than 7. Adsorbed Tetanus Toxoid conforms to the requirements of Adsorbed Tetanus Toxoid in the Specifications for Biological products of Korea. Description Factor VIII Inhibitor Bypassing Activity Complex is a white or pale white. Diphtheria toxoid and a liquid containing tetanus toxoid obtained by detoxifying the tetanus toxin with formalin without impairing its immunogenicity.1108 Monographs. Description Absorbed Diphtheria-Tetanus Combined Toxoid becomes homogeneous. Adsorbed Diphtheria-Tetanus Toxoid-Purified Pertussis Combined Vaccine Adsorbed Diphtheria-Tetanus Toxoid-Purified Pertussis Combined Vaccine is a liquid for injection consisting of a liquid containing the protective antigen of Bordetella pertussis. Cholera Vaccine conforms to the requirements of Cholera Vaccine in the Specifications of Biological Products of Korea. if necessary. Adsorbed Diphtheria-Tetanus Toxoid-Purified Pertuissis Combined Vaccine conformed to the requirement of Adsorbed Diphtheria-Tetanus Toxoid-Purified Pertuissis Combined Vaccine in the Specifications for Biolog- Description Adsorbed Diphtheria-Tetanus ToxoidPurified Pertussis Combined Vaccine becomes homogeneous. Factor VIII Inhibitor Bypassing Activity Complex conforms to the requirements of Factor VIII Inhibitor Bypassing Activity Complex in the Specifications of Biological Products of Korea. Factor VIII Inhibitor Bypassing Activity Complex Factor VIII Inhibitor Bypassing Activity Complex is a dried preparation containing factor VIII inhibitor bypassing activity complex. Cholera Vaccine Cholera Vaccine is a liquid for injection containing inactivated vibrio cholerae of Ogawa and Inaba strains. to which aluminum is added to make the antigen and the toxoid insoluble. Adsorbed Diphtheria-Tetanus Combined Toxoid Adsorbed Diphtheria-Tetanus Combined Toxoid is a liquid for injection containing diphtheria toxoid and tetanus toxoid which are prepared by treating diphtheria toxin and tetanus toxin with formaldehyde by a method involving no appreciable loss the immunogenicity and rendered insoluble by adding aluminum salt. Description Adsorbed Diphtheria Toxoid becomes homogeneous turbid liquid on shaking. Part II ical Products of Korea. Adsorbed Diphtheria Toxoid conforms to the requirements of Adsorbed Diphtheria Toxoid in the Specifications of Biological Products of Korea. turbid liquid on shaking. turbid liquid on shaking. . dried preparation and becomes a colorless liquid on addition of solvent. Adsorbed Diphtheria-Tetanus Combined Toxoid conformed to the requirements of Adsorbed DiphtheriaTetanus Combined Toxoid in the Specifications for Biological Products of Korea. 2) Biologic Preparations Adsorbed Diphtheria Toxoid Adsorbed Diphtheria Toxoid is a liquid for injection containing diphtheria toxoid prepared by treating diphtheria toxin with formaldehyde by a method involving no appreciable loss of the immunogenicity and rendered insoluble with aluminium salt. Description Adsorbed Tetanus Toxoid becomes a homogeneous turbid liquid on shaking. Description Cholera Vaccine is white turbid liquid. Monotypic product may be manufactured. Adsorbed Tetanus Toxoid Adsorbed Tetanus Toxoid is a liquid for injection containing tetanus toxoid prepared by treating tetanus toxin with formaldehyde by a method involving no appreciable loss of immunogenicity and rendered insoluble by the addition of aluminum salt. Freeze-dried Human Blood Coagulation Factor VIII:C is a dried preparation for injection containing human blood coagulation factor III:C removed von Billebrandt factor using monoclonal antibody obtained from human plasma. Description Freeze-dried Concentrated Human Blood Coagulation Factor VIII becomes a colorless or light yellow. Freeze-dried Human Blood Coagulation Factor VIII:C conforms to the requirements of Factor VIII:C Monoclonal Antibody-purified. Freeze-Dried BCG Vaccine Freeze-dried BCG Vaccine contains a dried preparation for injection containing live bacteria derived from a culture of the baccilus of Calmette and Guerin. Freeze-dried Concentrated Human Antithrombin III Freeze-dried Concentrated Human Antithrombin III is a dried preparation containing Human Antithrombin Ⅲ of human serum. clear liquid on addition of solvent. Description Freeze-dried BCG Vaccine becomes a white to light yellow. clear or slightly turbid liquid on addition of solvent. Description Freeze-Dried Agkistrodon (Salmusa) Antivenum (Equine) becomes a colorless or light yellow-brown. Freeze-dried Human Blood Coagulation Factor VIII:C Factor VIII:C Monoclonal Antibody-purified. Freeze-dried Concentrated Human Blood Coagulation Factor VIII conforms to the requirements of Freezedried Concentrated Human Blood Coagulation Factor VIII in the Specifications of Biological Products of Korea. except for coagulatory proteins. except for coagulatory proteins. Freeze-dried Concentrated Human Antithrombin III conforms to the requirements of Freeze-dried Concentrated Human Antithrombin Ⅲ in the Specifications of Biological Products of Korea. clear liquid or slightly whitish turbid liquid on addition of solvent. Freeze-dried Concentrated Human Blood Coagulation Factor VIII (dry heat treated) conforms to the requirements of Freeze-dried Concentrated Human Blood Coagulation Factor VIII (dry heat treated) in the Specifications of Biological Products of Korea. Freeze-dried BCG Vaccine conforms to the requirements of Freeze-dried BCG Vaccine in the Specifications for Biological Products of Korea. . Freeze-dried Human Blood Coagulation Factor VIII:C in the Specifications for Biological products of Korea.KP VIII 1109 Factor VIII:C Monoclonal Antibody-purified. Freeze-dried Concentrated Human Blood Coagulation Factor VIII (dry heat treated) Freeze-dried Concentrated Human Blood Coagulation Factor VIII (dry heat treated) contains blood coagulation factor VIII of human serum and is a dried preparation for injection having low protein contents. Freeze-Dried Agkistrodon (Salmusa) Antivenum (Equine) conforms to the requirements of Freeze-Dried Agkistrodon (Salmusa) Antivenum (Equine) in the Specifications of Biological Products of Korea. colorless or yellowish solution in addition of solvent. turbid liquid on addition of solvent. Description Freeze-dried Concentrated Human Antithrombin III becomes a colorless or light yellow. Factor VIII:C Monoclonal Antibody-purified. Freeze-dried Human Blood Coagulation Factor VIII:C is a white dried preparation and becomes clear. Description Factor VIII:C Monoclonal Antibodypurified. Freeze-dried Concentrated Human Blood Coagulation Factor VIII Freeze-dried Concentrated Human Blood Coagulation Factor VIII contains blood coagulation factor VIII of human serum and is a dried preparation for injection having low protein contents. Freeze-Dried Agkistrodon (Salmusa) Antivenom (Equine) Freeze-Dried Agkistrodon (Salmusa) Antivenum (Equine) contains Agkistrodon (Salmusa) Antivenum in immunoglobulin of horse origin. mumps and rubella virus. clear solution. Freeze-dried Human Fibrinogen Freeze-dried Human Fibrinogen is a dried powder or solid that contains fibrinogen of human plasma. dried preparation and becomes a colorless or light yellow. Description Freeze-Dried Diphtheria Antitoxin (Equine) becomes a colorless or light yellow-brown. Freeze-Dried Live Attenuated Measles Vaccine conforms to the requirements of Freeze-Dried Live Attenuated Measles Vaccine in the Specifications for Biological Products of Korea. Freeze-dried Human Normal Immunoglobulin with Histamine Freeze-dried Human Normal Immunoglobulin with Histamine is a dried preparation containing histamine 2 acid salt and immunoglobulin G obtained from serum globulin of human plasma. Freeze-Dried Live Attenuated Measles-Mumps-Rubella Combined Vaccine Freeze-Dried Live Attenuated Measles-Mumps-Rubella Combined Vaccine is a dried preparation for injection containing live attenuated measles. clear liquid or a slightly whitish turbid liquid on addition of solvent. Freeze-dried Human Fibrinogen conforms to the requirements of Freeze-dried Human Fibrinogen in the Specifications of Biological Products of Korea. Freeze-dried Human Blood Coagulation Factor Ⅸ Complex conforms to the requirements of Freeze-dried Human Blood Coagulation Factor Ⅸ Complex in the Specifications of Biological Products of Korea. the preparation becomes a white or pale yellow. Description Freeze-dried Human Normal Immunoglobulin with Histamine becomes clear. colorless or yellowish liquid on addition of solvent. Freeze-Dried Diphtheria Antitoxin (Equine) Freeze-Dried Diphtheria Antitoxin (Equine) contains diphtheria antitoxin in immunoglobulin of horse origin. Freeze-dried Human Normal Immunoglobulin with Histamine conforms to the requirements of Freezedried Human Normal Immunoglobulin with Histamine in the Specifications of Biologic Products of Korea. Description Freeze-Dried Live Attenuated Measles Vaccine becomes colorless to reddish clear liquid on addition of solvent. Description Freeze-Dried Live Attenuated MeaslesMumps-Rubella Combined Vaccine becomes colorless to reddish clear liquid on addition of solvent. Description When reconstituted with a solvent stated on the label. Part II Description Freeze-dried Concentrated Human Blood Coagulation Factor VIII (dry heat treated) is a white or pale white.1110 Monographs. Freeze-dried Human Blood Coagulation Factor Ⅸ Complex Freeze-dried Human Blood Coagulation Factor Ⅸ Complex is a preparation that contains blood coagulation factor IX complex of human plasma. the preparation forms an almost colorless. Freeze-Dried Diphtheria Antitoxin (Equine) conforms to the requirement of Freeze-Dried Diphtheria Antitoxin (Equine) in the Specifications for Biological Product of Korea. Description When reconstituted with a solvent stated on the label. Freeze-Dried Live Attenuated Measles-Mumps-Rubella Combined Vaccine conforms to the requirements of Freeze-Dried Live Attenuated Measles-Mumps-Rubella Combined Vaccine in the Specifications of Biological Products of Korea. . Freeze-Dried Live Attenuated Measles Vaccine Freeze-Dried Live Attenuated Measles Vaccine a dried preparation for injection containing live attenuated Measles virus. slightly opalescent solution. clear or slightly turbid liquid on addition of solvent. Freeze-Dried Live Attenuated Rubella Vaccine conforms to the requirements of Freeze-Dried Live Attenuated Rubella Vaccine in the Specifications for Biological Products of Korea. Human Normal Immunoglobulin conforms to the requirements of Human Normal Immunoglobulin in the Specifications for Biological Products of Korea. Human Hepatitis B Immunoglobulin conforms to the requirements of Human Hepatitis B Immunoglobulin in the Specifications of Biological Products of Korea. Freeze-Dried Live Attenuated Rubella Vaccine Freeze-Dried Live Attenuated Rubella Vaccine is a dried preparation for injection containing live attenuated rubella virus. Description Human Normal Immunoglobulin is a clear. transparent liquid preparation added maltose as tranquilizer in the solution containing Human Hepatitis B Immunoglobulin-G obtained from through S/D treatment for the cooled ethanol fractionation and deactivated virus to the blood plasma being used in the fractionate preparation showing positive antibody to the surface antigen of hepatitis B.KP VIII 1111 Freeze-Dried Live Attenuated Measles-Mumps Combined Vaccine Freeze-Dried Live Attenuated Measles-Mumps Combined Vaccine a dried preparation for injection containing live attenuated measles and mumps virus. Description Human Hepatitis B Immunoglobulin for Intravenous Administration is a colorless or yellowish-brown. Description Freeze-Dried Live Attenuated Mumps Vaccine becomes clear. yellowish or reddish clear liquid on addition of solvent. Human Hepatitis B Immunoglobulin Human Hepatitis B Immunoglobulin is a liquid for injection containing hepatitis B immunoglobulin which is a kind of human immunoglobulin G. colorless or yellowish red liquid on addition of solvent. . Freeze-Dried Live Mumps Vaccine conforms to the requirements of Freeze-Dried Live Attenuated Mumps Vaccine in the Specifications of Biologic Products of Korea. transparent liquid preparation. Description Human Hepatitis B Immunoglobulin a colorless or yellowish-brown. Description Freeze-Dried Live Attenuated MeaslesMumps Combined Vaccine becomes colorless to reddish clear liquid on addition of solvent. Freeze-Dried Live Mumps Vaccine Freeze-Dried Live Mumps Vaccine is a dried preparation for injection containing live attenuated mump virus. transparent liquid preparation. this solution is a colorless or yellowish-brown. colorless or yellow-brown liquid.. Human Hepatitis B Immunoglobulin for Intravenous Administration Human Hepatitis B Immunoglobulin for Intravenous Administration is not detected hepatitis B antigen. Description Freeze-Dried Live Attenuated Rubella Vaccine becomes a colorless. Human Hepatitis B Immunoglobulin for Intravenous Administration conforms to the requirements of Human Hepatitis B Immunoglobulin for Intravenous Administration in the Specifications for Biological Products of Korea. Human Normal Immunoglobulin Human Normal Immunoglobulin is a liquid for injection containing immunoglobulin G in serum globulins of humans. Freeze-Dried Live Attenuated Measles-Mumps Combined Vaccine conforms to the requirements of FreezeDried Live Attenuated Measles-Mumps Combined Vaccine in the Specifications of Biological Products of Korea.. Human Tetanus Immunoglobulin Human Tetanus Immunoglobulin is a liquid for injection containing tetanus antitoxin among Human Tetanus Immunoglobulin-G. Description Inactivated Hepatitis B Vaccine becomes a homogeneous. Human Varicella Immunoglobulin Human Varicella Immunoglobulin is a liquid preparation for injection containing human varicella antibody among Human Immunoglobulin-G. white turbid liquid on shaking. Human Plasma Protein Fraction conforms to the requirements of Human Plasma Protein Fraction in the Specifications of Biological Products of Korea. Influenza HA Vaccine conforms to the requirements of Influenza HA Vaccine in the Specifications of Biological Products of Korea. yellow-brown liquid.25) is a colorless liquid. Description Human Normal Serum Albumin is a clear.25) Human Normal Immunoglobulin in Maltose (pH4. transparent liquid preparation. Description Human Plasma Protein Fraction is a clear. Description Human Normal Immunoglobulin in Maltose (pH4. Human Normal Immunoglobulin in Maltose (pH4. yellow-brown liquid.25) conforms to the requirements of Human Normal Immunoglobulin in Maltose (pH4. Human Varicella Immunoglobulin conforms to the requirements of Human Varicella Immunoglobulin in the Specifications for Biological Products of Korea.1112 Monographs. Description Human Tetanus Immunoglobulin is a colorless or yellowish-brown. for sectional preparation. Human Tetanus Immunoglobulin conforms to the requirements of Human Tetanus Immunoglobulin in the specifications for Biological Products of Korea. Human Plasma Protein Fraction Human Plasma Protein Fraction is a liquid for injection containing albumin and other plasma protein of human serum. by S/D treatment for the inactivation of virus and cold ethanol partialization method. Influenza HA Vaccine Influenza HA Vaccine is a liquid for injection containing hemagglutinin of influenza virus. Description Human Varicella Immunoglobulin is a colorless or yellowish-brown. Description Inactivated Rabies Vaccine is a white to light yellow-brown turbid liquid. Inactivated Hepatitis B Vaccine conforms to the requirements of Inactivated Hepatitis B Vaccine in the Specifications of Biological Products of Korea.25) in the Specifications of Biological Products of Korea. Human Normal Serum Albumin conforms to the requirements of Human Normal Serum Albumin in the Specifications of Biological Products of Korea. Part II Human Normal Immunoglobulin in Maltose (pH4. Inactivated Hepatitis B Vaccine Inactivated Hepatitis B Vaccine is a liquid for injection containing inactivated surface antigen of hepatitis B virus. . transparent liquid preparationon.25) is a colorless solution for injection prepared from the addition of maltose as a stabilizer to the liquid containing human immunoglobulin G obtained from plasma. Inactivated Rabies Vaccine conforms to the Requirements of Inactivated Rabies Vaccine in the Specifications of Biological Products of Korea. Human Normal Serum Albumin Human Normal Serum Albumin is a liquid for injection containing albumin of human serum. Inactivated Rabies Vaccine Inactivated Rabies Vaccine is a liquid for injection containing inactivated rabies virus. Freezedried Human Blood Coagulation Factor VIII:C is a white or off-white powder and becomes a clear. colorless solution when reconstituted with a solvent stated on the label. white turbid liquid on shaking. Freeze-dried Human Blood Coagulation Factor VIII:C is plasma derived and a dried powder for injection. Freeze-dried Human Blood Coagulation Factor Ⅷ:C Monoclonal Antibody-purified. Monovalent or bivalent product may be prepared. Freezedried Human Blood Coagulation Factor VIII:C in the specifications of Biological Products of Korea. 2 and 3. Description Live Oral Poliomyelitis Vaccine is a light yellow-red to light red. white turbid liquid on shaking. Freeze-dried Human Blood Coagulation Factor VIII:C conforms to the requirements of Monoclonal antibody-purified. Description Purified Protein Derivative of Tuberculin (PPD) is a clear. Pertussis Vaccine Pertussis Vaccine is a liquid for injection containing inactivated Bordetella pertusis. Description Leptospira Vaccine becomes a homogeneous. Leptospira Vaccine Leptospira Vaccine is a liquid for injection containing inactivated Leptospira strain. Monoclonal Antibody-purified. Japanese Encephalitis Vaccine conforms to the requirements of Japanese Encephalitis Vaccine in the Specifications of Biological Products of Korea. Live Oral Poliomyelitis Vaccine conforms to the requirements of Live Oral Poliomyelitis Vaccine in the Specifications for Biological Products of Korea. Monoclonal Antibody-purified. Typhoid Vaccine conforms to the requirements of Typhoid Vaccine in the Specifications of Biological Products of Korea. if necessary. Description Pertussis Vaccine becomes a homogeneous. Purified Protein Derivative of Tuberculin (PPD) conforms to the requirements of Purified Protein Derivative of Tuberculin (PPD) in the Specifications for Biological products of Korea. Pertussis Vaccine conforms to the requirements of Pertussis Vaccine in the Specifications of Biological Products of Korea. Purified Protein Derivative of Tuberculin (PPD) Purified Protein Derivative of Tuberculin is a liquid for injection containing culture filtrate of the tubercle bacillus (Mycobacterium tuberculosis or Mycobacterium bovis). . Description Japanese Encephalitis Vaccine is clear liquid or a slightly whitish turbid and colorless liquid. clear liquid. Japanese Encephalitis Vaccine Japanese Encephalitis Vaccine is a liquid for injection containing inactivated Japanese Encephalitis Virus. Monoclonal Antibody-purified. Description Typhoid Vaccine is a white turbid liquid. Description Monoclonal Antibody-purified.KP VIII 1113 Description Influenza HA Vaccine is clear liquid or a slightly whitish turbid liquid. Freeze-dried Human Blood Coagulation Factor VIII:C is purified from von Willebrand Factor (VWF) by a monoclonal antibody. Leptospira Vaccine conforms to the requirements of Leptospira Vaccine in the Specifications of Biological Products of Korea. Typhoid Vaccine Typhoid Vaccine is a liquid for injection containing inactivated typhoid bacilli (Salmonella typhosa). Live Oral Poliomyelitis Vaccine Live Oral Poliomyelitis Vaccine contains live attenuated poliovirus of types 1. colorless liquid. add 3 mL of ammonium chloride TS and 1 mL of ammonia TS: a white. Each mL of 0. Add Methyl Parahydrxybenzoate or Ethyl Parahydrxybenzoate and Propyl Parahydroxybenzoate or Butyl Parahydroxybenzoate to Purified Water. Boil for 5 minutes. mix to make emulsion. add 30. Sorbitan Sesquioleate. Perform a blank determination and make any necessary correction. evaporate on a water-bath to dryness and dissolve the residue in 5 mL of water: the solution responds to the Qualitative Tests for potassium salt. add an excess of magnesium oxide and filter. Chlorpheniramine and Calcium Powder Chlorpheniramine and Calcium Powder contains not less than 0. Aromatic Castor Oil Method of Preparation Caster Oil 990 mL Orange Oil 5 mL Mentha Oil 5 mL ⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯ 1000 mL Mix the above ingredients. Dissolve the fused matter in 30 mL of water.33% of chlorpheniramine maleate (C16H19ClN2·C4H4O4: 390. lustrous. Acidify the filtrate with hydrochloric acid: white crystals are produced.8. White Beeswax. and Lauromacrogol by heating on a water-bath.33% of aluminum potassium sulfate [AlK(SO4)2·12H2O: 474.27% and not more than 0. Assay Pipet 50. Description Aromatic Caster Oil is a colorless or milky yellow. and stir thoroughly until it congeals. Cetanol. Method of Preparation Chlorpheniramine Maleate 3g . Description Absorptive Ointment is a white. cool. Method of Preparation Aluminum Potassium Sulfate 3g Mentha Water 50 mL Water or Purified Water a sufficient quantity ⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯ To make 1000 mL Dissolve and mix the above ingredients. viscous liquid. Identification (1) Take 5 mL of Alum Solution.02 mol/L disodium ethylene-diaminetetraacetate VS and add 20 mL of acetic acid-ammonium acetate buffer solution.0 mL of Alum Solution. Combine both solutions.1114 Monographs. and maintain at about 75 o C . pH 4. Part II 3) Compound Preparations Absorptive Ointment Method of Preparation White Petrolatum 400 g Cetanol 100 g White Beeswax 50 g Sorbitan Sesquioleate 50 g Lauromacrogol 5g Ethyl Parahydroxybenzoate or Methyl Parahydroxybenzoate 1g Butyl Parahydroxybenzoate or Propyl Parahydroxybenzoate 1g Purified Water a sufficient quantity ⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯ To make 1000 g Melt White Petroleum. and has a slightly characteristic odor. cool. dissolve by warming at 80 o C . gelatinous precipitate is produced.0 mL of 0. add 55 mL of ethanol and titrate with 0. add 1 g of potassium hydroxide and heat the mixture carefully to fuse: a characteristic odor is perceptible. Alum Solution has a mentha oil-like odor and an astringent taste. Alum Solution Alum Solution contains not less than 0. Identification Take 3 g Aromatic Caster Oil. Packaging and Storage Preserve in tight containers.27% and not more than 0.39]. (2) Place 100 mL of Alum Solution in an evaporating dish. Description Alum Solution is a clear. which changes to red upon the addition of 5 drop of alizarin S TS (Aluminum sulfate). has aromatic odor. colorless liquid.86).488 mg of AlK(SO4)2·12H2O Packaging and Storage Preserve in tight containers. clear. mix. Packaging and Storage Preserve in tight containers. (3) Alum Solution responds to the Qualitative Tests (1) and (2) for sulfate.02 mol/L zinc acetate VS (indicator: 2 mL of dithizone TS) until the color of the solution changes from light dark green to pale red.02 mol/L disodium ethylenediaminetetraacetate VS = 9. add 30 mL of ether.11). add 20 mL of 0. methanol. using 0. add 58 mL of 0. viscous liquid. Extract twice with 50 mL vo- lumes of ether. add 5 mL of methanol.KP VIII 1115 Dibasic Calcium Phosphate 800 g Starch.3w/v% of total iodine (as I) and not less than 0. filter and use the filtrate as the test solution. add 0. of the test solution and the standard solution at 265 nm.05 mol/L sulfuric acid. shake well and filter: the filtrate responds to the Qualitative Tests (2) for phospahte.3w/v % of iodine (I: 126.1w/v% and not more than 1. not less than 2. shake and allow to stand for 5 minutes. dissolve about 75 mg of Chlorpheniramine Maleate RS. mixing thoroughly. dissolve 10 mg of chlorpheniramine maleate in 17 mL of methanol and use this solution as the standard solution. Spot 10 µL each of the test solution and the standard solution on the plate of silica gel with fluorescent indicator for Thin-Layer chromatography. Compound Iodine Glycerin Compound Iodine Glycerin contains not less than 1. (3) Take 0.00). (2) Take 0.25 mol/L sulfuric acid VS.2w/v% and not more than 2. Spray evenly Dragendorff's TS for spraying on the plate: the spot from the standard solution and the corresponding spot from the test solution reveal an orange color. Air-dry the plate and examine under ultraviolet light (main wavelength: 254 nm): the spots form the test solution and the standard solution show the same Rf value. Amount (mg) of Chlorpheniramine Maleate (C16H19ClN2·C4H4O4) = amount (mg) of A 1 Chlorpheniramine Maleate RS × T × AS 50 Packaging and Storage Preserve in well-closed containers.05 mol/L sulfuric acid VS.43w/v% and not more than 0. Separately.5 g of Chlorpheniramine and Calcium Powder. shake for 5 minutes. as directed in the Ultraviolet-visible Spectrophotometry. AT and AS . transfer to a 30-mL glassstoppered centrifuge tube. Liquefied Phenol and add sufficient Purified Water to make 1000 mL. 20 mL and 5 mL volumes of 0. add Mentha Water. Determine the absorbances. Identification (1) Determine the absorption spectrum of the test solution obtained in the Assay as directed under the Ultraviolet-visible Spectrophotometry: it exhibits a maximum between 263 nm and 267 nm (chlorpheniramine maleate).6w/v% of potassium iodide (KI: 166. centrifuge and collect the supernatant liquid.23. Add 20 mL of 0.53w/v% of phenol (C6H6O : 94.05 mol/L sulfuric acid VS. wash with 20 mL of water and extract the ether layer with 20 mL.25 mol/L sulfuric acid VS to make exactly 50 mL and use this solution as the test solution. not less than 2. Pipet 2. . shake well and filter: the filtrate responds to the Qualitative Tests (3) for calcium salt. (4) Take 1 g of Chlorpheniramine and Calcium Powder.05 mol/L sulfuric acid VS and 30 mL of ether and shake. Method of Preparation Iodine 12 g Potassium Iodide 24 g Glycerin 900 mL Mentha Water 45 mL Liquefied Phenol 5 mL Purified Water a sufficient quantity ⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯ To make 1000 mL Dissolve Potassium Iodide and Iodine in about 25 mL of Purified Water. has a characteristic odor. 20 Specific gravity⎯ d 20 : About 1. Develop the plate with a mixture of chloroform. Extract the ether layer twice with 10 mL volumes of 0.5 g of Chlorpheniramine and Calcium Powder.0 mL of the solution into a 200 mL separatory funnel. combine the ether layer. Transfer all the supernatant liquid to a 200 mL separatory funnel. respectively. Description Chlorpheniramine and Calcium Powder is white. add 10 mL of dilute hydrochloric acid.25 mol/L sulfuric acid VS as the blank. Filter the water layer through dry filter paper into another separatory funnel.05 mol/L sulfuric acid VS to make exactly 100 mL. shake well. combine the washing with the water layer in the preceding separatory funnel and add 10 mL of ammonia TS. previously dried at 105 °C for 3 hours and accurately weighed.05 mol/L sulfuric acid VS and add 0. Assay Weigh accurately about 0. filter the extracts into the preceding separatory funnel containing the water layer. Proceed in the same manner as the test solution and use the solution as the standard solution.7w/v% and not more than 3. It may be prepared with an appropriate quantity of Concentrated Glycerin and Purified Water in place of Glycerin. Lactose.5 g of Cholrpheniramine and Calcium Powder. Description Compound Iodine Glycerin is red-brown. Separately. in 10 mL of 0. After adding Glycerin.05 mol/L sulfuric acid VS to the residue and proceed twice in the same manner mentioned above.90). add 10 mL of dilute nitric acid. or their mixture a sufficient quantity ⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯ To make 1000 g Prepare as directed under Powders. Combine all the extracts. Perform the test with the test solution and the standard solution as directed under the Thin-layer Chromatography. acetone and strong ammonia (73 : 15 : 10 : 2) to a distance of about 10 cm. Wash the filter paper with 5 mL of 0. with the above ingredients. weigh accurately about 80 mg of Iodine RS and about 0. for the test solution and the standard solution. AT and AS . accurately weighed. Pipet exactly 3 mL each of the test solution and the standard solution into 50-mL separatory funnel. previously dried at 105 o C for 4 hours. 1 mL of diluted dilute hydrochlorlc acid (1 in 2). Separately. mix with shaking. pipet exactly 10 mL of each of the water layers and to each. add water to make exactly 50 mL and use this solution as the test solution. Amount (mg) of iodine (KI) = amount (mg) of Potassium Iodine RS × AT AS (3) Total iodine—Measure the specific gravity of Compound Iodine Glycerin according to Method 2 under Specific Gravity and Density. Amount (mg) of total iodine (I) A = amount (mg) of Potassium Iodine RS × T × 0. at 512 nm as directed under the Ultravioletvisible Spectrophotometry. Separate the chloroform-hexane layers and filter through absorbent cotton. Amount (mg) of iodine (I) = amount (mg) of Iodine RS × AT AS (2) Potassium iodide—Separate the water layers of the test solution and the standard solution obtained in (1).5 mol/L sodium hydroxide TS.7644 AS (4) Phenol—Measure the specific gravity of Compound Iodine Glycerin according to Method 2 under Specific Gravity and Density. proceed in the same manner as the test solution and use this solution as the standard solution. add 10 mL of ethanol and mix. separate the chloroform-hexane layers [use the water layers in (2)] and filter through absorbent cotton. Determine the absorption spectrum of this solution as directed under the Ultraviolet-visible Spectrophotometry: it exhibits maxima between 510 nm and 514 nm (potassium iodide). Combine all of the chloroform extract and extract twice with 10 mL of 0. previously dried at 105 o C for 4 hours. Then add 2 mL of sodium hydroxide TS.1116 Monographs. equivalent to about 2 mL of Compound Iodine Glycerin. pipet exactly 2 mL of this solution.2 g of Potassium Iodide RS. Determine the absorbances of the filtrates. in ethanol to make exactly 100 mL.1 mol/L sodium thiosulfate VS. extract twice with 10 mL volumes of chloroform. respectively. add 1 mL of a solution of cupric chloride in ethanol (1 in 10) and shake: a blue color is observed (glycerin). Weigh accurately an amount. shake until the color of iodine disappears and heat under a reflux condenser on a water-bath for 30 minutes. respectively. Pipet exactly 4 mL each of the test solution and the standard solution into 30-mL separatory funnel and to each add 5 mL of water. 1 mL of sodium nitrite TS and 10 mL of a mixture of chloroform and hexane (2 : 1) shake well immediately and proceed as directed in (2). Determine the absorption spectrum of this solution as directed under the Ultraviolet-visible Spectrophotometry : it exhibits a maximum between 510 nm and 514 nm (iodine). Wash the flask twice with 10 mL volumes of warm water and combine the filtrate and the washings. After cooing. Separately. AT and AS . using a mixture of chloroform and hexane (2 : 1) as the blank. Combine all of the water extracts. equivalent to about 5 mL of Compound Iodine Glycerin and add water to make exactly 50 mL.17 g of Potassium Iodide RS. Pipet exactly 5 mL of this solution. add 3 mL of 0. dissolve in water to make exactly 50 mL. (2) The colored solution obtained in the Assay (2) has a red color. Allow to stand for 10 minutes and add exactly 2 mL of a solution of sodium nitrite (1 in 100). to each add exactly 10 mL of a mixture of chloroform and hexane (2 : 1) and exactly 15 mL of water successively and shake immediately and vigorously. Weigh accurately an amount.5 g of Phenol RS. add 1 mL of diluted dilute hydrochloric acid (1 in 2). dissolve about 0. for the test solution and the standard solution. add water to make exactly 500 mL and use this solution as the test solution. Assay (1) Iodine⎯Measure the specific gravity of Compound iodine Glycerin according to Method 2. Separately. Weigh accurately an amount. to each add 2 mL of dilute hydrochloric acid and place in a water-bath at 30 o C . at 512 nm as directed under the Ultraviolet-visible Spectrophotometry. Part II Identification (1) The colored solution obtained in the Assay (1) has a red color. shake and allow . add 0.5 g of zinc powder and 5 mL of glacial acetic acid. using a mixture of chloroform and hexane (2 : 1) as the blank. Determine the absorption spectrum of this solution as directed under the Ultraviolet-visible Spectrophotometry: it exhibits maxima between 401 nm and 405 nm (phenol). add ethanol to make exactly 200 mL and use this solution as the test solution. Pipet exactly 5 mL of this solution into a 50-mL flask. (3) The colored solution obtained in the Assay (4) has a yellow color. Wash the condenser with 10 mL of hot water and filter through a glass filter (G3). add 2 mL of dilute hydrochloric acids. Determine the absorbances. Pipet exactly 3 mL each of the test solution and the standard solution. (4) Take 1 mL of Compound Iodine Glycerin in a glass-stoppered test tube. add 5 mL of glacial acetic acid and water to make exactly 50 mL and use this solution as the standard solution. dissolve in ethanol to make exactly 200 mL and use this solution as the standard solution. 1 mL of sodium nitrite TS and 10 mL of a mixture of chloroform and hexane (2 : 1) and shake immediately and vigorously. equivalent to about 7 mL of Compound iodine Glycerin. weigh accurately about 0. 0 mL of the internal standard solution and diluted methanol (1 in 2) to make 100 mL and use this solution as the standard solution. and has characteristic odor.0 mL of the internal standard solution. add cautiously 5 mL of sulfuric acid: the color of the solution changes to yellow-red with evolution of gas (thianthol). Develop the plate with a mixture of chloroform. of the test solution and the standard solution. respectively. Examine under ultraviolet light (main wavelength: 254 nm): three spots obtained from the test solution and the corresponding spots of standard solutions (1). Dissolve 10 mg each of salicylic acid. To 0. Filter. pH 2. (3) Wash the upper phase obtained in (2) with 10 mL of sodium bicarbonate TS and extract with 10 mL of dilute sodium hydroxide TS. add 10. Method of Preparation Thianthol 200 mL Salicylic Acid 20 g Phenol 20 g Olive Oil 50 mL Ether 100 mL Petroleum Benzin a sufficient quantity ⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯ To make 1000 mL Dissolve salicylic acid and phenol in ether. perform the test as directed under the Liquid Chromatography according to the following operating conditions and calculate the rations. Spot 5 μL each of the test solution and the standard solutions (1). Add dilute potassium hydroxide·ethanol TS to make exactly 25 mL. at 403 nm as directed under Ultraviolet-visible Spectrophotometry. Determine the absorbances. (2) Take 10 mL of Compound Thianthol and Salicylic Acid Solution. discard the first 10 mL of the filtrate and use the subsequent filtrate as the test solution. phenol and thianthol in 5 mL each of ethanol and use each solution as standard solutions (1). of the peak area of salicylic acid and phenol.KP VIII 1117 to stand at 30 o C for 60 minutes. previously dried in a desiccator (silica gel) for 3 hours and about 0. QTa and QTb . add 10 mL of sodium bicarbonate TS and separate the water layer. Description Compound Thianthol and Salicylic Acid Solution is pale yellow liquid. of the peak area of salicylic acid and phenol to that of the internal standard for the test solution and the ratios. AT 1 × AS 50 Preserve in light-resistant. add hydrochloric acid-potassium chloride buffer solution.8% and not more than 2. Spray evenly ferric chloride TS on the plate: the spot from standard solution (1) and the corresponding spot from the test solution reveal a purple color . (2) and (3) on a plate of silica gel with fluorescent indicator for thin-layer chromatography. acetone and glacial acetic acid (45 : 5 : 1) to a distance of about 10 cm and air-dry the plate. mix well and add diluted methanol (1 in 2) to make 100 mL. (2) and (3). then add 70 mL of diluted methanol (1 in 2). (2) and (3) show the same Rf value. Assay Measure 2. add 5 mL of a solution of ferric nitrate (1 in 200): a red-purple color is produced (salicylic acid). Amount (mg) of salicylic acid (C7H6O3) Q 1 = amount (mg) of Salicylic Acid RS × Ta × QSa 5 Amount (mg) of phenol (C6H6O) Q 1 = amount (mg) of Phenol RS × Tb × QSb 5 Internal standard solution⎯A solution of theophy- .0 mL of this solution.11). Identification (1) Place 1 mL of Compound Thianthol and Salicylic Acid Solution to a porcelain dish and evaporate on a water-bath to dryness. Compound Thianthol and Salicylic Acid Solution Compound Thianthol and Salicylic Acid Solution contains not less than 1.8% and not more than 2.5 mL of the water layer. With 5 μL each of the test solution and the standard solution.12) and not less than 1. QSa and QSb .2 g of Salicylic Acid RS.2% of Phenol (C6H6O : 94. mix with shaking and use this solution as the test solution.2 g of Phenol RS. Pipet 10. to that of the internal standard in the standard solution. Amount (mg) of phenol (C6H6O) = amount (mg) of Phenol RS × Packaging and Storage tight containers. (4) Take 1 mL of Compound Thianthol and Salicylic Acid Solution add 10 mL of ethanol. AT and AS . add 1 mL of sodium nitrate TS and 1 mL of dilute hydrochloric acid. To 1 mL of the extract.0. To the residue. mix and dissolve to make 1000 mL. to make 50 mL and to 5 mL of this solution. Perform the test with the test solution and the standard solutions as directed under the Thin-layer Chromatography.2% of Salicylic Acid (C7H6O3: 138. mix with shaking and add 3 mL of sodium hydroxide TS: a yellow color is observed (phenol). dissolve in diluted methanol (1 in 2) to make exactly 50 mL. olive oil and petroleum benzene to this solution. add thianthol. Weigh accurately about 0. using the solution prepared in the same manner with 3 mL of water instead of the test solution as the blank.0 mL of Compound Thianthol and Salicylic Acid Solution. add 10. respectively. anhydrous zinc sulfate and Zinc Oxide and a solution containing Cresol. add 20 mL of ether and 20 mL of 0. 0. To 10 mL of this solution. dissolve 10 mg of procaine hydrochloride in 5 mL of water and use this solution as standard solution. Dental Triozinc Paste Dental Triozinc Paste consists of a powder containing Paraformaldehyde. 2 g of potassium iodide and 10 mL of acetic acid and titrate the liberated iodine with 0. add 10 mL of acetylacetone TS and heat on a water-bath for 10 minutes: a yellow color is observed (paraformaldehyde).15 g of Dental Paraformaldehyde Paste. Separately. Method of Preparation (1) The powder Paraformaldehyde.2 g of benzoic acid. Operation Conditions Detector: An ultraviolet absorption photometer (wavelength: 270 nm). tight containers.1118 Monographs. Description Dental Antiformin is a clear. Suitable amounts of the two components are triturated before use. Examine under ultraviolet light (main wavelength: 254 nm): spots form the test solution and the standard solution show the same Rf value.0 and methanol (3 : 1). not exceeding 10 °C. Spot 5 µL each of the test solution and the standard solution on a plate of silica gel with fluorescent indicator for thin-layer chromatography. Mobile phase: A mixture of 0.0% and not more than 6. (2) Add dilute hydrochloric acid to Dental Antiformin: it evolves the odor of chlorine and the gas changes potassium iodide starch paper moistened with water to blue. add 25 mL of ether and 25 mL of water. Identification (1) Take 0. with the above ingredients. tight containers. dehydrated ethanol and strong ammonia water (50 : 5 : 1) to a distance of about 10 cm and air-dry the plate. separate the water layer and add water to make 100 mL. shake well. System performance: Dissolve 0. shake well and separate the water layer: the solution responds to the Qualitative Tests for primary aromatic amines (procaine hydrochloride). Dental Antiformin gradually changes by light. finely powdered 10 g . (2) Take the ether layer obtained in (1).1 mol/L phosphate buffer solution. Dental Antiformin Dental Antiformin contains not less than 3.2 g of salicylic acid and 50 mg of theophylline in 100 mL of diluted methanol (1 in 2). filter and use the filtrate as the test solution.15 g of Dental Paraformaldehyde Paste. Column: A stainless steel column.7221 mg of NaClO Packaging and Storage Preserve in light-resistant. shake. (3) Dental Antiformin responds to the Qualitative Tests (1) for sodium salt. Dental Paraformaldehyde Paste Method of Preparation Paraformaldehyde. Column temperature: A Room temperature. add 90 mL of diluted methanol (1 in 2). Identification (1) Dental Antiformin changes red litmus paper to blue and then decolorizes it. has characteristic odor.1mol/L sodium thiosulfate VS = 3. Perform the test with the test solution and the standard solution as directed under the Thinlayer Chromatography.1 mol/L sodium thiosulfate VS (indicator: 3 mL of starch TS) Each mL of 0. not exceeding 25 o C . pH 7.0% of sodium hydrochloride (NaClO: 74. finely powdered 35 g Hydrous Lanolin a sufficient quantity ⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯ To make 100g Prepare as directed under Ointments. packed with octadecylsilanized silica get for liquid chromatography (5 µm in particle diameter). To 1 mL of this solution. Description Dental Paraformaldehyde Paste is yellowish white. about 4 mm in inside diameter and 25 cm to 30 cm in length. Develop the plate with a mixture of ethyl acetate.0 mL of Dental Antiformin in an iodine flask. slightly pale yellowish green liquid and has slight odor of chlorine. Packaging and Storage Preserve in tight containers. salicylic acid and theophylline are eluted in this order and clearly dividing each peak. add 50 mL of water. Flow rate: Adjust the flow rate so that the retention time of salicylic acid is about 6 minutes. Assay Pipet 3. When the procedure is run with 10 µL of this solution under the above operating conditions: benzoic acid. finely powdered 35 g Procaine Hydrochloride. Part II line in methanol (1 in 1000). Potash Soap and Glycerin. (3) Take 0.44). Packaging and Storage Preserve in light-resistant.5 mol/L sodium hydroxide TS. Thymol. separate the water layer. add 5 mL of dilute hydrochloric acid and 20 mL of water. 03). Pipet 4. Add hot purified water or evaporate to make 100 g of solution. add water to make 250 mL of solution.KP VIII 1119 Thymol. Stand for 15 minutes after adding 1. Epinephrine Solution turns to pale red and brown due to air or light. previously heat at 100 °C and heat for 15 minutes to make a complete solution. Paraformaldehyde and Zinc Oxide. colorless liquid and has slight odor of formaldehyde. colorless or pale reddish solution.05 mol/L iodine VS = 1. Mix 3. Description Formalin Water is clear. white powder and has characteristic odor. Formalin Water is almost neutral.1 mol/L sodium hydroxide VS. Assay Dissolve Glycerin Suppositories equivalent to 8 g of glycerin in 50 mL of water. Glycerin Suppositories Glycerin Suppositories contain not less than 66. stand for 5 minutes and titrate with 0. Method of Preparation Gelatin 14 g Glycerin 25 g Purified water a suitable quantity Dissolve gelatin in 30 mL of hot purified water. finely powdered 3g Zinc Sulfate 9g Zinc Oxide 82 g ⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯ 100 g Heat Zinc Sulfate. Epinephrine Solution Epinephrine Hydrochloride Solution Epirenamine Hydrochloride Solution Adrenaline Hydrochloride Solution Epinephrine Solution contains not less than 0.5 g Diluted hydrochloric acid (9 in 100) 10 mL Preservative a suitable amount Stabilizer a suitable amount Purified Water sufficient quantity ⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯ To make 1000 mL Description Epinephrine Solution is a clear. then add 0. make Glycerin Suppositories by pouring hot solution into the suppository mold and cool.5 mL of 1 mol/L sodium hydroxide VS and add water to make 100 mL.1 mol/L sodium hydroxide TS. cool and pulverize to a fine powder.5% and not more than 73. viscous liquid and has the odor of cresol.3 and 5. Mix homogeneously this powder with Thymol. add 150 mL of water.5013 mg of CH2O Packaging and Storage Preserve in tight containers.0. . Description The powder of Dental Triozinc Paste is fine. yellow-brown to red-brown. pH⎯Between 2. Packaging and Storage tight containers.1 w/v% of formaldehyde (CH2O: 30.6 g of sodium periodate. Assay Proceed as directed in the Assay under Epinephrine Injection.115% of epinephrine (C9 H13NO3: 183. Assay Transfer exactly 20 mL Formalin Water to a 100-mL volumetric flask containing 2. add hot glycerin. Identification Proceed as directed in the Identification under Epinephrine Injection.20). Pipet exactly 10 mL of this solution and proceed as directed in the Assay under Formalin.0 mL of isopropanol with this solution. (2) The solution Cresol 40 g Potash Soap 40 g Glycerin 20 g ⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯ 100 g Dissolve Potash Soap in a mixture of Cresol and Glycerin. Packaging and Storage Preserve in tight containers. Method of Preparation Formalin 30 mL Water of Purified Water a sufficient quantity ⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯ To make 1000 mL Prepare by mixing the above ingredients. Method of Preparation Epinephrine 1g Sodium Hydroxide 8.25 mL of bromcresolpurple TS which was neutralized with 0.0 mL of this solution. at about 250 o C to obtain anhydrous zinc sulfate. Each mL of 0. previously. The solution of Dental Triozinc Paste is clear.5% of Glycerin (C3H8O3).9 w/v% and not more than 1.085% and not more than 0. Preserve in light-resistant Formalin Water Formalin Water contains not less than 0. Mix with a glass rod. Immerse the lower outlet of the condenser in the receiver containing exactly 30 mL of 0. distil slowly collect about 50 mL of the distillate and titrate the excess sulfuric acid with 0. Hydrophilic Petrolatum retains the consistency of ointment. Place in a refrigerator to cause the upper layer to congeal. has sweet. Hydrophilic Petrolatum Method and preparation White Beeswax 80 g Stearly Alcohol or Cetanol 30 g Cholesterol 30 g White Petrolatum A sufficient quantity ⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯ To make 1000 g Melt and mix Stearyl Alcohol or Cetanol. dissolve in purified water and warm to about 75 o C .25 mol/L sulfuric acid. stir and keep temperature of the mixture at about 75 o C .1 mol/L sodium hydroxide VS = 9. acid taste. Stop warming and stir until the mixture congeals. Packaging and Storage Preserve in tight containers Hydrophilic Ointment Method of Preparation White Petrolatum 250 g Stearyl Alcohol 200 g Propylene Glycol 120 g Polyoxyethylene hydrogenated castor oil 60 40 g Glycerin Monostrateae 10 g Methyl Parahydroxybenzoate 1g Propyl Parahydroxybenzoate 1g Purified water a sufficient quantity ⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯ To make 1000 g Melt White Petrolatum. Pipet exactly 100 mL of this solution in a flask. cool. Packaging and Storage Preserve in tight containers.25% of ammonia (NH3: 17. stir to form emulsion. has slight. Description Hydrochloric Acid Lemonade is clear. add 3 g of paraffin and 20 mL of sodium hydroxide solution (4 in 20) and connect a condenser. cover with a watch glass and allow to stand for 15 to 20 minutes. Packaging and Storage Preserve in tight containers. if necessary. characteristic odor. Method of Preparation Ichthammol 100g Purified Lanolin 100g Petrolatum 800g ⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯ Total amount 1000g Thoroughly incorporate the Ichthammol with the Purified Lanolin and combine this mixture with the Petrolatum. with frequent agitation for 10 minutes.1120 Monographs. Repeat the extraction several times in the same manner until the aqueous extract is practically colorless. Assay Transfer an accurately weighed volume of Ichthammol Ointment. cool and stir thoroughly until it congeals.210 mg C3H8O3 Packaging and Storage Preserve in tight containers. with the above ingredients. melt by warming. filter with an absorbent cotton. polyoxyethylene hydrogenated castor oil 60 and Glycerin Monostearate by heating on a water-bath. colorless liquid. to a 250-mL of beaker and add 70 mL of boiling water. add Methyl Parahydroxybenzoate and Propyl Parahydroxybenzoate. White Beeswax and White Petrolatum on a water-bath. Hydrochloric Acid Lemonade Method of Preparation Dilute hydrochloric acid 5 mL Simple syrup 80 mL Purified water a sufficient quantity ⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯ To make 1000 mL Prepare before use as directed under Lemonade. Add this solution to the above mixture. To Propylene Glycol.5 mol/L sodium hydroxide VS (indicator: methylet red TS). Ichthammol Ointment Ichthammol Ointment contains an amount of Ichthammol equivalent to not less than 0. Description Hydrophilic Petrolatum is white. When mixed with an equal volume of water. Perform a blank determination. Part II Each ml of 0. characteristic odor. equivalent to 10 g of Ichthammol. .03). heat on a water-bath. has slight. Combine all the filtrates and add water to make 500 mL. Add Cholesterol and melt completely by stirring. Stearyl Alcohol. Description Hydrophilic Ointment is white. 05 mol/L potassium iodate VS used as above and the volume ( b mL) of 0.2w/v% of potassium iodide (KI: 166. Perform the pretreatment (ii) in the Method 1.5 g of potassium iodide. allow the mixture to stand for 5 minutes. Amount (mg) of potassium iodide (KI) b 2 Iodine Tincture = 16 .90). Identification (1) Take a mixture of 1 mL of starch TS and 9 mL of water and add 1 drop of Dilute Iodine Tincture: a dark blue-purple color develops. and not less than 1.KP VIII 1121 Each mL of 0.690 mg of I .2w/v % of iodine (I: 126. Each mL of 0. Description Dilute Iodine Tincture is dark red-brown liquid. and add 1 drop of Iodine Tincture: a dark blue-purple color develops.600 × ( a − ) Iodine Tincture contains not less than 5.05 mol/L potassium iodate VS.7 (Method 2). the mixture should be Assay (1) Iodine—Pipet exactly 10 mL of Dilute Iodine Tincture. It may be prepared with an appropriate quantity of Ethanol or a mixture of Ethanol for Disinfection and Purified Water in place of 70vol% ethanol. It may also be prepared by adding 70% ethanol to 500 mL of iodine tincture to make 1000 mL.00). titrated further with 0. Dilute Iodine Tincture Dilute Iodine Tincture contains not less than 2. If the color reappears.690 mg of I Alcohol Number Not less than 6. with agitating the mixture vigorously and continuously. with the above ingredients. Packaging and Storage Preserve in tight containers. add 20 mL of water. Alcohol Number Not less than 6.1 mol/L sodium thiosulfate VS used in the titration under the Assay (1). It may be prepared with an appropriate quantity of Ethanol or a mixture of Ethanol for Disinfection and Purified Water in place of 70% ethanol.25 mol/L sulfuric acid VS = 8. add 0. 20 Specific gravity⎯ d 20 : About 0. 20 Specific gravity⎯ d 20 : About 0. Perform the pretreatment (ii) in the Method 1 (2) Potassium iodide—Pipet exactly 5 mL of Iodine Tincture into an iodine flask. 20 mL of water and 1 mL of dilute hydrochloric acid and titrate with 0. Method of Preparation Iodine 30 g Potassium Iodide 20 g 70vol% Ethanol a sufficient quantity ⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯ To make 1000 mL Prepare as directed under Medicated Spirits.3w/v% of Iodine (I: 126. Identificatien (1) Take a mixture of 1 mL of starch TS and 9 mL of water.515 mg NH3 Packaging and Storage Preserve in tight containers and store under 30 o C . Calculate the amount (mg) of potassium iodide from the volume ( a mL) of 0. add 0.1 mol/L sodium thiosulfate VS = 12. 20 mL of water and 1 mL of dilute hydrochloric acid and titrate with 0.05 mol/L potassium iodate VS until the red-purple color disappears from the chloroform layer. (2) Evaporate 3 mL of Iodine Tincture to dryness on a water-bath and heat gently over a free flame: a white residue is produced which responds to the Qualitative Tests for potassium salt and iodide.9w/v% and not more than 2.1w/v% of potassium iodide (KI: 166.1 mol/L sodium thiosulfate VS (indicator: 2 mL of starch TS).00).8w/v% and not more than 4.6 (Method 2). (2) Evaporate 3 mL of Diluted Iodine Tincture to dryness on a water-bath and heat gently over a free flame: a white residue is produced which responds to the Qualitative Tests for potassium salt and iodide Each mL of 0. Description Iodine Tincture is dark red-brown liquid and has characteristic odor.7w/v% and not more than 6.1 mol/L sodium thiosulfate VS (indicator: 2 mL of starch TS). Cool to room temperature and titrate with 0. After the chloroform layer has been decolorized.5 g of potassium iodide.1 mol/L sodium thiosulfate VS = 12. Method of Preparation Iodine 60 g Potassium Iodide 40 g 70% ethanol a sufficient quantity ⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯ To make 1000 mL Prepare as directed under Tinctures. Assay (1) Iodine—Pipet exactly 5 mL of iodine Tincture. Dilute Iodine Tincture has characteristic odor.93.97. 50 mL of hydrochloric acid and 5 mL of chloroform.90) and not less than 3.8w/v% and not more than 3. with the above in gradients. If the color reappears. 50 mL of hydrochloric acid and 5 mL of chloroform. Amount (mg) of iodine (I) . extract with 10 mL of ether and use the ether extract as the test solution. Develop the plate with a mixture of chloroform. shake and separate the chloroform-hexane layers [use the water layers in (2)]. mix with shaking and add 3 mL of sodium hydroxide TS: a yellow color develops (phenol). Salicylic Acid and Phenol Spirit is dark red-brown liquid.0. (3) Take 1 mL of Iodine. using a mixture of chloroform and hexane (2 : 1) as the blank and make any necessary correction. Description Iodine.12). (2) and (3) as directed under the Thin-layer Chromatography. with the above ingredients. the mixture should be titrated further with 0.88w/v% of potassium iodide (Kl: 166. Filter through absorbent cotton and determine the absorbances. (2) and (3).12) Method of Preparation Iodine Tincture 200 mL Salicylic Acid 50g Phenol 20g Benzoid Acid 80g Ethanol for Disinfection a sufficent quantity ⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯ To make 1000 mL Prepare as directed under Medicated Spirits. Salicylic Acid and Phenol Spirit. add ethanol to make exactly 50 ml and use this solution as the test solution.2 g of Iodine RS and about 0. Identification (1) Take a mixture of 1 mL of starch TS and 9 mL of water and add 1 drop of Iodine.00). Salicylic Acid and Phenol Spirit. Calculate the amount (mg) of potassium iodide from the volume ( a mL) of 0. not less than 1. weigh accurately about 1. respectively. add 20 mL of water and 5 mL of dilute hydrochloric acid. add 20 mL of water and 5 mL of dilute hydrochloric acid and extract with 25 mL of ether. Amount (mg) of potassium iodide (KI) = 16 . add 1 mL of sodium thiosulfate TS. acetone and glacial acetic acid (45 : 5 : 1) to a distance of about 10 cm and airdry the plate. AT and AS .2w/v% of phenol (C6H6O: 94.1122 Monographs. Part II (2) Potassiun iodide—Pipet exactly 10 mL of Dilute Iodine Tincture into an iodine flask. add 1 mL of sodium nitrite TS and 1 mL of dilute hydrochloric acid. mix with shaking. add 5 mL of a solution of ferric nitrate (1 in 200): a red-purple color develops (salicylic acid). pH 2. add 20 mL of water.05 mol/L potassium iodateVS consumed as above and the volume ( b mL) of 0. To 15 mL of this solution.2w/v% and not more than 8. (4) Take 1 mL of Iodine. Salicylic Acid and Phenol Spirit.90).600 × ( a − b ) 2 Packaging and Storage Preserve in tight containers. and has an odor of phenol. Iodine.32w/v% of iodine (I: 126.8w/v% and not more than 2. Perform the test with the test solution and the standard solutions (1). Salicylic Acid and Phenol Spirit Iodine. (2) Take 1 mL of iodine.5w/v% of salicylic acid (C7H6O3: 138. Further add exactly 10 mL of water.8 g of Potassium Iodide RS. not less than 4.08w/v% and not more than 1. allow the mixture to stand for 5 minutes. 10 mg of Phenol RS and 40 mg of benzoic acid RS in 5 mL each of ether. It may be prepared with an appropriate quantity of Ethanol and Purified Water in place of Ethanol for Disinfectant. previously dried at 105 o C for 4 hours and dissolve in ethanol to make exactly 100mL. Spray evenly ferric chloride TS on the plate: the spot from standard solution (1) and the corresponding spot from the test solution has a purple color Assay (1) Iodine—Pipet exactly 4 mL of Iodine. After the chloroform layer has been decolorized. dissolve 25 mg of Salicylic Acid RS. add hydrochloric acidpotassium chloride buffer solution. Salicylic Acid and Phenol Spirit contains not less than 1. at 512 nm as directed under the Ultraviolet-visible Spectrophotometry. Separately. add ethanol to make exactly 50 mL and use this solution as the standard solution. (2) and (3) on a plate of silica gel with fluorescent indicator for thin-layer chromatography. to each add exactly 25 mL of a mixture of chloroform and hexane (2 : 1) and shake. Pipet exactly 4 mL of this solution. Examine under ultraviolet light (main wavelength: 254 nm): the 3 spots from the test solution show the same Rf value as the corresponding spots of the standard solutions (1). Salicylic Acid and Phenol Spirit. add 1 mL of sodium thiosulfate TS. respectively and use these solutions as the standard solutions (1). Separately.72w/v% and not more than 0. of the filtrates from the test solution and the standard solution. Pipet exactly 3 mL each of the test solution and the standard solution. Cool to room temperature and titrate with 0. (2) and (3). Spot 5 µL of each the test solution and the standard solutions (1).1 mol/L sodium thiosulfate VS consumed in the titration under the Assay (1). not less than 0. Salicylic Acid and Phenol Spirit: a dark blue-purple color develops (iodine). Wash the ether extract twice with 25 mL volumes of sodium bicarbonate TS and extract with 10 mL of dilute sodium hydroxide TS. mix with shaking.5w/v% and not more than 5.05 mol/L potassium iodate VS. To 1 mL of the extract.11) and not less than 7. to make 50 mL. add 5 mL of ethanol and water to make 50 mL.05 mol/L potassium iodate VS until the red-purple color in the chloroform layer disappears while agitating vigorously and continuously. To 1 mL of this solution.8w/v% of benzoic acid (C7H6O2: 122. 2 g of salicylic acid and 50 mg of theophylline in 100 mL of dilute methanol (1 in 20). Proceed with 10 μL of this solution under the above operating conditions: Use a column giving elution of benzoic acid. To 10 mL of this solution. Column: A stainless steel column. dissolve in diluted methanol (1 in 2) to make exactly 50 mL. Amount (mg) of salicylic acid (C7H6O3) Q 1 = amount (mg) of Salicylic Acid RS × Ta × QSa 2 Amount (mg) of Phenol (C6H6O) Q 1 = amount (mg) of Phenol RS × Tb × QSb 2 Amount (mg) of benzoic acid (C7H6O2) Q 1 = amount (mg) of benzoic acid RS × Tc × QSc 2 Internal standard solution—A solution of theophylline in methanol (1 in 1000). Immediately after shaking. Packaging and Storage Preserve in tight containers. about 4 mm in inside diameter and 25 cm to 30 cm in length. salicylic acid and theophylline in this order and clearly dividing each peak. phenol and benzoic acid—Pipet exactly 2 mL of Iodine.2 g of Salicylic Acid RS.KP VIII 1123 = amount (mg) of Iodine RS × AT 1 × AS 25 (2) Potassium iodide—Pipet exactly 8 mL each of the water layers of the test solution and the standard solution obtained in the Assay (1) and add 1 mL of diluted dilute hydrochloric acid (1 in 2) and 1 mL of sodium nitrite TS. Column temperature: A room temperature. Packaging and Storage tight containers Preserve in light-resistant. Pipet exactly 25 mL of this solution.033% of atropine sulfate hydrate [(C17H23NO3)2·H2SO4·H2O: 694.0) and methanol (3 : 1). Mentha Water Method of Preparation Mentha oil 2 mL Purified Water a sufficient quantity ⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯ To make 1000 mL Prepared as directed under Aromatic Waters. packed with octadecylsilanized silica gel for liquid chromatography (5 μm in particle diameter). Amount (mg) of potassium iodide (KI) A 1 = amount (mg) of Potassium Iodide RS × T × AS 25 (3) Salicylic acid. Description Mentha Water is a clear. QSc of the peak areas of salicylic acid.2 g of benzoic acid. Morphine and Atropine Injection contains not less than 0. QTa . Calculate the ratios. Separately weigh accurately about 0. Mobile phase: A mixture of 0. about 80 mg of Phenol RS and 0. add exactly 10 mL of a mixture of chloroform and hexane (2 : 1). respectively. phenol and benzoic acid. QTb and QTc .1 mol/L sodium thiosulfate VS until the color of iodine disappears. previously dried in a desiccator (silica gel) for 3 hours. previously dried in a desiccator (silica gel) for 3 hours. add 20 mL of diluted methanol (1 in 2) and 0. Flow rate: Adjust the flow rate so that the retention time of salicylic acid is about 6 minutes. phenol and benzoic acid. to those of the internal standard of the test solution and the ratios.09% of morphine hydrochloride hydrate (C17H19NO3·HCl·3H2O: 375. shake and proceed in the same manner as for the Assay (1). and has a mentha oil-like odor. Sailcylic Acid and Phenol Spirit. Operating conditions Detector: An ultraviolet absorption photometer (wavelength: 270 nm). of the peak areas of salicylic acid.91% and not more than 1.84] Method of Preparation Morphine Hydrochloride Hydrate 10 g Atropine Sulfate Hydrate 0. and colorless liquid. to those of the internal standard of the standard solution.027% and not more than 0.3 g Water for Injection a sufficient quantity . Morphine and Atropine Injection Morphine and Atropine Injection is an aqueous solution for injection. add 90 mL of dilute methanol (1 in 20).1 mol/L phosphate buffer (pH 7. add exactly 20 mL of the internal standard solution.32 g of benzoic acid RS. 0. Perform the test with 3 uL of the test solution and the standard solution as directed under the Liquid Chromatography according to following operating conditions. add exactly 20 mL of the internal standard solution and diluted methanol (1 in 2) to make 200 mL and use this solution as the standard solution. respectively.84) and not less than 0. then add diluted methanol (1 in 2) to make 200 mL and use this solution as the test solution. with the above ingredients. QSa and QSb . Selection of column: Dissolve 0. then add water to make 50 mL and use this solution as the test solution. add 70 mL of tetrahydrofuran and mix. Flow rate: Adjust the flow rate so that the retention time of morphine is about 10 minutes. Separately. QT and QS of the peak areas of atropine to that of the internal standard. (2) Atropine Sulfate Hydrate⎯ Pipet 2 mL of Morphine and Atropine Injection. Morphine and Atropine Injection is slowly affected by light.0 g of sodium lauryl sulfate in 500 mL of diluted phosphoric acid (1 in 1000) and adjust the pH with sodium hydroxide TS to 3. and use this solution as the test solution.1124 Monographs. conditions and calculate the ratio. add 2 mL of ammonia TS and extract with 10 mL of ether. Perform the test with 20 μL of the test solution and the standard solution as directed under the Liquid Chromatography according to the following operating Amount (mg) of atropine sulfate hydrate [(C17H23NO3)2· H2SO4·· H2O] = amount (mg) of Atropine Sulfate Hydrate RS. Assay (1) Morphine Hydrochloride Hydrate⎯Pipet 2. Separately.0. add exactly 2 mL of the internal standard solution. Develop the plate with a mixture of methanol and ammonia solution (200:3) to a distance of about 10 cm. System suitability System Performance: When the procedure is run with 20 μL of the standard solution under the above operating conditions. perform with 2 mL of this solution the same procedure as used for preparation of the test solution. and use the solution so obtained as the standard solution (1). packed with octadecylsilanized silica gel for liquid chromatography (5 μm in particle diameter). dissolve 3 mg of atropine sulfate in 10 mL of water. and use this solution as the test solution. with the above ingredients. and calculate the ratios. colorless liquid. and air-dry the plate. Description Morphine and Atropine Injection is clear. Pipet 2 mL of this solution. add exactly 2 mL of the internal standard solution. add exactly 10 mL of the internal standard solution to dissolve. the relative standard deviation of the ratios of the peak area of morpine to that of the internal standard is not more than 1. then add water to make 50 mL and use this solution as the standard solution.1679 S Identification To 2 mL of Morphine and Atropine Injection. dissolve the residue in 1 mL of dehydrated ethanol. Amount (mg) of morphine hydrochloride hydrate (C17H19NO3·HCl·3H2O) = amount (mg) of Morphine Hydrochloride Hydrate RS.5 and 5. morphine and the internal standard are eluted in this order with resolution between the two peaks being not less than 3. Mobile phase: Dissolve 1. To 240 mL of this solution.0. Filter the extract with a filter paper. and use this solution as the standard solution. Column temperature: A constant temperature of about 40 °C. pH⎯between 2. and dissolve in water to make exactly 50 mL. System repeatability: When the test is repeated 6 times with 20 μL of the standard solution under the above operating conditions. Spray evenly Dragendor’s TS on the plate: the two spots obtained from the test solution show the same color tone and the same Rf value with either spot of orange color obtained from the standard solution (1) or the standard solution (2) (morphine and atropine). It Determination of Volume of Injection in Containers It meets the requirement. Perform the test with 20 µL each of the test solution and the standard solution as directed under the Liquid Chromatography according to the following conditions. Sterility Test It meets the requirement.1 g of morphine hydrochloride in 10 mL of water.0 mL of Morphine and Atropine Injection. evaporate the filtrate on a water-bath to dryness. QT calculated on the anhydrous basis × Q × 1. Separately. Foreign Insoluble Particulate Matter Test the requirement. and use the solution so obtained as the standard solution (2). Column: A stainless steel column. about 4 mm in inside diameter and about 15 cm in length. respectively. calculated . Part II ⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯ To make 1000 mL Prepare as direction under Injections. Perform the test with these solutions as directed under the Thin-layer Chromatography. weigh accurately about 15 mg of Atropine Sulfate RS (previously determine its loss on drying). Spot 10 µL each of the test solution and standard solutions (1) and (2) on a plate of silica gel for thin-layer chromatography. perform with 2 mL of this solution the same procedure as used for preparation of the test solution. QT and QS of the peak area of morphine to that of the internal standard for the test solution and the standard solution. dissolve 0. It meets Insoluble Particulate Matter Test for Injections meets the requirement. Separately. add 10.0 mL of the internal standard solution. Internal standard solution⎯A solution of etilefrine hydrchloride (1 in 500) Operating conditions Detector: An ultraviolet absorption photometer (wavelength: 285 nm). weigh accurately about 25 mg of Morphine Hydrochloride Hydrate RS.0%. and about 0.5 g Chlorpheniramine maleate 1g Chlorobutanol 2g Glycerin 50 mL Purified water a sufficient quantity ⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯ To make 1000 mL Dissolve and mix the above ingredients. System repeatability: When the test is repeated 6 times with 20 µL of the standard solution under the above operating conditions.09% and not more than 0. dissolve the residue in 5 mL of methanol and use this solution as the test solution. distil off the solvent. (3) Take 20 mL of Naphazoline and Chlorpheriamine Solution. 2 mL of sodium hydroxide TS and 1 mL of solution of cupric chloride in ethanol (1 in 10) and shake: a blue color is observed (glycerin). dissolve in water to make exactly 100 mL. add 5 mL of sodium hydroxide TS. Assay Pipet 4. Separately.87). QSa and QSb . and the resolution between morphine and the internal standard is not less than 3. to that of the internal standard of the test solution and the ratios.0266 S Internal standard solution⎯A solution of etilefrine hydrochloride (1 in 12500). then add water to make 10 mL and use this solution as the test solution. add 4. Detector: An ultraviolet absorption photometer (wavelength: 225 nm). respectively and use these solutions as the standard solutions (1) and (2). column temperature. Pipet 4. (2) Place 10 mL of Naphazoline and Chlorpheniramine Solution in a glass-stoppered test tube. Spray evenly Dragendorff’s TS on the plate: the spots from standard solutions (1) and (2) and the corresponding spot from the test solutions reveal an orange color.1 g of Chlorpheniramine Maleate RS.0%. QTa and QTb . System suitability System performance: When the procedure is run with 20 µL of the test solution under the above operating conditions.0 mL of Naphazoline and Chlorpheniramine Solution.KP VIII 1125 1 QT on the dried basis × Q × 50 × 1. Packaging and Storage hermetic containers. Spot 5 μL each of the test solution and the standard solutions (1) and (2) on a plate of silica gel with fluorescent indicator for thin-layer chromatography.11% of chlorpheniramine maleate (C16H19ClN2·C4H4O4: 390. Method of Preparation Naphtazoline nitrate 0.045% and not more than 0.0 mL of the internal standard solution. add exactly 4 mL of the internal standard solution. add 2 mL of a solution of potassium hydroxide (7 in 10) and 5 mL of pyridine and heat at 100 o C for 5 minutes: a red color is observed (chlorobutanol).0 mL of this solution. the relative standard deviation of the ratios of the peak area of atropine to that of the internal standard is not more than 1. Operating conditions Column. morphine. acetone and strong ammonia water (73 : 15 : 10 : 2) to a distance of about 10 cm and airdry the plate. add 10 mL of ethanol. Develop the plate with a mixture of chloroform. Examine under an ultraviolet light (main wavelength: 254 nm): two spots from the test solution exhibit the same Rf value as the spots from standard solutions (1) and (2). Perform the test with 10 μL each of the test solution and the standard solution as directed under the Liquid Chromatography according to the following operating conditions and calculate the ratios. dissolve 10 mg each of Naphazoline Nitrate RS and Chlorpheniramine Maleate RS in 10 mL and 5 mL of methanol. to that of the internal standard of the standard solution.29) and not less than 0. respectively. respectively. previously dried at 105 o C for 2 hours. Description Naphazoline and Chlorpheniramine Solution is a clear and colorless liquid. extract with 10 mL of ether and separate the ether layer. the internal standard and atropine are eluted in this order. Perform the test with the test solution and the standard solutions (1) and (2) as directed under the Thin-layer Chromatography. Naphazoline and Chlorpheniramine Solution Naphazoline and Chlorpheniramine Solution contains not less than 0. Preserve in light-resistant. methanol. Flow rate: Adjust the flow rate so that the retention time of morphine is about 7 minutes. then add water to make 10 mL and use this solution as the standard solution. previously dried at 105 o C for 3 hours. of the peak height of naphazoline nitrate and chloropheniramine maleate. of the peak height of naphazoline nitrate and chlorpheniramine maleate.055% of naphazoline nitrate (C14H14N2·HNO3 : 273. and mobile phase: Proceed as directed in the operating conditions in the Assay (1). Take 5 mL of this solution. Amount (mg) of naphazoline nitrate (C14H14N2·HNO3) = amount (mg) of Naphazoline Q 1 Nitrate RS × Ta × QSa 25 Amount (mg) of chlorpheniramine maleate (C16H19CIN2·C4H4O4) = amount (mg) of . Identification (1) Take 20 mL of Naphazoline and Chlorpheniramine Solution. weigh accurately about 50 mg of Naphazoline Nitrate RS. Separately. ASa and ASb . Dissolution Perform the test with 1 tablet of Norgestrel and Ethinylestradiol Tablets at 50 revolutions per minute according to Method 2 under the Dissolution Test. Column: A stainless steel column. The dissolution rate of Norgestrel and Ethinylestradiol Tablets in 45 minutes is not less than 70%. add 6 mL of sodium hydroxide TS. elute with 3 mL of methanol and evaporate the effluent on a water-bath to dryness at about 40 o C with the aid fo a current air. Norgestrel and Ethinylestradiol Tablets Norgestrel and Ethinylestradiol Tablets contain not less than 90. evaporate to dryness on a water-bath. naphazoline nitrate and chlorpheniramine maleate are eluted in this order with complete separations among the three peaks. Column temperature: A room temperature. dissolve 10 mg of Norgestrel RS and 1 mg of Ethinylestradiol RS in 10 mL each of chloroform. shake vigorously and centrifuge. weigh the accurately about 25 mg of Norgestrel RS and about 2. Use these solutions as standard solutions (1) and (2). Weigh accurately a portion of the powder. of norgestrel and ethinylestradiol. packed with octadecylsilanized silica gel for liquid chromatography (5 μm in particle diameter). dissolve in diluted methanol (7 in 10) to make exactly 100 mL.40). Dissolve the residue in 2. transfer exactly 30 mL of the subsequent into a chromatography column [prepared by packing 0. respectively. equivalent to 10 mg of norgestrel. Method of Preparation Prepare as directed under Tablets.0% and not more than 110. Dissolution rate (%) with respect to the labeled amount of norgestrel (C21H28O2) A 1 = WSA × Ta × × 1.0% of the labeled amount of norgestrel (C21H28O2: 312. about 4 mm in inside diameter and 25 cm to 30 cm in length. respectively.8 μmol/L. Flow rate: Adjust the flow rate so that the retention time of chlorpheniramine maleate is about 10 minutes. Pipet 1 mL of chloroform layer and evaporate to dryness on a water-bath. Packaging and Storage tight containers.0 mL of the filtrate. After washing the column with 15 mL of water. To this solution add 1 mL of ice cold diazo TS. shake and cool in ice-bath.0 mL of the filtrate produced in (1). Spray ethanol solution of p-toluene sulfonic acid (1 in 5) to the plate.1126 Monographs. methanol and water (368 : 32 : 1) to a distance of about 10 cm and air-dry the plate. heat for 5 minutes at 100 o C and examine the plate under an ultraviolet light (main wavelength: 365 nm): two spots from the test solution and spots from the each standard solution show the same color and the same Rf value.8 ASa Ca . shake for 10 minutes and filter. Selection of column: Proceed with 10 μL of the standard solution under the above operating conditions and use the column from which the internal standard. add 10 mL of chloroform. Part II Chlorpheniramine Maleate RS × QTb 1 × QSb 25 Internal standard solution—A solution of ethenzamide in methanol (1 in 1000). Mobile phase: A mixture of acetonitrile and a solution of sodium laurylsulfate (1 in 500) in diluted phosphoric acid (1 in 1000) (1 : 1).5 mg of Ethinylestradiol RS. Separately. ATa and ATb . from the standard solution. Illuminate UV (main wavelength: 365 nm) to this solution: a reddish-brown fluorescence develops (norgestrel). Take 50 mL or more of the dissolved solution 45 minutes after starting the test and membrane fiber through a membrane filter with pore size of not more than 0.2 dichloroethane. Pipet 2. (3) Use the filtrate in (1) as a test solution. Separately.0 mL of this solution. using 900 mL of water as the dissolution solution. Operating conditions Detector: An ultraviolet absorption photometer (wavelength: 254 nm). add diluted methanol (7 in 10) to make exactly 100 mL and use this solution as the standard solution. Perform the test with the test solution and the standard solutions (1) and (2) as directed under the Thin-1ayer Chromatography. shake and add 1 mL of sodium hydroxide solution: a reddish-brown color is observed (ethinylestradiol).45) and ethinylestradiol (C20H24O2: 296.36 g of octadecylsilanized silica gel for pretreatment (55 μm to 105 μm in particle diameter) in a tube about 1 cm in inside diameter]. Dissolve the residue in 2 mL of ethanol and add 1 mL of sulfuric acid: a reddish-purple color develops. of norgestrel and ethinylestradiol. Identification (1) Powder Norgetrel and Ethinylestradiol Tablets. respectively. Develop the plate with a mixture of 1. from the test solution and the peak areas. Spot 20 μL each of the test solution and the standard solutions (1) and (2) on a plate of silica gel for thin-layer chromatography. then pipet 3. Discard the first 10 mL of the filtrate. (2) Pipet 1. Perform the test with 50 µL each of the test solution and the standard solution as directed under the Liquid Chromatography according to the operating conditions as directed under the Assay. respectively.0 mL of diluted methanol (7 in 10) and use this solution as the test solution. Determine the peak area. with Norgestrel and Ethinylestradiol. Preserve in light-resistant. To the residue add 1 mL of boric acid-methanol buffer solution. 0%. packed with octadecylsilanized silica gel for liquid chromatography (10 µm in particle diameter).8 ASb Cb WSA : Amount (mg) of Norgestrel RS. add 4. exactly 4 mL of the internal standard solution. Filter the supernatant liquid through a membrane filter with pore size of not more than 0. Column temperature: A constant temperature of about 25 o C . weigh accurately about 50 mg of Norgestrel RS and about 5 mg of Ethinylestradiol RS. Operating conditions Detector: Norgestrel⎯An ultraviolet absorption photemeter (wavelength: 241 nm). Packaging and Storage Preserved in tight containers. respectively. equivalent to about 1 mg of norgestrel (C21H28O2). Amount (mg) of norgestrel (C21H28O2) Q 1 = amount (mg) of Norgestrel RS × Ta × QSa 100 Amount (mg) of ethinylestradiol (C20H24O2) Q = amount (mg) of Ethinylestradiol RS × Tb × 100 QSb Internal standard solution—A solution of diphenyl in diluted methanol (7 in 10) (1 in 50000). of the peak areas of norgestrel and ethinylestradiol. Ca : Labeled amount of norgestrel (C21H28O2) in 1 tablet. Amount (mg) of norgestrel (C21H28O2) Q 1 = amount (mg) of Norgestrel RS × Ta × QSa 50 Amount (mg) of ethinylestradiol (C20H24O2) Q 1 = amount (mg) of Ethinylestradiol RS × Tb × QSb 50 Internal standard solution⎯A solution of dipheynyl in diluted methanol (7 in 10) (1 in 50000). norgestrel and the internal standard are eluted in this order with the resolution between the norgestrel peak and the internal standard peak being not less than 8. Perform the test with 20 µL each of the test solution and the standard solution as directed under the Liquid Chromatography according to the operating conditions as directed under the Assay. Perform the test with 20 µL each of the test solution and the standard solutions as directed under the Liquid Chromatography according to the following operating conditions. weigh accurately quantities of Norgestrel RS and of Ethinylestradiol RS. to the peak area of the internal standard of the standard solution.KP VIII 1127 Dissolution rate (%) with respect to the labeled amount of ethinylestradiol (C20H24O2) A 1 = WSB × Tb × × 1.0 mL each of the solutions. of the peak areas of the norgestrel and ethinylestradiol. Separately. QTa and QTb . shake for 20 minutes and centrifuge. add 2 mL of diluted methanol (7 in 10). QSa and QSb . QTa and QTb .2 µm and use this filtrate as the test solution. Separately. to the peak area of the internal standard of the standard solution.0 mL of the internal standard solution. add exactly 4 mL of the internal standard solution and use these solutions as the standard solution. respectively.0 mL of the internal standard solution. dissolve in diluted methanol (7 in 10) to make exactly 200 mL. WSB : Amount (mg) of Ethinylestradiol RS. shake for 20 minutes and centrifuge. add 2. QTa and QTb . of the peak area of the internal standard of the test solution and also the ratios. System suitability System performance: When the procedure is run with 20 µL of the standard solution under the above operating conditions: eythinlestradiol. Assay Weigh accurately and powder not less than 20 Norgestrel and Ethinylestradiol Tablets. Take 1 tablet of Norgestrel and Ethinylestradiol Tablets. Eythinlestradiol⎯A fluorophotometer (excitation wavelength: 281 nm. about 4 mm in inside diameter and about 25 cm in length. Cb : Labeled amount of ethinylestradiol (C20H24-O2) in 1 tablet. dissolve in diluted methanol (7 in 10) to make exactly 200 mL. Pipet 2. equivalent to 100 times each of the labeled amounts. the relative standard deviation of the ratios of the peak area of ethinylestradiol and norgestrel to that of the internal standard are not more than 1. of the peak area of the internal standard of the test solution and also the ratios.2 µm and use this filtrate as the test solution. emission wavelength: 305 nm) Column: A stainless steel column. Filter the supernatant liquid through a membrane filter with pore size not more than 0. Calculate the ratios.0 mL of diluted methanol (7 in 10). respectively. Flow rate: Adjust the flow rate so that the retention time of norgestrel is about 10 minutes. add 2. respectively. Mobile phase: A mixture of acetonitrile water (11 : 9). Calculate the ratios.0 mL each of the solutions. Pipet 4. . Weigh accurately a portion of the powder. Uniformity of Dosage Units It meets the requirements when the content uniformity test is performed according to the following procedure. System repeatability: When the test is repeated 6 times with 20 µL of the standard solution under the above operating conditions. Evaporate the filtrate to dryness on a water-bath. Identification (1) Take 10 mL of Phenolated Water. combine the washing with filtrate and add water to make 50 mL.3 w/v% of phenol (C6H6O: 94. add 10 mL of chloroform. colorless liquid.05 mol/L bromine VS = 1. (2) Proceed with 5 mL of a solution of Phenolated Water for Disinfection (1 in 200) as directed in the Identification (2) under Phenol for Disinfection. Part II Identification (2) under Phenol for Disinfection. Phenolated Water for Disinfection Identification (1) Take 2 g of Phenovalin and Magnesium Oxide Powder. then add exactly 40 mL of 0.8 w/v% and not more than 2.3 w/v% of phenol (C6H6O: 94. Assay Take exactly 2 mL of Phenolated Water into an iodine flask. (2) Take 1 g of Phenovalin and Magnesium Oxide Powder. if necessary. mix with shaking.5686 mg of C6H6O Packaging and Storage Preserve in tight containers. Description Phenovalin and Magnesium Oxide Powder is white powder. Phenolated Water Phenolated Water contains not less than 1. Identification (1) Add 1 drop of ferric chloride TS to 10 mL of Phenolated Water for Disinfection: a bluepurple color is observed. add water to make 50 mL and filter: the filtrate responds to the Qualitative Test (1) for magnesium salt. with the above ingredients.11) Method of preparetion Phenol for Disinfection 31 g Water or Purified Water a sufficient quantity ⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯ To make 1000mL Mix the above ingredients. and has the odor of phenol. add water to make exactly 100 mL. Prepare the control solu- . and has the odor of phenol.1128 Monographs. dissolve the residue in 20 mL of dilute hydrochloric acid and evaporate on a water-bath to dryness. mix with shaking and filter. Description Phenolated Water is clear. Phenolated Water for Disinfection contains not less than 2. or their mixture a sufficient quantity ⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯ To make 1000 g Prepare as directed under Powders. (2) Proceed with 5 mL of a solution of Phenolated Water for Disinfection (1 in 200) as directed in the Purity (1) Heavy metals⎯Incinerate 1.05 mol/L bromine VS = 1. Phenovalin and Magnesium Oxide Powder Phenovalin and Magnesium Oxide Powder contains not less than 45. Each mL of 0.5 g of Phenovalin and Magnesium Oxide powder by strong heating.5685 mg of C6H6O Assay Take exactly 5 mL of Phenolated Water for Disinfection.0% of magnesium oxide (MgO: 40. colorless liquid. Method of Preparation Phenovalin 250 g Magnesium Oxide 500 g Starch. Description Phenolated Water for Disinfection is clear. Lactose. Filter.0% and not more than 55. (i) Heat 0.05 mol/L bromine VS and 5 mL of hydrochloric acid and proceed as directed in the Assay under Phenol for Disinfection. Perform the test.1g of the residue with 1mL of sodium hydroxide TS: a red color is observed and it disappears upon addition of excess hydrochloric acid (phenovalin). then pipet exactly 25 mL of the solution into an iodine flask and proceed as directed in the Assay under Phenol for Disinfection. Packaging and Storage Preserve in tight containers. and add 1 drop of ferric chloride TS: a blue-purple color is observed. (i) Heat 0. add 5 mL of dilute hydrochloric acid. add 25 mL of water. Wash the filter paper with water.30).8 w/v% and not more than 3. Method of Preparation Liquefied Phenol 22 mL Water or Purified Water a sufficient quantity ⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯ To make 1000mL Mix the above ingredients.1g of the residue with 3 mL of diluted ethanol (7 in 10) and 4 drops of sulfuric acid: the odor of ethylacetate is perceptible (phenovalin). Dissolve the residue in 35 mL of water and 2 mL of dilute acetic acid. Each mL of 0.11). Phenovalin and Magnesium Oxide Powder has a slightly red color on standing. Description Potash Soap is yellow-brown. dissolve the residue in 5 mL of dilute hydrochloric acid. Assay Weigh accurately about 5. Each mL of 0. Add 1 mL of phosphomolybdic acid (1 in 10) to the filtrate: yellowish green precipitate is produced. Uniformity of Dosage Units(divided) It meets the requirement. If necessary to get a proper viscosity. Packaging and Storage Preserve in tight containers.4 g of Phenovalin and Magnesium Oxide Powder. Dry the residue 80 o C to a constant weight and weigh as fatty acids. heat in a water-bath and continue the saponification. add 5 mL of dilute hydrochloric acid.02). After complete saponification. Particle Size Distribution Test It meets the requirement. evaporate ether on a water-bath at a temperature as low as possible. 4. Perform the test (not more than 6. Transfer the ether solution to a tared flask. Pipet 25. Description Polyethyleneglycol Ointment is a white. add 1 mL of barium chloride. Method of Preparation Fixed Oil 470 mL Potassium Hydroxide a sufficient quantity Water or Purified Water a sufficient quantity ⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯ To make 1000 g Dissolve Potassium Hydroxide. in Water or Purified Water. Packaging and Storage Preserved in tight containers.50 mL of 1 mol/L hydrochloric acid VS: no turbidity is produced. and has characteristic odor.0152 mg of MgO Packaging and Storage Preserved in well-closed containers. and titrate with 0. add 10 mL of water and 4. Ringer's Solution contains not less than 0.KP VIII 1129 tion as follows: evaporate 20 mL of dilute hydrochloric acid to dryness and add 2 mL of dilute acetic acid. adjust amounts of the Polyethyleneglycol 400 and Polyethyleneglycol 4000 up to 100 g with total amount of 1000 g. and has a slight.0% as fatty acids. previously warmed. add water to make exactly 100 mL and filter.0 mL of dilute hydrochloric acid and shake.7.30 g of Phenovalin and Magnesium Oxide Powder by strong heating. accurately weighed.036% of calcium chloride (CaCl2· 2H2O: 147.030% and not more than 0. pH 10. if necessary. Discard the first 20 mL of the filtrate. Acidify the mixture with dilute sulfuric acid and cool. Identification Take 50 mg of Polyethylenelycol Ointment.58% of chlorine [as (Cl: 35. Add 1 drop of phenophthalein TS to this solution: no red color develops.0 mL of the subsequent filtrate and shake twice with 5 mL volumes of chloroform. unctuous. (2) Arsenic⎯Incinerate 0. 40 mL and 30 mL volumes of ether. Extract the solution with 50 mL.6 ppm). Separate the water layer. Purity Silicic acid and alkali⎯Dissolve 10 g of Potash Soap in 30 mL of ethanol and add 0.0 g of Potash Soap. transparent. soft mass.53% and not more than 0. To this solution.05 mol/L disodiumethylenediaminetetraacetate VS (indicator: 40 mg of eriochrome black T-sodium chloride indicator). in required quantity for saponification. Mix well and allow to cool and stir until congealed.45)] and not less than 0. stir thoroughly. Potash Soap Potash Soap containers not less than 40. add this solution to fixed oil. Polyethylenglycol Ointment Macrogol Ointment Method of Preparation Polyethyleneglycol 4000 500 g Polyethyleneglycol 400 500 g ⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯ Total 1000 g Melt Polyethyleneglycol 4000 and Polyethyleneglycol 400 by warming on a water-bath to 65 o C . Assay Take about 0. mix with shaking and filter if necessary. Ringer’s Solution Ringer's Solution is an aqueous solution for injection. add 50 mL of water and 5 mL of ammonia-ammonium chloride buffer solution. dissolve in 100 mL of hot water and transfer to a separatory funnel. add a sufficient quantity of Ethanol. Method of Preparation . characteristic odor.05 mol/L disodiumethylenediaminetetraacetate VS = 2. Potash Soap is freely soluble in water and in ethanol.0 mL of standard lead solution and water to make 50 mL (not more than 27 ppm). Wash the combined ether extracts with 10 mL volumes of water until the washing contains no acid. add Water or Purified Water to make 1000 g. previously dried in desiccator (silica gel) for 3 hours and accurately weighed. Pipet 10. Spot 5 μL each of the test solution and the standard solution on the plate of silica gel with fluorescent indicator for thin-layer chromatography.3% of salicylic acid (C7H6O3: 138.0 mL each of the test solution . Discard the first 10 mL of the filtrate and use the subsequent filtrate test solution. Each mL of 0. Perform the test with the test solution and the standard solution as directed under the Thinlayer Chromatography. dissolve 10 mg of Salicylic Acid RS in 5 mL of methanol and use this solution as the standard solution.3 g Calcium Chloride 0.1 mol/L silver nitrate VS shaking vigorously (indicator: 3drops of sodium fluorescein TS). Develop the plate with a mixture of chloroform.0 mL of this solution. Method of Preparation Salicylic acid.3 ppm). dilute with ethanol to make exactly 100 mL and use the solution as the standard solution. colorless liquid. Identification (1) Evaporate 10 mL of Ringer's Solution to 5 mL: the solution responds to the Qualitative Tests for potassium salt and calcium salt. (2) Arsenic—Proceed with 20 mL of Ringer's Solution and perform the test (not more than 0.1 ppm). with the above ingredients. Assay Weigh accurately about 0. Prepare the control solution as follows: to 3.1 mol/L silver nitrate VS = 3.0 mL of standard lead solution.0 and 7.3 g of Salicylated Alum Powder with 5 mL of methanol. add 2 mL of dilute acetic and add water to make 50 mL.0 mL of Ringer's solution. Description powder.0 mL of Ringer's Solution.7% and not more than 3. Bacterial Endotoxins Less than 0. Examine the plate under ultraviolet light (main wavelength: 254 nm): the spot from the test solution and that from the standard solution show the same R f value.5453 mg of Cl (2) Calcium chloride—Pipet 50. with the above ingredients. It meets Insoluble Particulate Matter Test for Injections meets the requirement. No preservative may be added.(not more than 0. Description Ringer's solution is a clear.01 mol/L disodium ethylenediaminetetraacetate VS until the color of the solution changes from red-purple to blue. (2) Shake 0. Salicylated Alum Powder Salicylated Alum Powder contains not less than 2.6 g Potassium Chloride 0. Separately. and has a saline taste.1 g of Salicylic Acid RS. Foreign Insoluble Particulate Matter Test the requirement.50 EU per mL of Ringer’s Solution.33 g Water for Injection a sufficient quantity ⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯ To make 1000 mL Prepare as directed under Injection. add 30 ml of water and titrate with 0. Salicylated Alum Powder is a white Identification (1) The colored solution obtained in the Assay has a red-purple color and exhibit absorbance maximum between 520 nm and 535 nm (salicylic acid). Part II Sodium Chloride 8. finely powdered 30 g Dried Aluminum Potassium Sulfate.33 g of Salicylated Alum Powder. (2) Ringer's Solution responds the Qualitative Tests for sodium salt and chloride. Pipet 10. Separately. pH Between 5. Sterility Test It meets the requirement. filter and use the filtrate as the test solution. Each mL of 0. Purity (1) Heavy metals—Evaporate 100 mL of Ringer's Solution to about 40 mL on a water bath. acetone and glacial acetic acid (45 : 5 : 1) to a distance of about 10 cm and air-dry the plate. Dilute with ethanol to make exactly 100 mL and filter. add 2 mL of dilute acetic acid and water to make 50 mL and perform the test.5. dissolve about 0.1130 Monographs. add 80 mL of ethanol and shake vigorously.12). Assay (1) Chlorine—Pipet 20.01 mol/L disodium ethylenediaminete- traacetate VS = 1.4701mg of CaCl2·2H2O Packaging and Storage Preserve in hermetic containers and plastic containers for aqueous infusions may be used. in sufficient ethanol to make exactly 100 mL. very finely powdered a sufficient quantity ⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯ To make 1000 g Prepare as directed under Powders. It Determination of Volume of Injection in Containers It meets the requirement. very finely powdered 640 g Talc. add 2 mL of 8 mol/L potassium hydroxide TS 50 mg of NN indicator and titrate immediately with 0. Spray evenly ferric chloride TS upon the plate: the spot from the standard solution and the corresponding spot from the test solution reveal a purple color. add 10 mL of ethanol and water to make exactly 100 mL. with the above ingredients.0 mL of this solution. instead of the test solution and make any necessary correction. pH 2. resin. using a blank solution prepared in the same manner with water instead of the test solution. and use this solution as the standard solution.0 mL of ferric nitrate solution (1 in 200) and dilute with hydrochloric acid-potassium chloride buffer solution.88. Description Salicylic Acid Spirit is clear. Salicylic Acid Adhesive Plaster Method of Preparation Salicylic Acid.8 (Method 2). colorless liquid. respectively.43% and not more than 0. in 10 mL of ethanol and add water to make exactly 100 mL.3 g of Salicylic Acid RS. with the above ingredients. pH 2.0 mL of Salicylic Acid Spirit. of the test solution and the standard solution at 530 nm as directed under the Ultraviolet-visible Spectrophotometry. previously dried in a desiccator (silica gel) for 3 hours and accurately weighted. Assay Take 10.. Pipet 10. respectively.3% of salicylic acid (C7H6O3: 138. Amount (mg) of salicylic acid (C7H6O3) = amount (mg) of Salicylic Acid RS × AT AS Packaging and Storage Preserve in tight containers. Description Compound Salicylic Acid Spirit is a clear. Packaging and Storage Preserved in light-resistant. Separately. using a blank solution prepared in the same manner with 10 mL of ethanol.11). add with hydrochloric acidpotassium chloride buffer solution. Salicylic Acid Spirit Salicylic acid spirit contains not less tha 2. to make exactly 25 mL.0. Method of Preparation Salicylic acid 20 g Liquefied Phenol 5 mL Glycerin 40 mL Ethanol 800 mL Water or Purified Water a sufficient quantity ⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯ To make 1000 mL Prepare as directed under Medicated Spirits. AT and AS. finely powdered 500 g Adhesive plaster base a sufficient quantity ⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯ To make 1000 g Adhesive plaster consists of a mixture of the following ingredient with carefully selected rubber. to make exactly 25 mL.0. Pipet 3. Description The surface of Salicylic Acid Adhesive Plaster is white and adheres well to the skin. 20 Specific gravity⎯ d 20 : About 0. Determine the absorbances. add hydrochloric acid-potassium chloride . Determine the absorption spectrum of the solution as directed under the Ultraviolet-visible Spectrophotometry: it exhibits a maximum between 520 nm and 535 nm (salicylic acid). pH 2. to make exactly 100 mL.86. Identification (1) Take 1 mL of Compound Salicylic Acid Spirit. add 5 mL of a solution of ferric nitrate (1 in 200) and add hydrochloric acid-potassium chloride buffer solution.0 mL of the test solution and the standard solution. to make exactly 100 mL and use this solution as the test solution. add 5.0. Alcohol Number Not less than 8.12) and not less than 0. Pipet 3. Determine the absorbance. zinc oxide and other substances. add hydrochloric acid-potassium chloride buffer solution. respectively. Identification The solution obtained in the Assay is red-purple. Amount (mg) of salicylic acid (C7H6O3) = amount (mg) of Salicylic Acid RS × AT 1 × AS 10 Packaging and Storage Preserve in well-closed containers. Method of Preparation Salicylic Acid 30 g Glycerin 50 mL Ethanol a sufficient quantity ⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯ To make 1000 mL Prepare as directed under Medicated Spirits. well-closed containers.KP VIII 1131 and the standard solution into stoppered test tubes.0. Salicylic Acid Adhesive Plaster has adhesive properties.12).8% and not more than 2. 20 Specific gravity⎯ d 20 : About 0. AT and AS. colorless to pale red liquid.2% of salicylic acid (C7H6O3: 138. Compound Salicylic Acid Spirit Compound Salicylic Acid Spirit contains not less than 1.7% and not more than 3. Salicylic Acid Adhesive Plaster spreads evenly on a fabric.53% of phenol (C6H6O: 94.0 mL of this solution. as directed under the Ultraviolet-visible Spectrophotometry. dissolve 0. for the test solution and the standard solution. pH 2. Spray evenly ferric chloride TS upon the plate: the spot from the standard solution (1) and the corresponding spot from the test solution (1) reveal a purple color. Proceed with 10 μL of this solution under the above operating conditions. 0.2 g of benzoic acid. Operating conditions Detector: An ultraviolet absorption photometer (wavelength: 270 nm). acetone and glacial acetic acid (45 : 5 : 1) to a distance of about 10 cm and air-dry the plate. with the above ingredients.0 mL of this solution. Selection of column: Dissolve 0.5 (Method 2). Scopolia Extract and Ethyl Aminobenzoate Powder Scopolia Extract and Ethyl Aminobenzoate Powder contains not less than 22. . Flow rate: Adjust the flow rate so that the retention time of salicylic acid is about 6 minutes. Column: A stainless steel column. add 5 mL of ferric nitrate (1 in 200): a red purple color is observed (salicylic acid). of the peak area of salicylic acid and phenol to that of the internal standard in the standard solution. May be prepared with 10% Scopolia Extract Powder in place of Scopolia Extract. dissolve in diluted methanol (1 in 2) to make exactly 100 mL. Separately. Assay Measure accurately 2 mL of Compound Salicylic Acid Sprit. add 5 mL of dilute hydrochloric acid. respectively.1 mol/L phosphate buffer solution.5% of ethyl aminobenzoate (C9H11NO2: 165. Weigh accurately about 0. extract with 5 mL of chloroform and use the extract as the test solution (1). add 5.5 mL of Compound Salicylic Acid Spirit. pH 7. Use a column giving elution of benzoic acid.0. Lactose or their mixture a sufficient quantity ⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯ To make 1000 g Prepare as directed under Powders. add 5. Develop the plate with a mixture of chloroform. add 5 mL of dilute hydrochloric acid. (2) Take 1 mL of Compound Salicylic Acid Spirit. pH 2. allow to stand for 10 minutes and add 3 mL of sodium hydroxide TS: a yellow color is observed (phenol).2 g of salicylic acid and 50 mg of theophylline in 100 mL of diluted methanol (1 in 2).0 and methanol (3 : 1). Column temperature: A room temperature. To 10 mL of this solution add 90 mL of dilute methanol (1 in 2). (3) Take 0. Mobile phase: A mixture of 0. Method of Preparation Scopolia Extract 10 g Ethyl Aminobenzoate 250 g Magnesium Oxide 150 g Sodium Bicarbonate 500 g Starch. Part II buffer solution. Examine under ultraviolet light (mail wavelength: 254 nm): the spot from the test solution (1) and the standard solution (1) show the same R f value and the spots from the test solution (2) and the standard solution (2) shows the same R f value. wash the twice extract with 5 mL volumes volume of sodium bicarbonate TS and use the chloroform extract as the test solution (2). in the test solution and the ratios.5% and not more than 27. salicylic acid and theophylline in this order and clearly dividing each peak. To 5 mL of this solution. Wash the extract twice with 5 mL volumes of sodium bicarbonate TS and extract with 10 mL of dilute sodium hydroxide TS and 1 mL of dilute hydrochloric acid. QSa and QSb . dissolve 10 mg each of salicylic acid and phenol in 5 mL each of chloroform and use both solution as the standard solution (1) and the standard solution (2). of the peak area of salicylic acid and phenol to that of the internal standard. previously dried in a desiccator (silica gel) for 3 hours and about 50 mg of Phenol RS.1132 Monographs. Perform the test with the test solutions (1) and (2) and the standard solutions (1) and (2) as directed under the Thin-layer Chromatography.0 mL of the internal standard solution and diluted methanol (1 in 2) to make 100 mL and use this solution as the test solution. to make 200 mL. peaked with octadecylsilanized silica gel for liquid chromatography (5 μm in particle diameter). Packaging and Storage Preserve in tight containers. Spot 5 μL each of the test solutions (1) and (2) and the standard solutions (1) and (2) on a plate of silica gel with fluorescent indicator for thinlayer chromatography. about 4 mm in inside diameter and 25 cm to 30 cm in length. Alcohol Number Not less than 7. To 2 mL of Compound Salicylic Acid Spirit. Perform the test with 15 μL each of the test solution and the standard solution as directed under the Liquid Chromatography according to the following operating conditions and calculate the ratios.2 g of Salicylic Acid RS. Amount (mg) of salicylic acid (C7H6O3) = amount (mg) of Salicylic Acid RS × Q Ta 1 × Q Sa 5 Amount (mg) of phenol (C6H6O) = amount(mg) of Phenol RS × Q Tb 1 × Q Sb 5 Internal Standard Solution—A solution of theophylline in methanol (1 in 1250). QTa and QTb . Pipet 20.0 mL of the internal standard solution and diluted methanol (1 in 2) to make 100 mL and use this solution as the standard solution. add 20 mL of water and 5 mL of dilute hydrochloric acid and extract with 20 mL of ether. extract with 5 mL of chloroform.19). Use a blank prepared in the same manner with 5 mL of water in place of the test solution and make any necessary correction. transfer to a Soxhlet extractor. AT and As.19). (i) Dissolve 10 mg of the residue in 1 mL of dilute hydrochloric acid and 4 mL of water: the solution responds to the Qualitative Test for primary aromatic amines. Pipet 5. Add 2 mL of N(1-naphthyl)-N-diethylethylenediamine oxalate-acetone TS. add 20 mL of ether. Wash the ether layer twice with 10 mL volumes of a saturated solution of sodium chloride. Papaverine and Ethyl Aminobenzoate Powder contains not less than 10. Assay Weigh accurately about 0. Method of Preparation Scopolia Extract Papaverine Hydrochloride 15 g 15 g . at 550 nm. (ii) Dissolve 0. Identification (1) Take 2 g of Scopolia Extract and Ethyl Aminobenzoate Powder. Amount(mg) of ethyl aminobenzoate (C9H11NO2) = amount(mg) of ethyl aminobenzoate RS × AT AS Packaging and Storage Preserve in well-closed containers. and has a slightly bitter taste. combine the filtrate and the washing. add 10 mL of dilute hydrochloric acid. place this solution in a separatory funnel. shake and filter: the filtrate responds to the Qualitative Test for magnesium salt. Perform the test with the test solution and the standard solutions (1) and (2) as directed under the Thin- layer Chromatography.3 g of Scopolia Extract and Ethyl Aminobenzoate Powder. respectively. leaving a sensation of numbness on the tongue. shake and filter through a glass filter (G4). Evaporate the filtrate to dryness. add 100 mL of water. wash twice with 25 mL volumes of a mixture of hexane and ether (1 : 1) by shaking well and place the water layer in another separatory funnel. After cooling. separate the ether layer. dissolve 20 mg of Atropine Sulfate RS and 10 mg of Scopolamine Hydrobrominde in 10 mL each of ethanol and use these solutions as standard solution (1) and standard solution (2). Wash the residue three times with 10 mL volumes of ether. shake gently and filter: the filtrate responds to the Qualitative Test for sodium salt and for bicarbonate. (2) Take the ether-insoluble residue obtained in (1). Spot 10 μL each of the test solution and the standard solutions on a plate of silica gel for thin-layer-chromatography. prepared before use and allow to stand for 5 minutes with occasional shaking. (3) Take the water-insoluble residue obtained in (2). Add 0. shake well and to stand for 10 minutes. as directed under the Ultraviolet-visible Spectrophotometry. until the color of the solution changes from green to yellow-green. After cooling.KP VIII 1133 Description Scopolia Extract and Ethyl Aminobenzoate Powder is slightly brownish white.0 mL each of the test solution and the standard solution.2 mL of ethanol and use this solution as the test solution. Separately. to each add 10 mL of 1 mol/L hydrochloric acid TS. Dissolve the residue in 25 mL of 1 mol/L and use this solution prepared 100 mL with water as the test solution.0 mL of this solution and the standard solution.1 g of the residue in 5 mL of water with the aid of dilute hydrochloric acid added dropwise and add iodine TS dropwise: a brown precipitate is produced. respectively. water and strong ammonia water (90 : 7 : 3) to a distance about 10 cm and dry the plate at 80 °C for 10 minutes. Transfer the residue in the flask to the same glass filter with the filtrate and filter the residue by suction while pressing vigorously the residue on the same glass filter.8% and not more than 13. dissolve the residue in 0. add 3 g of anhydrous sodium sulfate. extract with 100 mL of ether for 1 hour and evaporate the ether on a water-bath. (4) Place 30 g of Scopolia Extract and Ethyl Aminobenzoate Powder in a glass-stoppered conical flask. shake and filter through absorbent cotton. previously dried in a desiccator (silica gel) for 3 hours. Weigh accurately about 75 mg of ethyl aminobenzoate RS.2 mL of bromocresol green TS to this solution and add dilute sulfuric acid drop-wise while shaking thoroughly.2% of ethyl aminobenzoate (C9H11 NO2: 165. shake for 30 minutes and filter immediately by suction through a glass filter (G3). Make slightly alkaline with ammonia TS. determine the absorbances. evaporate to dryness and perform the following test with the residue (ethyl aminobenzoate). Allow to stand for 2 hours. Scopolia Extract. Develop the plate with a mixture of acetone. add immediately 30 mL of ether and shake well. mix immediately and add water to make exactly 50 mL. then add 1 mL of a solution of sodium nitrite (1 in 200). add 30 mL of water. Place 75 mL of the filtrate in a 300-mL beaker and add cautiously 10 mL of diluted sulfuric acid (1 in 3). Add 5 mL of ammonium sulfate TS. of the test solution and the standard solution. spray evenly Dragendorff's TS for spraying on the plate: two principal spots from the test solution show the same color and Rf value with each yellow-red spot from the standard solutions. Papaverine and Ethyl Aminobenzoate Powder Scopolia Extract. (iii) Warm 50 mg of the residue with 2 drops of acetic acid and 5 drops of sulfuric acid: the odor of ethyl acetate is perceptible. Pipet 5. dissolve in 25 mL of 1 mol/L hydrochloric acid TS and add water to make exactly 100 mL. weigh accurately about 75 mg of ethyl aminobenzoate RS. determine the absorbances. Evaporate the filtrate to dryness. Make the aqueous layer slightly alkaline with ammonia TS. (3) Place 20 g of Scopolia Extract. Papaverine and Ethyl Aminobenzoate Powder in a glass-stoppered conical flask. add 1 drop of formalinsulfuric acid TS: a colorless or pale yellow-green color. Particle Size Distribution Test It meets the requirement.0 mL each of the test solution and the standard solution. shake for 15 minutes and filter by suction through a glass filter (G3). add water to make exactly 250 mL and use this solution as the standard solution. add water to make exactly 250 mL and use this solution as the test solution. Pipet 5. add immediately 30 mL of ether and shake well. Papaverine and Ethyl Aminobenzoate Powder. is observed. Dissolve 20 mg of Atropine Sulfate RS.1 mol/L hydrochloric acid TS. as directed under the Ultraviolet-visible Spectrophotometry. May be prepared with 10% Scopolamine Extract Powder in place of Scopolamine Extract. and has slightly bitter tastes. Spot 10 μL each of the test solution and the standard solution on a plate of silica gel for thinlayer chromatography. respectively. filter and further wash the residue with 10 mL of chloroform.6 g of Scopolia Extract. After cooling. add 20 mL of ether. Use a blank prepared in the same manner with 5 mL of water in place of the test solution and make any necessary correction. then add 1 mL of a solution of sodium nitrite (1 in 200) prepared before use and allow to stand for 5 minutes. (i) To 1 mg of the residue. add 10 mL of 1 mol/L hydrochloric acid TS to each. Develop the plate with a mixture of chloroform. Wash the ether layer with two 10 mL volumes of a saturated solution of sodium chloride and separate the ether layer. Pipet 5. separate the chloroform layer. (2) and (3) show the same R f values. dissolve the residue in 0. combine the filtrate and the washing. (ii) Dissolve 1 mg of the residue in 3 mL of acetic anhydride and 5 drops of sulfuric acid. mix immediately and add water to make exactly 50 mL. Evaporate the filtrate to dryness. After shaking. for the test solution and the standard solution. Pipet 5. (iii) Warm 50 mg of the residue with 2 drops of acetic acid and 5 drops of sulfuric acid: the odor of ethyl acetate is perceptible. dissolve in 25 mL of 1 mol/L hydrochloric acid TS and add water to make exactly 100 mL. methanol. at 550 nm. (ii) Dissolve 0.5 mL of 1 mol/L hydrochloric acid TS and extract three times with 20 mL volumes of chloroform by shaking. AT and AS. It meets the require- Assay Weigh accurately about 0. with the above ingredients. heat in a waterbath for 1 minute and view under ultraviolet light: the resolution shows a yellow-green fluorescence. Wash the residue three times with 10 mL volumes of ether. Part II Ethyl Aminobenzoate 120 g Starch. Combine the filtrate and the washing. add 2 g of anhydrous sodium sulfate. Amount (mg) of ethyl aminobenzoate (C9H11NO2) = amount(mg) of ethyl aminobenzoate RS × AT AS . add 20 mL of chloroform. add 0. leaving a sensation of numbness on the tongue. Transfer 60 mL of the filtrate to a separatory funnel.0 mL of this solution. Allow to stand for 2 hours. shake and filter through absorbent cotton. Perform the test with the test solution and the standard solutions (1). transfer to a Soxhlet extractor and extract with 100 mL of ether for 1 hour and evaporate the ether on a waterbath. spray Dragendorff's TS upon the plate evenly: three yellow-red principal spot obtained from the test solution and the corresponding spots from the standard solutions (1). dry the residue at 105 °C for 3 hours and perform the following tests (papaverine hydrochloride). Description Scopolia Extract. changing to red-purple. (2) Take the ether-insoluble residue obtained in (1). Dissolve the residue in 25 mL of 1mol/L hydrochloric acid TS and add water to make exactly 100 mL. Lactose or their mixture a sufficient quantity ⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯ To make 1000 g Prepare as directed under Powders. shake and filter through a pledget of cotton. 10 mg of Scopolamine Hydrobromide RS and 20 mg of Papaverine Hydrochloride RS in 10 mL each of ether and use these solutions as the standard solutions (1). acetone and strong ammonia water (73 : 15 : 10 : 2) to a distance of about 10 cm and dry the plate at 80 °C for 20 minutes. shake well and allow to stand for 10 minute. add 80 mL of water. Identification (1) Take 4 g of Scopolia Extract.1 g of the residue in 5 mL of water with the aid of dilute hydrochloric acid added dropwise and add iodine TS dropwise: a brown precipitate is produced. transfer this solution to a separatory funnel and add 10 mL of 0.2 mL of ethanol and use this solution as the test solution. Add 2 mL of N(1-naphthyl)-N-diethylethylenediamine oxalate-acetone TS. Add 3 g of anhydrous sodium sulfate. Separately.0 mL of this solution. shake well. evaporate to dryness and perform the following test with the residue (ethyl aminobenzoate): (i) Dissolve 10 mg of the residue in 1 mL of dilute hydrochloric acid and 4 mL of water: the solution responds to the Qualitative Test for primary aromatic amines. previously dried in a desiccator (silica gel) for 3 hours. (2) and (3) as directed under the Thin-layer Chromatography. Papaverine and Ethyl Aminobenzoate Powder is brownish yellow to grayish yellow-brown. shake and filter through a glass filter (G4). (2) and (3).1134 Monographs. Papaverine and Ethyl Aminobenzoate Powder. Add 5 mL of ammonium sulfamate TS. Uniformity of Dosage Units ment. Preserve in light-resistant. heat with occasional shaking in a water-bath for 45 minutes and cool. Add 2 mL of nitric acid. colorless liquid . with the above ingredients.787 mg of Ag Packaging and Storage tight containers. (4) Place 3 mL of Silver Protein Solution in a crucible.1 mol/L ammonium thiocyanate VS = 16. Add 5 mL of a solution of sodium hydroxide (1in 10) to the filtrate and add 2 mL of diluted cupric sulfate (2 in 25): a purple color is observed (silver protein). Assay Pipet exactly 25 mL of Silver Protein Solution into a 250 mL Kjeldahl flask and heat cautiously until a white gas of glycerin is evolved. cover the flask with a small funnel and heat gently for 5 minutes.1 mol/L ammonium thiocyanate VS (indicator: 2mL of ferric ammonium sulfate TS). Assay Weigh accurately 20 mL of Silver Nitrate Ophthalmic Solution. Simple Ointment Method of Preparation Yellow Beeswax 330 g Fixed oil a sufficient quantity ⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯ To make 1000 g Prepare as directed under Ointments. Silver Protein Solution Silver Protein Solution contains not less than 0. Description Silver Protein Solution is clear. mix and add 2 mL of sodium hydroxide TS. add 30 mL of water and 2 mL of nitric acid and titrate with 0.87). add 10 mL of ethanol.22% and not more than 0. Then ignite gradually to ash.95w/v% and not more than 1.1 mol/L ammonium thiocyanate VS (indicator: 3mL of ferric ammonium sulfate TS). dissolve the residue in 1 mL of nitric acid by warming and add 10 mL of water: the solution responds to the Qualitative Tests (1) for silver salt.05w/v% of silver nitrate (AgNO3: 169. heat cautiously and evaporate almost to dryness. Add immediately 1 mL of a solution of cupric chloride in ethanol (1 in 10). After cooling. Insoluble Particulate Matter Test for Ophthalmic Solutions It meets the requirement. Preserve in light-resistant. shake frequently for 5 minutes and filter. brown liquid.87). with the above ingredients. boil gently and repeat this operation until the solution becomes colorless upon cooling. Method of Preparation Silver Protein Glycerin Mentha Water 30 g 100 mL a sufficient quantity ⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯ To make 1000 mL Dissolve and mix the above ingredients. . (2) Take 3 mL of Silver Protein Solution. Identification Silver Nitrate Ophthalmic Solution responds to the Qualitative Tests for silver salt and for nitrate.KP VIII 1135 Packaging and Storage well-closed containers. drop gradually 5 mL of nitric acid. shake and filter: the filtrate is blue (glycerin).987 mg of AgNO3 Packaging and Storage tight containers.26% of silver (Ag: 107. Preserve light-resistant. Boil gently for 5 minutes. Method of Preparation Silver Nitrate 10g Sterile Purified Water a sufficient quantity ⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯ To make 1000 mL Prepare as directed under Ophthalmic Solution. Silver Nitrate Ophthalmic Solution Silver Nitrate Ophthalmic Solution is an aqueous eye lotion containing not less than 0. Identification (1) Take 1 mL of Silver Protein Solution. Each mL of 0. add water to make 10 mL. (3) Take 5 mL of the test solution obtained in (2) and add ferric chloride TS dropwise: a brown precipitate is produced (silver protein). Foreign Insoluble Matter Test It meets the requirement. Sterility Tests It meets the requirement.1mol/L ammonium thiocyanate VS = 10. cool and titrate with 0. add 25 mL of sulfuric acid. Transfer cautiously the cooled content in the flask into a 500-mL Erlenmyer flask with 250 mL of water. Each mL of 0. Description Silver Nitrate Ophthalmic Solution is clear. and has the odor of mentha oil. add 2 mL of dilute hydrochloric acid. After cooling. Method of Preparation Sucrose 850 g Purified Water a sufficient quantity ⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯ To make 1000 mL Prepare as direction under Syrup. with the above materials. 1 g of residue so obtained. separate the ether layer.1 mol/L sodium hydroxide VS (indicator: 1 mL of phenolphthalein TS): total acid is not less than 0. Description Simple Syrup is a clear. d 20 Purity (1) Artificial sweetening agent⎯Take 100 mL of Simple Syrup.80 w/v%. Each mL of 0. To each volume.07) (by specific gravity) and not less than 0. stopper and allow to stand for 10 minutes. is odorless.5 g of activated charcoal. has a characteristic. Description White ointment is white. Wash the beaker with 100mL of water and combine the washings in the distillation . containing previously added 100 g of sodium chloride. Wine contains no artificial sweetener and no artificial coloring agent. Cool. add water to make 100 mL. Description Wine is a pale yellow or reddish purple to red-purple liquid.09). White Ointment Method of Preparation White Beeswax 50g Sorbitan Sesquioleate 20g White Petrolatum a sufficient quantity ⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯ To make 1000g Prepare as directed under Ointments. To 100 mL of the filtrate add 10 mL of a saturated solution of sodium sulfate.990 and 1. aromatic odor and a slightly astringent and faintly irritating taste.1 mol/L sodium hydroxide VS = 7. add 100 mL of ether. acidify 50 mL volume of the solution with dilute sulfuric acid and make another 50 mL volume alkaline with sodium hydroxide TS. shake.310 and 1. add 2 mL of dilute sulfuric acid. (2) Salicylic acid⎯Take the residue obtained in (1) and add 2 to 3drops of dilute ferric chloride TS: no purple color is observed. colorless to pale yellow. Wine Wine is an alcoholic liquid obtained by fermenting the juice of the fruits of Vitis vinifera Linné or allied plants (Vitaceae). Part II Description Simple Ointment is yellow and has a slight characteristic odor. Multiply the optical rotation observed by 1. Cool. Wine contains not less than 11 vol% and less than 14 vol% of ethanol (C2H6O: 46. Packaging and Storage Preserve in tight containers. shake. and has slight.1 g of the residue obtained in (1). add 4 mL of sodium hydroxide TS and 3 mL of Fehling's TS and heat to boiling: a red to dark red precipitate is produced. shake well and filter.504 mg of C4H6O6 (2) Volatile acid [as acetic acid (C2H4O2: 60.05)]⎯Transfer 100 mL of Wine to a beaker.10 w/v% and not more than 0.1 mol/L sodium hydroxide VS titrated in (1) to make the solution alkaline and concentrate to 50 mL on a waterbath. Simple Syrup Simple Syrup is an aqueous solution of Sucrose. add 0. combine the two ether layers and evaporate the ether extract on a waterbath to dryness: the residue has no sweet taste. when ignited.1136 Monographs.010. add 1 mL of 1 mol/L sodium hydroxide VS and the same volume of 1 mol/L sodium hydroxide VS as that of 0. d 20 Purity (1) Total acid [as tartaric acid (C4H6O6)]⎯Take exactly 10 mL of Wine. Allow 20 mL of the test solution to stand for 24 hours. add 16 mL of lead subacetate TS. boil. to bulky charcoal. add 250 mL of freshly boiled and cooled water and titrate with 0. and has a sweet taste.3 o Boil 160 mL of Wine.40 w/v% of tartaric acid (C4H6O6: 150. with the above materials. Identification (1) Evaporate Simple Syrup on a water-bath to dryness. filter and use the filtrate as the test solution.40 w/v% and not more than 0.21 and designate as the optical rotation of Wine Specific Gravity 20 : Between 0. (2) Take 0. transfer to a 1000 mL distillation flask. Filter and observe the optical rotation of the filtrate in a 200 mm cell. shake. shake well.325. characteristic odor. viscous liquid. Optical Rotation α D : Between -0. emitting an odor of caramel. Packaging and Storage Preserve in tight containers.3 o and +0. dilute with water to make 160 mL. Specific Gravity 20 : Between 1. neutralize with potassium hydroxide TS and concentrate to 80 mL on a water-bath. add 100 mL of water. melted to swell and decomposes. Packaging and Storage Preserve in tight containers. Each mL of 0. the coloration of starch TS produced by 1 drop of 0. evaporate 90 mL of the filtrate on a water-bath. wash successively with hot water.5 mg. extending nearly to the bottom of the flask. After cooling. Heat on a water-bath.1 mol/L sodium hydroxide VS (indicator: 5 drops of phenolphthalein TS). ending to the neck of the flask. A. Pass carbon dioxide for further 15 minutes. When the color of starch TS in the U tube is discharged. remove the stopper of the flask a little. add exactly 25 mL of Wine. When the liquid become sticky. Titrate a 250 mL volume of the test solution with 0. add 1 to 2 drops of dilute sulfuric acid and allow to stand for 1 hour: a white precipitate is produced.01 mol/L iodine VS from a burette. add 1 to 2 drops of 0. combine the washings with the contents of the flask.005 mg of C2H4O (3) Sulfur dioxide⎯Stopper a 750-mL roundbottomed flask with a stopper having two holes. (5) Arsenic⎯Evaporate 10 mL of Wine on a waterbath to dryness. taking care not to boil the solution during the evaporation. cool.01 mol/L iodine VS consumed when exactly 60 minutes have passed after the beginning of distillation. A. shake vigorously each time and allow to stand. add 50 mL of boiling Fehling’s TS and heat for exactly 2 minutes. B.01 mol/L iodine VS = 0. Cool. to a Liebig’s condenser and the end of the condenser to a joint of which inner diameter is 5 mm at the lower end. Filter through a dry filter paper.KP VIII 1137 flask. supplying the water lost by distillation. add 0. with ethanol and with ether and continue to dry the precipitates by suction. cool and add dehydrated ethanol to make exactly 100 mL. neutralize with a solution of potassium hydroxide (1 in 100). insert a glass tube. add 10 to 12 mL of a dehydrated ethanol while agitating. Transfer the washings to the weighing bottle and evaporate carefully on a water-bath. 180 mL of freshly boiled and cooled water. While passing carbon dioxide. flat weighing bottle.01 mol/L iodine VS dropwise from a burette so that the color of the starch TS remains pale blue to blue during the distillation.325 g.1 mol/L sodium hydroxide VS = 6. (6) Glycerin⎯Pipet exactly 100 mL of Wine into a 150-mL porcelain dish and concentrate on a water-bath to 10 mL. dry at 105 o C for 1 hour: the residue is not less than 0. boil and add 50 mL of a solution prepared by dissolving 5. add 5 mL of dehydrated ethanol and grind to a grue-like substance.06) is not more than 7. In this case. Dilute the distillate to exactly 500 mL with water and use this solution as the test solution. Connect the tube. Through the other hole. Dissolve the residue in a small amount of dehydrated ethanol.6406 mg of SO2 (4) Total sulfuric acid⎯Transfer 10 mL of Wine to a beaker. Add 7. Each mL of 0. heat the distillation flask with caution so that 40 to 50 drops of the distillate may be obtained in 1 minute.01 mol/L iodine VS should persist at least for 1 minute: the amount of sulfur dioxide (SO2: 64. transfer to a 50 mL glass-stoppered volumetric cylinder. Read the volume of 0.5 mL volumes of dehydrated ether three times. When the solution becomes quite clear.15 w/v%. insert a glass tube. To this solution. Cover the beaker and heat on a water-bath for 2 hours. neutralize with diluted hydrochloric acid (1 in 30). add 4 drops of sodium carbonate TS. followed by further addition of 5mL of diluted hydrochloric acid (1 in 30). filter . 1) and make the solution strongly alkaline by adding a solution prepared by dissolving 4 g of calcium hydroxide in 6 mL of water. Prepare the test solution with the residue according to Method 3 and perform the test (not more than 0. Connect the other end of the joint with a holed rubber stopper to a U tube having three bulbs as shown in the Figure. Displace the air in the apparatus by carbon dioxide and place 50 mL of a freshly prepared and diluted starch TS (1 in 5) and 1 g of potassium iodide in the U tube. Through one hole. (8) Sucrose⎯Transfer 50 mL of the test solution obtained in the Optical rotation to a 100-mL flask. however. (7) Reducing sugars⎯Pipet exactly 25 mL volume of the test solution obtained in the Optical rotation. Add 5 mL of a solution of tartaric acid (3 in 20) and distil with steam cautiously to maintain the volume of the solution in the flask until 450 mL of the distillate is obtained for 45 minutes.608 g of barium chloride in 50 mL of hy- drochloric acid and water to make 1000 mL. transfer to a tared. Pass carbon dioxide washed with a solution of potassium permanganate (3 in 100) through the tube. Filter the separated precipitates by a tared filter containing asbestos mat by suction. From the other end of the U tube. Perform a blank determination and make any necessary correction: the volatile acid is not more than 0. 0.2 g of tannic acid and 30 mL of phosphoric acid and stopper again. wash with several volumes of dehydrated ethanol and add the washings to the solution in the cylinder to make 15 mL.2 ppm). Heat the filter gently at first and then strongly until the precipitates become completely black. Heat in a water-bath for 30 minutes. Cool the precipitates in a desiccator (silica gel) and weigh as cupric oxide: cupric oxide is not more than 0. centrifuge and decant the supernatant liquid in another beaker. Wash the dish seven times with 10 mL volumes of hot dehydrated ethanol. Heat on a water-bath with constant stirring and pushing down any material adhering to the wall of the dish until the contents of the dish become soft masses.45 g and not more than 0. B.90 g. Add 1 g of sea sand (No. Wash the volumetric cylinder with 5 mL of a mixture of dehydrated ether and dehydrated ethanol (3 : 2). boil and transfer to a 100 mL volumetric flask. previously dried at 105 o C for 2. Add 10 mL of ethanol. gravity d15 (2) Tartaric acid⎯Pipet 100.985. Dry the residue at 105 o C for 2 hours. add 10 g of sodium chloride and 2 mL of dilute hydrochloric acid and extract with three 10 mL volumes of ether.982 and 0. Control solution⎯Using 5 mL of water instead of the distillate. cooling and dissolving 25 g of oxalic acid in 500 mL of this dilute sulfuric acid.40%. Titrate the solution with 0. Assay (1) Ethanol⎯Pipet Wine into a 100-mL volumetric flask at 15 o C . allow to stand in water at 15 o C for 30 minutes and add water to make exactly 100 mL.5%. cool and weigh. Pipet exactly 50 mL of Wine to a tared porcelain dish and evaporate to dryness on a water-bath. Perform the test as directed under the Ultraviolet-visible Spectrophotometry with this solution. neutralize with 1 mol/L hydrochloric acid VS and add 5 mL of potassium chloride-hydrochloric acid buffer solution and water to make exactly 50mL. accurately measured. Separately. connect the flask to a distillation tube having a trap and distil using the volumetric flask as a receiver. add 2 mL of the solution prepared by adding water to 75 mL of phosphoric acid to make 500 mL and then dissolving 15 g of potassium permanganate in this solution. . wash the filter with 50 mL of hot water. measured exactly. using a solution prepared in the same manner instead of the test solution as the blank: the absorbance is not more than 0.0 mL of Wine.5 mL of ethanol containing no methanol to make exactly 50 mL and use this solution as the standard solution. evaporate on a water-bath to dryness and ignite: a half of the residue does not respond to Qualitative Tests (1) for borate. add 5 mL of sodium carbonate TS. add water to make exactly 20 mL and use this solution as the test solution. (11) Methanol⎯Take 1.2 g of tartaric acid. perform the test in the same manner. The number obtained by adding 0. deduct the amount (g) of cupric oxide determined in (7) and multiply again the number so obtained by 1. Combine the alkaline extracts.017 mg of C4H6O6 Packaging and Storage Preserve in tight containers. Shake well and determine the specific gravity at 15 o C according to Method 3 under the Specific Gravity: the specific 15 is between 0. (10) Boric acid⎯Transfer 50 mL of Wine to a porcelain dish. wash with two 5 mL volumes of water and extract with three 10 mL volumes of 0.15 at a wavelength between 220 nm and 340 nm.5 g of calcium carbonate. cinnamic acid and salicylic acid⎯Transfer exactly 50 mL of the test solution obtained in (2) to a separatory funnel. Add the washings to the sample in the flask. 0. combine the washings with the filtrate and add water to make 100 mL. add 5 mL of acetyl acetone Ts. rub the inner wall of the beaker strongly for 1 minute to induce the crystallization and allow to stand between 0 o C and 5 o C for more than 15 hours. to 1.13% and 0. transfer to a 300-mL to 500-mL flask and wash this volumetric flask with two 15 mL volumes of water.2 mol/L sodium hydroxide VS consumed.104 (g). To 25 mL of this solution. The test solution has no more color than the standard solution (12) Formaldehyde⎯Take 25 mL of Wine. wash with water.1 mol/L sodium hydroxide VS. cool.2 mol/L sodium hydroxide VS immediately (indicator: 1 mL of phenolphthalein TS). Filter the crystals with 3 mL volumes of a solution prepared by dissolving 15 g of powdered potassium chloride in 120 mL of diluted ethanol (1 in 6) and repeat the washings five times. Extract Content Between 1. add allow to stand for 15 minutes. Dissolve another half of the residue in 5 mL of hydrochloric acid: it does not respond to Qualitative Tests (2) for borate.2 mol/L sodium hydroxide VS consumed represents the amount (mL) of 0. 1). combine the washings in the beaker and dissolve the crystals by heating. Ash Between 0. Part II into a 100 mL volumetric flask.9 and 3.2: the number obtained is not more than 0. To 5 mL of the distillate. Pipet 25 mL of Wine to a 200-mL tared beaker containing 10 g of sea sand (No. Each mL of 0. distil and obtain 15 mL of the distillate. and mix with of fuchsinsulfurous acid TS. mix and heat on a waterbath for 10 minutes: the solution has no more color than that of the following control solution. Pipet exactly 5 mL of this solution. add 2 mL of glacial acetic acid.0 g of methanol add water to make exactly 1000 mL.75 to the amount (mL) of 0. Allow to stand for 30 minutes and ordinary temperature. From the number obtained by multiplying the mass (g) of cupric oxide by 2. add 50 mL of boiling Fehling’s TS and proceed as directed in (7) and weigh as cupric oxide. add 5 g of sodium chloride and 0. (9) Benzoic acid. Ignite the residue to constant weight. Combine the ether extracts. Transfer the crystals together with the filter paper to a beaker.1138 Monographs.5 mL of a solution of potassium acetate (1 in 5) and 15 g of powdered potassium chloride and shake vigorously to dissolve as much as possible. Transfer 5 mL each of the test solution and the standard solution. cool in a desiccator (silica gel) and weigh. add 2. When about 80 mL of the distillate is obtained (it takes about 20 minutes).5 hours and evaporate to dryness on a water-bath. evaporate the ether by warming on a water-bath.2 mol/L sodium hydroxide VS = 30. Decolorize these solutions by adding 2 mL of the solution prepared by adding sulfuric acid earefully to an equal volume of water.0 mL of ethanol layer obtained by Method 1 of the Alcohol Number Determination distilling without adding water after shaking with 0. stop the distillation. to test tubes. 0% of zinc oxide (ZnO: 81.33% of zinc sulfate (ZnSO4. (2) Zinc Sulfate Ophthalmic Solution responds to the Qualitative Tests for borate. mixed well.KP VIII 1139 Zinc Oxide Oil Zinc Oxide Oil contains not less than 45.27% and not more than 0. add 100 mL of water and 2 mL of ammonia-ammonium chloride buffer solution.41). pH 10.7H2O .7.5 g of Zinc Oxide Oil in a crucible. add 2 to 3 drops of potassium ferrocyanide TS: a white precipitate is produced (zinc oxide).05 mol/L disodium ethylenediaminetetraacetate VS = 4. Packaging and Storage Preserve in tight containers. Description Zinc Oxicie Oil is white to milky white.7 and titrate with 0. place in a crucible. separating a part of its ingredients when stored for a prolonged period. Add 5 mL of ammonia-ammonium chloride buffer solution.5 mL of hydrochloric acid and add water to make exactly 100 mL.8756 mg of ZnSO4. and titrate with 0. heat gradually raising the temperature until the mass is thoroughly charred and then ignite strongly: a yellow color is observed and disappears on cooling. Description Zinc Sulfate Ophthalmic Solution is a clear. Assay Pipet exactly 25 mL of Zinc Sulfate Ophthalmic Solution. To the filtrate. Method of Preparation Zinc Sultate 3g Boric Acid 20 g Sodium Chloride 5g Fennel Oil 2 mL Purified Water a sufficient quantity ⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯ To make 1000 mL Prepare as directed under Ophthalmic Solutions. add 10 mL of water and 5 mL of dilute hydrochloric acid. Identification (1) Zinc Sulfate Ophthalmic Solution responds to the Qualitative Tests for zinc salt.01 mol/L disodium ethylenediaminetetraacetate VS (indicator: 40 mg of eriochrome black Tsodium chloride indicator). Method of Preparation Zinc Oxide 500 g Fixed oil a sufficient quantity ⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯ To make 1000 g Mix the above ingredients.56). Each mL of 0. Each mL of 0. To the residue. shake well and filter. with the above ingredients.0% and not more than 55. add 80 mL of water and add a solution of sodium hydroxide (1 in 50) until a small amount of precipitates begins to produce in the solution. slimy substance. Pipet exactly 20 mL of this solution. heat gradually raising the temperature until the mass is thoroughly charred and then ignite until the residue becomes yellow and cool. An appropriate quantity of Castor Oil or polysorbate 20 may be used partially in place of fixed oil. Identification Mix thoroughly and place 0.8 g of Zinc Oxide Oil.071 mg of ZnO Packaging and Storage Preserve in tight containers Zinc Sulfate Ophthalmic Solution Zinc Sulfate Ophthalmic Solution contains not less than 0. (3) Zinc Sulfate Ophthalmic Solution responds to the Qualitative Tests for chloride.05 mol/L disodium ethylenediaminetetraacetate VS (indicator: 40 mg of eriochrome black Tsodium chloride indicator). pH 10. colorless liquid. Dissolve the residue in 1 mL of water and 1.7H2O: 287. Assay Weigh accurately about 0.01 mol/L disodium ethylenediaminetetraacetate VS = 2. Sulfate and Potassium permanganate-reducing substances⎯To 20 mL of Acetic Acid. Description Acacia occurs as colorless or pale yellow-brown. Identification Acetic Acid changes blue litmus paper to red and responds to the Qualitative Tests for Purity (1) Chloride. colorless liquid and has a pungent. Dissolve the .0 mg.0% and not more than 101. Acid-insoluble Ash Not more than 0.05 mg of C2H4O2 Packaging and Storage Preserve in tight containers. add 40 mL of water and use this solution as the test solution. (3) Non-volatile residue⎯Proceed with 30 mL of Acetic Acid as directed in the Purity (5) under Glacial Acetic Acid.5%. crystalline mass and has a pungent and characteristic odor. Boiling point⎯About 118 °C.1140 Monographs. add 5 drops of silver nitrate TS: no opalescence is produced. but produces a mucilaginous sensation on a tongue.0 mL of water and the solution is acidic. Assay Take 5. Filter the warm mixture through a tared glass filter (G3). Prepare the control solution with 3. Glacial Acetic Acid C2H4O2: 60. Purity (1) Insoluble residue⎯To 5. Each mL of 1 mol/L sodium hydroxide VS = 60.0% of acetic acid (C2H4O2: 60. add 30 mL of water and titrate with 1 mol/L sodium hydroxide VS (indicator: 2 drops of phenolphthalein TS). Identification Take 10 mL of a solution of Acacia (1 in 50) and add 0. Purity (1) Chloride⎯Take 10 mL of Glacial Acetic Acid.05). (2) and (4) under Glacial Acetic Acid. One g of pulverized Acacia dissolves almost completely in 2.0% (6 hours).5 °C. To 10 mL of the test solution. Identification A solution of Glacial Acetic Acid (1 in 3) changes blue litmus paper to red and responds to the Qualitative Tests for acetate. ethanol or ether.05 Glacial Acetic Acid contains not less than 99. Acetic Acid is miscible with water.0 mL of Acetic Acid. ethanol or glycerin. is very brittle and the fractured surface is glassy and occasionally irridescent. colorless. Acacia is practically insoluble in ethanol. tasteless. Acetic acid is miscible with water.0%.0 g of pulverized Acacia.04.0% and not more than 32. Specific gravity⎯ d 2020 : About 1.049. Proceed as directed in the Purity (1). Description Acetic Acid is a clear. Perform the test. volatile liquid. add 100 mL of water and 10 mL of dilute hydrochloric acid and dissolve by gentle boiling for 15 minutes with swirling. Part II acetate. (2) Sulfate⎯Take 10 mL of the test solution obtained in (1) and add 1 mL of barium chloride TS: no turbidity is produced. 4) Excipients Acacia Acacia is the secretion obtained from the stems and branches of Acacia senegal Willdenow or other species of the same genus (Leguminosae). (2) Tannin-bearing gums⎯Take 10 mL of a solution of Acacia (1 in 50) and add 3 drops of ferric chloride TS: no dark green color is produced. characteristic odor and an acid taste. wash the residue thoroughly with hot water and dry at 105 °C for 5 hours: the residue is not more than 10.0 mL of standard lead solution by adding 2 mL of dilute acetic acid and water to make 50 mL (not more than 3 ppm). (3) Heavy metals⎯Evaporate 2. Loss on Drying Not more than 17.0 mL of Glacial Acetic Acid on a water-bath to dryness. flocculent precipitate is produced. Ash Not more than 4. or colorless or white. Description Glacial Acetic Acid is a clear. add water to make 100 mL and use this solution as the test solution. (2) Heavy metals⎯Evaporate 10 mL of Acetic Acid Solution on a water-bath to dryness and to the residue. Acacia is odorless. Acetic Acid Acetic Acid contains not less than 30. Specific gravity⎯ d 2020 : About 1. Congealing point Not below 14. translucent or somewhat opaque spheroidal tears. or angular fragments with numerous fissures on the surface. add 2 mL of dilute acetic acid and water to make 50 mL.2 mL of dilute lead subacetate TS: a white.0% of glacial acetic acid (C2H4O2). (3) Insoluble matter⎯Take 7. A boiling solution of Agar (1 in 100) is neutral. Cool the solution between 30 o C and 39 o C : the solution forms a firm.48) and palmitic acid (C16H32O2: 256. (2) Dissolve 1 g of Agar in 65 mL of water by boiling for 10 minutes with constant stirring and add a sufficient amount of hot water to refill the water lost by evaporation: the solution is clear. warm to dissolve.0 mg. with wrinkles and somewhat lustrous. Ash Not more than 4. shake the mixture vigorously with 50 mL of water and 30 mL of ether for 3 minutes and allow to stand. add several drops of phenolphthalein TS and proceed as directed in the Acid value . Aluminum Monostearate. Loss on Drying Not more than 22. or other red algae (Rhodophyta).05 mg of C2H4O2 solution obtained in (1) and add 2 drops of iodine TS: the solution does not decolorize at once and does not show a blue color. (4) Water absorption⎯Take 5.0 g of Agar in 100 mL of water by boiling: the solution is not acidic.98). Aluminum Monostearate is practically insoluble in water. string or flakes. allow to stand at 25 o C for 24 hours and filter through moistened glass wool in a 100-mL graduated cylinder: the volume of the filtrate is not more than 75 mL. Description Agar is white. (2) Sulfurous acid and starch⎯Take 5 mL of the Aluminum Monostearate is mainly aluminum compounds of stearic acid (C18H36O2: 284. Packaging and Storage Preserve in tight containers. After cooling.10 mL of 0.0 g of Agar. Agar is odorless. other species of the same genus (Gelidiaceae).0% (6 hours). add 100 mL of hot water. (4) Potassium permanganate-reducing substances⎯Take 20 mL of the test solution obtained in (1) and add 0. tasteless and mucilagenous. Aluminum Monostearate Agar Agar is the solid residue obtained by freeze-drying of a mucilage derived from Gelidium amansii Lamouroux. contains not less than 7. Take exactly 100 mL of the solution. filter while hot through a tared glass filter (G3). Rectangular column of Agar is about 26 cm in length. transfer a 250 mL glass-stoppered flask. in ethanol or in ether.5%. add 100 mL of a mixture of ether and ethanol (2 : 1). Assay Place 10 mL of water in a glass-stoppered flask and weigh accurately. Add about 1. semi-translucent rectangular column. To the separated aqueous layer. when dried.9% of aluminum (Al: 26.2% and not more than 8.02 mol/L potassium permanganate VS: the red color does not disappear within 30 minutes. Weigh accurately about 1 g of fatty acid obtained in the Identification (2). wash the residue with a small amount of hot water and dry the residue at 105 o C for 4 hours: the residue is not more than 15. Purity (1) Sulfuric acid⎯Dissolve 1. 4 cm2 in cross section and a string of Agar is about 35 cm in length and about 3 mm in width and flakes of Agar are about 3 mm in length. Each mL of 1 mol/L sodium hydroxide VS = 60. is odorless or has a slightly characteristic odor.0 mL of standard lead solution by adding 2. weigh accurately again. Agar is practically insoluble in organic solvents. Prepare the control solution with 2.KP VIII 1141 residue in 2 mL of dilute acetic acid and water to make 50 mL and perform the test. add 500 mL of water. Identification (1) Heat 3 g of Aluminum Monostearate with 30 mL of hydrochloric acid on a water-bath with occasional shaking for 10 minutes. add sodium hydroxide TS until the solution becomes slightly turbid and filter: the filtrate responds to the Qualitative Tests for aluminum salt.5%.42). which does not melt below 85 o C . heat to boiling.5 g of Glacial Acetic Acid. light and pliable.0 mL of dilute acetic acid and water to make 50 mL (not more than 10 ppm). then add 30 mL of water and titrate with 1 mol/L sodium hydroxide VS (indicator: 2 drops of phenolphthalein TS).5 g of Agar. resilient gel. Identification (1) Take a fragment of Agar and add drop-wise iodine TS: a dark blue to reddish purple color develops.0 mg. externally. Description Aluminum Monostearate is a white to yellowish white powder. boil for 15 minutes and add water to make exactly 500 mL. shake well. Acid-insoluble Ash Not more than 0. (2) Wash the ether layer separated in (1) twice with 20 mL volumes of water and evaporate the ether layer on a water-bath: the residue melts at above 54 o C (Method 2). Acid Value for Fatty Acid Between 193 and 210. add water to make 100 mL. (5) Non-volatile residue⎯Evaporate 10 mL of Glacial Acetic Acid on a water-bath to dryness and dry at 105 °C for 1 hour: the residue is not more than 1. Perform a blank determination and make any necessary correction. Prepare the control solution with 2.0 mg. wash the vessel and the filter paper with a small amount of a mixture of neutralized ethanol and ether (1 : 1).1 mL of 0. combine the washings with the filtrate. add water to make 5 mL and perform the test (not more than 2 ppm). continue the heating and gradually raising the temperature to ash. to the Qualitative Tests (1).5% and not more than 101. Add 55 mL of ethanol and titrate with 0. filter through dry filter paper.1142 Monographs.5 mL of nitric acid. Aluminum Potassium Sulfate Hydrate is freely soluble in water and practically insoluble in ethanol or ether. pH 4.8. Add drop-wise 0. filter. combine the filtrate and the washings and add 2.1 mol/L potassium hydroxide VS: a red color develops. Purity (1) Free fatty acid⎯Mix 1. Assay Weigh accurately about 1. Part II under the Fats and Fatty Oils. strongly astringent taste. boil for 5 minutes and cool. evaporate on a water-bath by heating and then heat strongly between 900 o C and 1100 o C to a constant weight. combine the filtrate and the washing and add 2 mL of dilute acetic acid and water to make 50 mL. Perform the test. (2) Water-soluble salts⎯Heat 2. add water to make 100 mL.0% of Aluminum Potassium Sulfate Hydrate [AlK(SO4)2·12H2O].0 g of Aluminum Monostearate over a small flame with caution at the beginning.0 g of Aluminum Monostearate with 2 g of magnesium nitrate.0 g of Aluminum Monostearate with 80 mL of water in a loosely stoppered Erlenmeyer flask on a water-bath for 30 minutes with occasional shaking. Aluminum Potassium Sulfate Hydrate Alum Aluminum potassium Sulfate AlK(SO4)2·12H2O: 474. (3) Arsenic⎯Prepare the test solution with 0. Amount (mg) of aluminum (Al) = amount (mg) of aluminum oxide (Al2O3) × 0. Prepare the control solution with 2.0 mL of standard iron solution (not more than 20 ppm).5293 Each mL of 0. moisten the residue after cooling with 0. Evaporate 10 mL of diluted hydrochloric acid (1 in 2) on a water-bath to dryness. 105 3 hours). Identification A solution of Aluminum Potassium Sulfate Hydrate (1 in 10) responds to the Qualitative Tests for aluminum salt. Description Aluminum Potassium Sulfate Hydrate is a colorless or white crystals or powder. Purity (1) Heavy metals⎯Proceed with 1. ignite gently to ash and cool. add exactly 30 mL of 0. Cool. ignite over a small flame. (4) Arsenic⎯Mix 1.05 mol/L zinc acetate VS (indicator: 2 mL of dithizone TS). After cooling. weigh rapidly the ignited residue and designate the mass as aluminum oxide (Al2O3: 101.0 mL of standard lead solution (not more than 20 ppm). add 2 mL of dilute acetic acid and 5. Loss on Drying Not more than 3.0 g of Aluminum Monostearate. Packaging and Storage Preserve in tight containers.0 g of Aluminum Potassium Sulfate Hydrate according to Method 1 and perform the test.719 mg of AlK(SO4)2·12H2O Packaging and Storage Preserve in well-closed containers.0 g of Aluminum Monostearate with about 50 mL of a mixture of neutralized ethanol and ether (1 : 1).3 ppm).6 g of Aluminum Potassium Sulfate Hydrate. After cooling.5 mL of nitric acid and heat. wash the residue with a small amount of water. A solution of Aluminum Potassium Sulfate Hydrate (1 in 20) is acid. filter through dry filter paper. Heat again the residue with 10 mL of dilute sulfuric acid until white fumes evolve. wash the residue with water. o C.5 g of Aluminum Potassium Sulfate Hydrate and dissolve in water to make exactly 200 mL. previously dried. evaporate on a water-bath and boil the residue with 20 mL of water for 1 minute. (3) Heavy metals⎯Heat 1. until the color of the solution changes from light dark green to pale red. evaporate 50 mL of this solution on a water-bath and ignite at 600 o C : the residue is not more than 10.0 g of Aluminum Potassium Sulfate Hydrate according to Method 1 and perform the test according to Method A. add 10 mL of diluted hydrochloric acid (1 in 2). is odorless and has a slightly sweet. .0 mL of standard lead solution.05 mol/L disodium ethylenediaminetetraacetate VS and 20 mL of acetic acidammonium acetate buffer solution. Assay Weigh accurately about 4.96). (3) and (4) for potassium salt and to the Qualitative Tests (1) and (3) for sulfate. After cooling.39 Aluminum Potassium Sulfate Hydrate contains not less than 99. according to Method 1 and perform the test (not more than 3. (2) Iron⎯Prepare the test solution with 1. Pipet exactly 20 mL of this solution.05 mol/L disodium ethylenediaminetetraacetate VS = 23. dilute with water to make 50 mL and use this solution as the control solution (not more than 50 ppm).0% (1 g. KP VIII 1143 Dried Aluminum Potassium Sulfate Burnt Alum Dried Aluminum Potassium Sulfate, when dried, contains not less than 98.0% and not more than 101.0% of Aluminum Potassium Sulfate [AlK(SO4)2]. Description Dried Aluminum Potassium Sulfate is a white mass or white powder, is odorless and has a slightly sweet, astringent taste. Dried Aluminum Potassium Sulfate is freely soluble in hot water and practically insoluble in ethanol. Dried Aluminum Potassium Sulfate dissolves slowly in water. Identification A solution of Dried Aluminum Potassium Sulfate (1 in 20) responds to the Qualitative Tests for aluminum salt, to the Qualitative Tests (1), (3) and (4) for potassium salt and to the Qualitative Tests (1) and (3) for sulfate. Purity (1) Water-insoluble substances⎯Take 2.0 g of Dried Aluminum Potassium Sulfate, add 40 mL of water, shake frequently and allow to stand for 48 hours. Collect the insoluble residue on a glass filter (G4), wash with 50 mL of water and dry at 105 o C for 2 hours: the residue is not more than 50 mg. (2) Heavy metals⎯Dissolve 0.5 g of Dried Aluminum Potassium Sulfate in 45 mL of water and filter, if necessary. Add 2 mL of dilute acetic acid and water to make 50 mL. Perform the test using this solution as the test solution. Prepare the control solution with 2.0 mL of standard lead solution, 2 mL of dilute acetic acid and water to make 50 mL (not more than 40 ppm). (3) Iron⎯Prepare the test solution with 0.54 g of Dried Aluminum Potassium Sulfate according to Method 1 and perform the test according to Method A. Prepare the control solution with 2.0 mL of standard iron solution (not more than 37 ppm). (4) Arsenic⎯Prepare the test solution with 0.40 g of Dried Aluminum Potassium Sulfate according to Method 1 and perform the test (not more than 5 ppm). Loss on Drying Not more than 15.0% (2 g, 200 °C, 4 hours). Assay Weigh accurately about 1.2 g of Dried Aluminum Potassium Sulfate, previously dried, add 80 mL of water and heat on a water-bath with occasional shaking for 20 minutes. Cool and add water to make exactly 100 mL and filter, if necessary. Discard the first 30 mL of the filtrate, take exactly the subsequent 20 mL of the filtrate and proceed as directed in the Assay under Aluminum Potassium Sulfate Hydrate. Each mL of 0.05 mol/L disodium ethylenediaminetetraacetate VS = 12.910 mg of AlK(SO4)2 Packaging and Storage Preserve in tight containers. AlK(SO4)2: 258.21 Light Anhydrous Silicic Acid Light Anhydrous Silicic Acid contains not less than 98.0% and not more than 101.0% of silicon dioxide (SiO2: 60.08), calculated on the incinerated basis. Description Light Anhydrous Silicic Acid is a white to bluish white, light, fine power, is odorless, tasteless and smooth to the touch. Light Anhydrous Silicic Acid is practically insoluble in water, in ethanol, or in ether. Light Anhydrous Silicic Acid dissolves in hydrofluoric acid, in potassium hydroxide TS or in hot sodium hydroxide TS and does not dissolve in dilute hydrochloric acid. Identification (1) Dissolve 0.1 g of Light Anhydrous Silicic Acid in 20 mL of sodium hydroxide TS by boiling and add 12 mL of ammonium chloride TS: a white, gelatinous precipitate is produced and the precipitate does not dissolve in dilute hydrochloric acid. (2) Take the precipitate obtained in (1), add 10 mL of a solution of methylene blue (1 in 10000) and wash with water: the precipitate has a blue color. (3) Prepare a bead by fusing dibasic sodium ammonium phosphate on a platinum loop. Bring the hot, transparent bead into contact with Light Anhydrous Silicic Acid and fuse again: an insoluble matter is perceptible in the bead. The resulting bead, upon cooling, becomes opaque and acquires a reticulated appearance. Purity (1) Chloride⎯Dissolve 0.5 g of Light Anhydrous Silicic Acid in 20 mL of sodium hydroxide TS by boiling, cool, filter, if necessary and wash with 10 mL of water. Combine the filtrate and washings, add 18 mL of dilute nitric acid, shake and add water to make 50 mL. Perform the test. Prepare the control solution as follows: to 0.15 mL of 0.01 mol/L hydrochloric acid VS, add 20 mL of sodium hydroxide TS, 18 mL of dilute nitric acid and add water to make 50 mL (not more than 0.011%). (2) Heavy metals⎯Dissolve 0.5 g of Light Anhydrous Siliclc Acid in 20 mL of sodium hydroxide TS by boiling, cool, add 15 mL of acetic acid, shake, filter, if necessary, wash with 10 mL of water, combine the filtrate and washings and add water to make 50 mL. Perform the test. Prepare the control solution as follows: add acetic acid to 20 mL of sodium hydroxide TS and 1 drop of phenolphthalein TS until the color of this solution disappears, add 2.0 mL of standard lead solution, 2 mL of dilute acetic acid and water to make 50 mL and use this solution as the control solution (not more than 40 ppm). 1144 Monographs, Part II (3) Aluminum⎯Dissolve 0.5 g of Light Anhydrous Silicic Acid in 40 mL of sodium hydroxide TS by boiling, cool, add sodium hydroxide TS to make 50 mL and filter. Measure 10 mL of the filtrate, add 17 mL of acetic acid, shake, add 2 mL of aluminon TS and water to make 50 mL and allow to stand for 30 minutes: the color of this solution is not more intense than that of the following control solution. Control solution⎯Dissolve 0.176 g of potassium aluminum sulfate in water and add water to make 1000 mL. To 15.5 mL of this solution, add 10 mL of sodium hydroxide TS, 17 mL of acetic acid, 2 mL of aluminon TS and water to make 50 mL. (4) Iron⎯Take 40 mg of Light Anhydrous Silicic Acid, add 10 mL of dilute hydrochloric acid and heat for 10 minutes in a water-bath while shaking. After cooling, add 0.5 g of L-tartaric acid and dissolve L-tartaric acid with shaking. Prepare the test solution with this solution according to Method 2 and perform the test according to Method B. Prepare the control solution with 2.0 mL of standard iron solution (not more than 500 ppm). (5) Calcium⎯Dissolve 1.0 g of Light Anhydrous Silicic Acid in 30 mL of sodium hydroxide TS by boiling, cool, add 20 mL of water, 1 drop of phenolphthalein TS and dilute nitric acid until the color of this solution disappears, immediately add 5 mL of dilute acetic acid, shake, add water to make 100 mL and obtain a clear liquid by centrifugation or filtration. To 25 mL of this liquid, add 1 mL of oxalic acid TS and ethanol to make 50 mL, immediately shake and allow to stand for 10 minutes: the turbidity of this solution is not more intense than that of the following control solution. Control solution⎯Dissolve 0.250 g of calcium carbonate, previously dried at 180 o C for 4 hours, in 3 mL of dilute hydrochloric acid and add water to make 100 mL. To 4 mL of this solution, add 5 mL of dilute acetic acid and water to make 100 mL. To 25 mL of this solution, add 1 mL of oxalic acid TS and ethanol to make 50 mL and shake. (6) Arsenic⎯Dissolve 0.40 g of Light Anhydrous Silicic Acid in 10 mL of sodium hydroxide TS by boiling in a porcelain crucible, cool, add 5 mL of water and 5 mL of dilute hydrochloric acid, shake and perform the test (not more than 5 ppm). Loss on Drying Not more than 7.0% (1 g, 105 4 hours). Loss on Ignition Not more than 12.0% (1 g, 850 to 900 o C , constant weight). o C, o C Volume Test Weigh 5.0 g of Light Anhydrous Silicic Acid, transfer gradually to a 200 mL measuring cylinder and allow to stand: the volume is not less than 70 mL. Assay Weigh accurately about 1.0 g of Light Anhydrous Silicic Acid, add 20 mL of hydrochloric acid and evaporate to dryness on a sand-bath. Moisten the residue with hydrochloric acid, evaporate to dryness and heat between 110 o C and 120 o C for 2 hours. Cool, add 5 mL of dilute hydrochloric acid and heat. Allow to cool to room temperature, add 20 mL to 25 mL of hot water, filter rapidly and wash the residue with warm water until the last washing becomes negative to the Qualitative Tests (2) for chloride. Transfer the residue together with the filter paper to a platinum crucible, ignite to ash and continue the ignition for 30 minutes. Cool, weigh the crucible and designate the mass as a (g). Moisten the residue in the crucible with water, add 6 mL of hydrofluoric acid and 3 drops of sulfuric acid and evaporate to dryness. Heat strongly for 5 minutes, cool, weigh the crucible and designate the mass as b (g). Amount (g) of silicon dioxide (SiO2) = a − b Packaging and Storage Preserve in tight containers. Apricot Kernel Water Apricot Kernel Water contains not less than 0.09% and not more than 0.11% of hydrogen cyanide (HCN: 27.03). Method of Preparation Prepare by one of the following methods. (1) Take Apricot Kernels, previously crushed and pressed to remove fixed oils as much as possible, add a suitable amount of Water or Purified Water, and carry out steam distillation. Determine the amount of hydrogen cyanide in the distillate by the method as directed in the Assay, and carry on the distillation until the content of hydrogen cyanide in the distillate is about 0.14%. To the distillate, add ethanol of about 1/3 of the volume of the distillate, and dilute with a mixture of purified water and ethanol (3 : 1) until the content of hydrogen cyanide meets the specification. (2) Dissolve 7.5 mL of freshly prepared mandelonitrile in 1000 mL of a mixture of Purified Water and Ethanol (3 : 1), mix well, and filter. Determine the amount of hydrogen cyanide in the solution as directed in the Assay, and, if the amount is more than that specified above, dilute the solution to the specified concentration by the addition of the mixture of Purified Water and Ethanol (3 : 1). Description Apricot Kernel Water is a clear, colorless or pale yellow liquid, has an odor of benzaldehyde and characteristic taste. pH—Between 3.5 and 5.0. Identification Take 2 mL of Apricot Kernel Water, add 1 mL of ammonia TS, and allow to stand for 10 minutes: a slight turbidity is produced. Alow to stand for 20 minutes: the turbidity becomes more intense. KP VIII 1145 Specific Gravity 20 : d 20 Between 0.986 and 0.978. Saponification Value Between 193 and 200. Purity (1) Sulfate—Add a few drops of 0.1 mol/L sodium hydroxide VS to 5.0 mL of Apricot Kernel Water to make slightly alkaline, evaporate on a water-bath to dryness, and ignite between 450 o C and 550 o C . Dissolve the residue in 1 mL of dilute hydrochloric acid, and add water to make 50 mL. Perform the test using this solution as the test solution. Prepare the control solution with 0.50 mL of 0.005 mol/L sulfuric acid VS (not more than 0.005%). (2) Heavy metals—Evaporate 50 mL of Apricot Kernel Water on a water-bath to dryness, ignite between 450 o C and 550 o C , dissolve the residue in 5 mL of dilute acetic acid with warming, add water to make exactly 50 mL, and filter. Discard the first 10 mL of the filtrate, dilute the subsequent 20 mL to 50 mL with water, and perform the test using this solution as the test solution. Prepare the control solution with 2.0 mL of standard lead solution, adding 2 mL of dilute acetic acid and water to make 50 mL (not more than 1ppm). (3) Free hydrogen cyanide—Take 10 mL of Apricot Kernel Water, add 0.8 mL of 0.1 mol/L silver nitrate VS and 2 to 3 drops of nitric acid at 15 o C , filter, and add 0.1 mol/L silver nitrate VS to the filtrate: no change occurs. (4) Residue on evaporation—Evaporate 5.0 mL of Apricot Kernel water to dryness, and dry: the residue is not more than 1.0 mg. Acid Value Not more than 2.0. Assay Take exactly 25 mL of Apricot Kernel Water, add 100 mL of water, 2 mL of potassium iodide TS and 1 mL of ammonia TS, and titrate with 0.1 mol/L silver nitrate VS until a yellow turbidity persists. Packaging and Storage Preserve in well-closed containers. Each mL of 0.1 mol/L silver nitrate VS = 5.405 mg of HCN White Beeswax Packaging and Storage tight containers. Preserve in light-resistant, Beef Tallow Beef Tallow is a purified fat obtained by wet steam rendering from the fresh fatty tissues of Bos taurus Linné var. domesticus Gmelin (Bovidae). Description Beef Tallow is a white, uniform mass, has characteristic odor and mild taste. Beef Tallow is freely soluble in ether or in petroleum ether, very slightly soluble in ethanol and practically insoluble in water. Beef Tallow is breakable at a low temperature, but softens above 30 o C . Melting point—Between 42 o C and 50 o C (Method 2). Iodine Value Between 33 and 50 (When the sample is insoluble in 20 mL of cyclohexane, dissolve it by shaking a glass-stoppered flask in warm water. If it is still insoluble, increase the volume of solvent.). Purity (1) Moisture and coloration⎯Take 5.0 g of Beef Tallow and melt by heating on a water-bath: the melting solution is clear and no water separates from the melting solution. And observe the melting solution in a 10-mm thick layer of the liquid: it is colorless or slightly yellow. (2) Alkali⎯Take 2.0 g of Beef Tallow, add 10 mL of water, melt by heating on a water-bath and shake vigorously. After cooling, add 1 drop of phenolphthalein TS to the separated water layer: no color develops. (3) Chloride⎯Take 1.5 g of Beef Tallow, add 30 mL of ethanol, boil for 10 minutes under a reflux condenser and filter after cooling. To 20 mL of the filtrate, add 5 drops of a solution of silver nitrate in ethanol (1 in 50): the turbidity of the mixture is not more than that of the following control solution. Control solution⎯Take 1.0 mL of 0.01 mol/L hydrochloric acid VS, add ethanol to make 20 mL and add 5 drops of the solution of silver nitrate in ethanol (1 in 50) White Beeswax is bleached Yellow Beeswax. Description White Beeswax is a white to yellowish white mass and has a characteristic odor. White Beeswax is slightly soluble in ether and practically insoluble in water or in dehydrated ethanol. White Beeswax is comparatively brittle when cooled and the fractured surface is granular and non-crystalline. Saponification Value Between 80 and 100. Weigh accurately about 3.0 g of White Beeswax, place in a 250 mL glass-stoppered flask and add 25 mL of 0.5 mol/L potassium hydroxide-ethanol VS and 50 mL of ethanol, heat for 4 hours on a water-bath under a reflux condenser and proceed as directed in the Saponification value under the Fats and Fatty Oils. Acid Value Between 5 and 9 or between 17 and 22. Weigh accurately about 6 g of White Beeswax, place in a glass-stoppered 250 mL flask and add 50 mL of dehydrated ethanol. Warm the mixture to dissolve the wax, 1146 Monographs, Part II add 1 mL of phenolphthalein TS and proceed as directed in the Acid value under the Fats and Fatty Oils. Perform a blank determination using solvent which is not previously neutralized and make any necessary correction. Melting Point 2). Between 60 o C and 67 o C (Method Purity Paraffin, fat, Korea wax or resin⎯Melt Yellow Beeswax at the lowest possible temperature, drip the liquid into a glass vessel containing ethanol to form granules and allow then to stand in air for 24 hours, Drop the granules into two mixtures of ethanol and water, one adjusted so as to have a specific gravity of 0.95 and the other 0.97: the granules sink or are suspended in the mixture with the specific gravity of 0.95 and float or are suspended in the other mixture. Packaging and Storage Preserve in well-closed containers. Yellow Beeswax Cera Flava Yellow Beeswax is the purified wax obtained from honeycombs such as those of Apis indica Radoszkowski or Apis mellifera Linné (Apidae). Description Yellow Beeswax is a pale yellow to brownish yellow mass, and has a characteristic odor, which is not rancid. Yellow Beeswax is comparatively brittle when cooled and the fractured surface is granular and non-crystalline. Saponification Value Between 80 and 100. Weigh accurately about 3 g of Yellow Beeswax, place in a 259-mL stoppered flask and add 25 mL of 0.5 mol/L potassium hydroxide-ethanol VS and 50 mL of ethanol, insert a reflux condenser, heat for 4 hours on a waterbath and proceed as directed in the Saponification value under the Fats and Fatty Oils. Acid Value Between 5 and 9 or Between 17 and 22. Weigh accurately about 6 g of Yellow Beeswax, place in a glass-stoppered 250-mL flask and add 50 mL of dehydrated ethanol. Warm the mixture to dissolve the wax, add 1 mL of phenolphthalein TS and proceed as directed in the Acid value under the Fats and Fatty Oils. Perform a blank determination using solvent which is not previously neutralized and make any necessary correction. Melting Point thod 2). Between 60 o C and 67 o C (Me- Purity Paraffin, fat, Japan wax or resin⎯Melt Yel- low Beeswax at the lowest possible temperature, drip the liquid into a glass vessel containing ethanol to form granules and allow then to stand in air for 24 hours, Drop the granules into two mixtures of ethanol and water, one adjusted so as to have a specific gravity of 0.95 and the other 0.97, the granules sink or are suspended in the mixture with the specific gravity of 0.95 and float or are suspended in the other mixture. Packaging and Storage Preserve in well-closed containers. Bentonite Bentonite is a natural, colloidal, hydrated aluminum silicate. Description Bentonite is a very fine, white to pale yellow-brown powder, is odorless. Bentonite has a slightly earthy taste. Bentonite is practically insoluble in water or in ether. Bentonite swells in water. Identification (1) Add 0.5 g of Bentonite to 3 mL of diluted sulfuric acid (1 in 3) and heat until white fumes are evolved. Cool, add 20 mL of water and filter. To 5 mL of the filtrate, add 3 mL of ammonia TS: a white, gelatinous precipitate is produced, which turns red on the addition of 5 drops of alizarin S TS. (2) Wash the residue obtained in (1) with water, add 2 mL of methylene blue solution (1 in 10000) and wash again with water: the residue is blue. pH Take 1.0 g of Bentonite, add 50 mL of water and shake: the pH of the suspension is between 9.0 and 10.5. Purity (1) Heavy metals⎯Take 1.5 g of Bentonite, add 80 mL of water and 5 mL of hydrochloric acid and boil gently for 20 minutes with thorough stirring. Cool, centrifuge, collect the supernatant liquid, wash the residue twice with 10 mL volumes of water and centrifuge. Combine the supernatant liquid and the washings and add drop-wise strong ammonia water. When a precipitate is produced, add drop-wise dilute hydrochloric acid with vigorous stirring and dissolve. To the solution, add 0.45 g of hydroxylamine hydrochloride and heat. Cool and add 0.45 g of sodium acetate, 6 mL of dilute acetic acid and water to make 150 mL. Pipet 50.0 mL, use this solution as the test solution and perform the test. Prepare the control solution as follows: to 2.5 mL of standard lead solution, add 0.15 g of hydroxylamine hydrochloride, 0.15 g of sodium acetate and 2 mL of dilute acetic acid and add water to make 50 mL (not more than 50 ppm). (2) Arsenic⎯Take 1.0 g of Bentonite, add 5 mL of dilute hydrochloric acid and gently heat to boil while stirring well. Cool immediately and centrifuge. To the residue, add 5 mL of dilute hydrochloric acid, shake well KP VIII 1147 and centrifuge. To the residue, add 10 mL of water and perform the same operations. Combine all the extracts and heat on a water-bath to concentrate to 5 mL. Perform the test(not more than 2 ppm). (3) Foreign matter⎯Place 2.0 g of Bentonite in a mortar, add 20 mL of water to swell, disperse evenly with a pestle and add water to make 100 mL. Pour the suspension through a No. 200 (74 μm) sieve and wash the sieve thoroughly with water: no grit is felt when the fingers are rubbed over the wire mesh of the sieve. Loss on Drying o C , 2 hours). Between 5.0% and 10.0% (2 g, 105 Gel Formation Mix 6.0 g of Bentonite with 0.30 g of magnesium oxide. Add the mixture, in several volumes, to 200 mL of water contained in a glass-stoppered 500 mL cylinder. Agitate for 1 hour, transfer 100 mL of the suspension to a 100 mL mass cylinder and allow to stand for 24 hours: not more than 2 mL of supernatant appears on the surface. Swelling Power Weigh 2.0 g of Bentonite, add to 100 mL of water in a glass-stoppered 100 mL cylinder, in ten volumes, allowing each volume to settle before adding the next and allow to stand for 24 hours: the apparent volume of the sediment at the bottom is not less than 20 mL. Packaging and Storage Preserve in well-closed containers. Benzyl Alcohol CH2OH C7H8O: 108.14 Benzyl Alcohol contains not less than 98.0% and not more than 100.5% of benzyl alcohol (C7H8O). The label states, where applicable, that it is suitable for the manufacture of injection forms. Description Benzyl Alcohol is a clear, colorless liquid. Benzyl Alcohol is miscible with ethanol, with fatty oils and with essential oils. Benzyl Alcohol is soluble in water. 20 Specific gravity d 20 : Between 1.043 and 1.049. Identification Determine the infrared spectra of Benzyl Alcohol and Benzyl Alcohol RS, both previously dried, as directed in the liquid film method under the Infrared Spectrophotometry: both spectra exhibit similar intensities of absorption at the same wavenumbers. Refractive Index nD20 : Between 1.538 and 1.541. Purity (1) Clarity and color of solution⎯Dissolve 2.0 mL of Benzyl Alcohol in 60 mL of water: the solution is clear and colorless. (2) Acid⎯Take 10 mL of Benzyl Alcohol, add 10 mL of neutralized ethanol, 2 drops of phenolphthalein TS and 1.0 mL of 0.1 mol/L sodium hydroxide VS: a red color develops. (3) Benzaldehyde and other related substances⎯ Use Benzyl Alcohol as the test solution. Separately, weigh exactly 0.750 g of benzaldehyde and 0.500 g of cyclohexylmethanol, add Benzyl Alcohol to make exactly 25 mL. Pipet 1 mL of this solution, add exactly 2 mL of the ethylbenzene internal standard solution and exactly 3 mL of the dicyclohexyl internal standard solution, add Benzyl Alcohol to make exactly 20 mL and use this solution as the standard solution (1). Perform the test with 0.1 µL each of the test solution and standard solution (1) as directed under the Gas Chromatography according to the following operating conditions: no peak of ethylbenzene or dicyclohexyl appears in the chromatogram obtained from the test solution. Proceed with injection of 0.1 µL of the standard solution (1) and adjust the sensitivity of the detector so that the peak height of ethylbenzene is not more than 30% of the full scale of the recorder. The peak area of benzaldehyde obtained from the test solution is not more than the difference between the peak areas of benzaldehyde of the test solution and the standard solution (1) (0.15%), and the peak area of cyclohexylmethanol from the test solution is not more than the difference between the peak areas of cyclohexylmethanol of the test solution and the standard solution (1) (0.10%). The total area of the peaks having the retention time smaller than benzyl alcohol and other than benzaldehyde and cyclohexylmethanol obtained from the test solution is not more than 4 times the peak area of ethylbenzene obtained from the standard solution (1) (0.04%). The total area of the peaks having the retention time larger than benzyl alcohol obtained from the test solution is not more than the peak area of dicyclohexyl from the standard solution (1) (0.3%). Disregard any peak having the area not more than 1/100 times the peak area of ethylbenzene from the standard solution (1) for these calculations. Benzyl Alcohol labeled that it is suitable for use in the manufacture of injection forms meets the following requirements. Use Benzyl Alcohol as the test solution. Separately, weigh exactly 0.250 g of benzaldehyde and 0.500 g of cyclohexylmethanol, and add Benzyl Alcohol to make exactly 25 mL. Pipet 1 mL of this solution, add exactly 2 mL of the ethylbenzene internal standard solution and exactly 2 mL of the dicyclohexyl internal standard solution, then add Benzyl Alcohol to make exactly 20 mL, and use this solution as the standard solution (2). Perform the test with 0.1 µL each of the test solution and standard solution (2) as directed under the Gas Chromatography according to the following operating conditions: no peak of ethylbenzene or dicyclohexyl ap- 1148 Monographs, Part II pears on the chromatogram obtained from the test solution. Proceed with injection of 0.1 µL of the standard solution (2) and adjust the sensitivity of the detector so that the peak height of ethylbenzene is not more than 30% of the full scale of the recorder. The peak area of benzaldehyde of obtained from the test solution is not more than the difference between the peak areas of benzaldehyde of the test solution and the standard solution (2) (0.05%), and the peak area of cyclohexylmethanol from the test solution is not more than the difference between the peak areas of cyclohexylmethanol of the test solution and the standard solution (2) (0.10%). The total area of the peaks having the retention time smaller than benzyl alcohol and other than benzaldehyde and cyclohexylmethanol obtained from the test solution is not more than 2 times the peak area of ethylbenzene from the standard solution (2) (0.02%). The total area of the peaks having the retention time larger than benzyl alcohol obtained from the test solution is not more than the peak area of dicyclohexyl from the standard solution (2) (0.2%). Disregard any peak having the area not more than 1/100 times the peak area of ethylbenzene from the standard solution (2) for these calculations. Ethylbenzene internal standard solution⎯Dissolve exactly 0.100 g of ethylbenzene in Benzyl Alcohol to make exactly 10 mL. Pipet 2 mL of this solution and add Benzyl Alcohol to make exactly 20 mL. Dicyclohexyl internal standard solution⎯Dissolve exactly 2.000 g of dicyclohexyl in Benzyl Alcohol to make exactly 10 mL. Pipet 2 mL of this solution, and add Benzyl Alcohol to make exactly 20 mL. Operating conditions Detector: A hydrogen flame ionization detector Column: A fused silica column about 0.32 mm in inside diameter and about 30 m in length, coated inside with polyethylene glycol 20 M for gas chromatography in 0.5 µm thickness. Column temperature: Raise the temperature at a rate of 5 o C per minutes from 50 o C to 220 o C , and maintain at 220 o C for 35 minutes. Temperature of injection port: A constant temperature of about 200 o C . Temperature of detector: A constant temperature of about 310 o C . Carrier gas: Helium Flow rate: Adjust the flow rate so that the retention time of benzyl alcohol is between 24 and 28 minutes. Split ratio: Splitless System suitability System performance: When the procedure is run with the standard solution (1) under the above operating conditions, the relative retention times of ethylbenzene, dicyclohexyl, benzaldehyde and cyclohexylmethanol with respect to benzyl alcohol are about 0.28, about 0.59, about 0.68 and about 0.71, respectively, with the resolution between the peaks of benzaldehyde and cyclohexylmethanol being not less than 3.0. In the case of Benzyl Alcohol labeled to use for injection, proceed with the standard solution (2) instead of the standard solution (1). (4) Peroxide value—Dissolve 5 g of Benzyl Alcohol, accurately weighed, in 30 mL of a mixture of glacial acetic acid and chloroform (3 : 2) in a glass-stoppered conical flask. Add 0.5 mL of potassium iodide saturated solution, shake exactly for 1 minute, add 30 mL of water, and titrate with 0.01 mol/L sodium thiosulfate VS until the blue color of the solution disappears after addition of 10 mL of starch TS near the end point where the solution is a pale yellow color. Perform a blank determination and make any necessary correction. Calculate the amount of peroxide by the following formula: not more than 5. [10 × (VI − V0 )] W VI : Volume (mL) of 0.01 mol/L sodium thiosulfate VS consumed in the test V 0 : Volume (mL) of 0.01 mol/L sodium thiosulfate VS consumed in the blank V : Amount (g) of Benzyl Alcohol taken Amount (mEq/kg) of peroxide = (5) Residue on evaporation—Perform the test after confirmation that the test specimen meets the requirement of the peroxide value. Transfer 10.0 g of Benzyl Alcohol to a porcelain or quartz crucible or platinum dish, previously weighed accurately, and heat on a hotplate at not exceeding 200 o C , taking care to avoid boiling, to evaporate to dryness. Dry the residue on the hot -plate for 1 hour, and allow to cool in a desiccator: not more than 5 mg. Assay Weigh accurately about 0.9 g of Benzyl Alcohol, add exactly 10 mL of a mixture of pyridine and acetic anhydride (17 : 3) and heat in a water-bath under a reflux condenser for 30 minutes. Cool, add 25 mL of water and titrate the excess acetic acid with 1 mol/L sodium hydroxide VS (indicator: 2 drops of phenolphthalein TS). Perform a blank determination and make any necessary correction. Each mL of 1 mol/L sodium hydroxide VS = 108.14 mg of C7H8O Packaging and Storage tight containers. Preserve in light-resistant, Benzyl Benzoate COOCH2 C14H12O2: 212.24 Benzyl Benzoate contains not less than 99.0% and not KP VIII 1149 more than 101.0% of benzyl benzoate (C14H12O2). o Description Benzyl Benzoate is a colorless, clear, viscous liquid, has a faint, aromatic odor and a pungent, burning taste. Benzyl Benzoate is practically insoluble in water. Benzyl Benzoate is miscible with ethanol or ether. Boiling point⎯About 323 o C . Congealing point⎯About 17 o C . 20 Specific gravity⎯ d 20 : about 1.123. Identification (1) Heat gently 1 mL of Benzyl Benzoate with 5 mL of sodium carbonate TS and 2 mL of potassium permanganate TS: the odor of benzaldehyde is perceptible. (2) Warm the titrated mixture obtained in the Assay on a water-bath to remove ethanol and add 0.5 mL of ferric chloride TS: a pale yellow-red precipitate is produced, which turns white on the addition of dilute hydrochloric acid. Refractive Index nD20 : Between 1.568 and 1.570. Purity Acid⎯Dissolve 5.0 mL of Benzyl Benzoate in 25 mL of neutralized ethanol and add 0.50 mL of 0.1 mol/L sodium hydroxide VS: a red color develops. Residue on Ignition Not more than 0.05% (2 g). Assay Weigh accurately about 2 g of Benzyl Benzoate, add 50.0 mL of 0.5 mol/L potassium hydroxideethanol VS and boil gently for 1 hour under a reflux condenser with a carbon dioxide-absorbing tube (soda lime). Cool and titrate the excess potassium hydroxide with 0.5 mol/L hydrochloric acid VS (indicator: 2 drops of phenolphthalein TS). Perform a blank determination and make any necessary correction. Each mL of 0.5 mol/L potassium hydroxide-ethanol VS = 106.12 mg of C14H12O2 Packaging and Storage Preserve in light resistant, tight containers. Cacao Butter Congealing point of the fatty acids⎯Between 45 C and 50 o C . Melting Point Between 31 o C and 35 o C (cram the test into a capillary tube without melting the test, then follow Method 2). Saponification Value Between 188 and 195. Specific Gravity 40 : Between 0.895 and 0.904. d 20 Acid Value Not more than 3.0. Iodine Value Between 35 and 43. Packaging and Storage Preserve in well-closed containers. Camellia Oil Camellia Oil is the fixed oil obtained from the peeled seeds of Camellia japonica Linné or other allied plants (Theaceae). Description Camellia Oil is a colorless or pale yellow, clear oil, is nearly odorless and tasteless. Camellia Oil is miscible with ether and petroleum ether. Camellia Oil slightly soluble in ethanol. Congealing point⎯Partially at -10 o C and completely -15 o C . 25 Specific gravity⎯ d 25 : Between 0.910 and 0.914. Identification Take 2 mL of Camellia Oil, add dropwise 10 mL of a mixture of fuming nitric acid, sulfuric acid and water (1 : 1 : 1), previously cooled to room temperature: a bluish green color develops at the zone of contact. Saponification Value Between 188 and 194. Unsaponifiable Matters Not more than 1.0%. Acid Value Not more than 2.8. Iodine Value Between 78 and 83. Oleum Cacao Packaging and Storage Preserve in tight containers. Cacao Butter is the fat obtained from the seed of Theobroma cacao Linné (Sterculiaceae). Description Cacao Butter is yellowish white, hard, brittle mass, has slight, chocolate-like odor and has no odor of rancidity. Cacao Butter is freely soluble in ether or in chloroform, soluble in boiling dehydrated ethanol and very slightly soluble in ethanol. Capsules Capsules are made of gelatin or a suitable material and their shape is a pair of cylinders with one end closed which can be overlapped on each other. 1150 Monographs, Part II Method of Preparation Dissolve Gelatin or the like in water by warming, add Glycerin or D-Sorbitol, emulsifier, preservatives, coloring substances and so forth, if necessary, to make a thick gluey solution and form into capsules while warm. Capsules may be coated with a lubricant, if necessary. Description Capsules are odorless and elastic. Purity Odor, Solubility and acidity or alkalinity⎯Place, without overlapping of the parts, 1 piece (1 pair) of Capsules in a 100 mL Erlenmeyer flask, add 50 mL of water and shake often, keeping the temperature at 37 o C ± 2 o C . Perform this test 5 times: they all dissolve within 10 minutes and all these solutions are odorless and neutral or slightly acidic. Packaging and Storage Preserve in well-closed containers. Castor Oil Oleum Ricini Castor Oil is the fixed oil obtained by compression from the seeds of Ricinus Communis Linné (Euphorbiaceae). Description Castor Oil is a colorless or pale yellow, clear, viscous oil, has a slight, characteristic odor and has bland at first and afterwards slightly acrid taste. Castor Oil is miscible with dehydrated ethanol or ether. Castor Oil is freely soluble in ethanol and practically insoluble in water. When cooled to 0 o C , Castor Oil becomes more viscous and turbidity is gradually formed. Identification Take 3 g of Castor Oil, add 1 g of potassium hydroxide and heat the mixture carefully to fuse: a characteristic odor is perceptible. Dissolve the fused matter in 30 mL of water, add an excess of magnesium oxide and filter. Acidify the filtrate with hydrochloric acid: white crystals are produced. Saponification Value Between 176 and 187. Specific Gravity 25 : d 25 Between 0.953 and 0.965. Acid Value Not more than 1.5. Hydroxyl Value Between 155 and 177. Iodine Value Between 80 and 90. Purity Adulteration⎯Shake to mix 1.0 g of Castor Oil with 4.0 mL of ethanol: it dissolves clearly. Add 15 mL of ethanol more: no turbidity is produced. Packaging and Storage Preserve in tight containers. Calcium Hydroxide Slaked Lime Ca(OH)2: 74.09 Calcium Hydroxide contains not less than 90.0% and not more than 101.0% of calcium hydroxide [Ca(OH)2]. Description Calcium Hydroxide is a white powder and has slightly bitter taste. Calcium Hydroxide is slightly soluble in water, very slightly soluble in boiling water and practically insoluble in ethanol or in ether. Calcium Hydroxide absorbs carbon dioxide from air. Calcium Hydroxide dissolves in dilute acetic acid, in dilute hydrochloric acid and in dilute nitric acid. Identification (1) Mix Calcium Hydroxide with 3 to 4 times its mass of water: the mixture is slushy and is alkaline. (2) Dissolve 1 g of Calcium Hydroxide in 30 mL of dilute acetic acid and boil. After cooling, neutralize with ammonia TS: the solution responds to the Qualitative Tests (2) and (3) for calcium salt. Purity (1) Acid-insoluble substances⎯Take 5 g of Calcium Hydroxide, add 100 mL of water, add hydrochloric acid drop-wise with stirring until the solution becomes acidic and further add 1 mL of hydrochloric acid. Boil this solution for 5 minutes, cool and filter through a tared glass filter (G4). Wash the residue with boiling water until the last washing exhibits no turbidity upon addition of silver nitrate TS and dry at 105 °C to constant weight: the amount is not more than 25 mg. (2) Heavy metals⎯Dissolve 1.0 g of Calcium Hydroxide in 10 mL of dilute hydrochloric acid, evaporate on a water-bath to dryness, dissolve the residue in 40 mL of water and filter. To 20 mL of the filtrate add 2 mL of dilute acetic acid and water to make 50 mL and perform the test. Prepare the control solution as follows: evaporate 5 mL of dilute hydrochloric acid on a water-bath to dryness and add 2 mL of dilute acetic acid, 2.0 mL of standard lead solution and add water to make 50 mL (not more than 40 ppm). (3) Magnesium and alkali metals⎯Dissolve 1.0 g of Calcium Hydroxide in a mixture of 20 mL of water and 10 mL of dilute hydrochloric acid, boil, neutralize with ammonia TS and precipitate calcium oxalate completely by adding drop-wise ammonium oxalate TS. Heat the mixture on a water-bath 1 hour, cool, add water to make 100 mL, shake and filter. To 50 mL of the filtrate, add 0.5 mL of sulfuric acid, evaporate to dryness and ignite at 600 °C to constant weight: the residue is not more than 24 mg. (4) Arsenic⎯Dissolve 0.5 g of Calcium Hydroxide Purity (1) Acid-insoluble substance⎯Dissolve 5. Dibasic Calcium Phosphate Hydrate is practically insoluble in water. Prepare the control solution by adding 10 mL of hydrochloric acid-ammonium acetate buffer solution. cool and add ammonia TS until precipitates begin to form in the solution. Prepare the control solution with 1.05 mol/L disodium ethylenediamine tetraacetate VS.02 mol/L zinc acetate VS (indicator: 25 mg of eriochrome black T-sodium chloride indicator). Each mL of 0. After cooling. collect the insoluble substance by filtration using filter paper for quantitative analysis. (5) Heavy metals⎯Dissolve 0.5. Pipet exactly 20 mL of this solution. (2) Dissolve 0. dissolve in 10 mL of dilute hydrochloric acid and add water to make 100 mL. Prepare the control solution with 0. add 90 mL of water and 1.7211 mg of CaHPO4 Packaging and Storage containers. (7) Arsenic⎯Dissolve 1. shake. add water to make 100 mL and filter. if necessary. Add 2 mL of potassium sulfate TS of the filtrate and allow to stand for 10 minutes: no turbidity is produced. Wash with water until no more turbidity of the washing is produced by adding silver nitrate TS.4 g of Dibasic Calcium Phosphate Hydrate.70 mL of 0. if necessary.0% and not more than 101. Dibasic Calcium Phosphate Hydrate dissolves in dilute hydrochloric acid or in dilute nitric acid. add water to make 100 mL and filter. crystalline powder. Assay Weigh accurately about 0. to 2.5 mL of 8 mol/L potassium hydroxide TS.KP VIII 1151 in 5 mL of dilute hydrochloric acid and perform the test (not more than 4 ppm). and add 2 mL of ammonium molybdate TS: a yellow precipitate is produced. Assay Weigh accurately about 1. is colorless and tasteless.0 g of Dibasic Calcium Phosphate Hydrate in 40 mL of water and 10 mL of hydrochloric acid and boil for 5 minutes.0 mL of this solution.0% (1 g. and water to make 50 mL and perform the test using this solution as the test solution. add exactly 25 mL of 0.0% of Dibasic Calcium Phosphate (CaHPO4: 136.0 mL of standard lead solution and add water to make 50 mL (not more than 31 ppm). pH 3. until the color of the solution changes from red-purple to blue.5 mL of ammonia TS dropwise with shaking and add 5 mL of ammonium oxalate TS: a white precipitate is produced. allow to stand for 3 minutes to 5 minutes and then add 0.0 g of Dibasic Calcium Phosphate Hydrate in 5 mL of water and 5 mL of dilute hydrochloric acid. Identification (1) Dissolve 0.1 g of NN indicator. Perform the test using this solution as the test solution. (4) Carbonate⎯Dissolve 1. if necessary.0 mL of diluted hydrochloric acid (1 in 6) by warming. pH 3. when dried.005 mol/L sulfuric acid (not more than 0. Dibasic Calcium Phosphate Hydrate CaHPO4·2H2O: 172. 3 hours).09 Dibasic Calcium Phosphate Hydrate. Take 30 mL of the filtrate and add 1 mL of dilute hydrochloric acid and add water to make 50 mL. Loss on Drying Between 19.0 g of Dibasic Calcium Phosphate Hydrate with 5 mL of water and add immediately 2 mL of hydrochloric acid: no foam is produced. pH 10. Perform the test using 50 mL of this solution as the test solution.65 g of Dibasic Calcium Phosphate Hydrate in a mixture of 5 mL of water and 5 mL of dilute hydrochloric acid by warming.7.05 mol/L disodium ethylenediamine tetraacetate VS = 3. warm for 1 to 2 minutes at 70 o C . Each mL of 0.5 g of Dibasic Calcium Phosphate Hydrate with 10 mL of water. (3) Sulfate⎯Dissolve by warming 1.0 g of Dibasic Calcium Phosphate Hydrate in 5 mL of dilute hydrochloric acid and perform the test with this solution as the test solution (not more than 2 ppm).5. Perform a blank determination and make any necessary correction.5 mg (not more than 0. Preserve in well-closed .02 mol/L disodium ethylenediaminetetraacetate VS. 50 mL of water and 5 mL of ammonia-ammonium chloride buffer solution.1 g of Dibasic Calcium Phosphate Hydrate in 5 mL of dilute nitric acid.02 mol/L disodium ethylendiaminetetraacetate VS = 2.160%).248%).5% and 22. 200 o C . (2) Chloride⎯Dissolve 0. add 2. Dissolve the precipitates by adding a small amount of dilute hydrochloric acid dropwise.1 g of Dibasic Calcium Phosphate Hydrate in 1. add 1 mL of hydrochloric acid dropwise with stirring and filter.0 g of Calcium Hydroxide. previously dried.06). Ignite to incinerate the residue and filter paper: the mass is not more than 2. Titrate immediately with 0. dissolve in 12 mL of dilute hydrochloric acid and add water to make exactly 200 mL.20 g of Dibasic Calcium Phosphate Hydrate in 20 mL of water and 13 mL of dilute nitric acid. contains not less than 98.01 mol/L hydrochloric acid (not more than 0. add 10 mL of hydrochloric acid-ammonium acetate buffer solution. (6) Barium⎯Heat 0. and titrate the excess disodium ethylenediaminetetraacetate with 0.7046 mg of Ca(OH)2 Packaging and Storage Preserve in tight containers. Piper 10. in ethanol or in ether.05%). Description Dibasic Calcium Phosphate Hydrate is white.0 mL of 0. 048%). contains not less than 90.0% (1 g. Prepare the control solution with 0.018%). if necessary. Description Anhydrous Dibasic Calcium Phosphate is a white.0 mL of 1 mol/L sodium hydroxide VS: the color changes to yellow.0% (1 g. previously dried. when dried. Heavy metals. add water to make 100 mL and filter.06 Anhydrous Dibasic Calcium Phosphate.005 mol/L sulfuric acid (not more than 0. (6) Arsenic⎯Dissolve 1. Perform the test using 50 mL of this solution as the test solution. Prepare the control solution with 0. Identification Proceed as directed in the Identification under Dibasic Calcium Phosphate Hydrate. Purity (1) Acid-insoluble substances and Chloride⎯Proceed as directed in the Purity (1) and (2) under Dibasic Calcium Phosphate Hydrate. Each mL of 0. in ethanol or in ether. Loss on Drying Not more than 3. if necessary. dissolve in 3 mL of dilute hydrochloric acid and add water to make exactly 100 mL. (2) Sulfates⎯Proceed as directed in the Purity (3) under Dibasic Calcium Phosphate Hydrate (not more than 0. Description Monobasic Calcium Phosphate Hydrate is white crystal or crystalline powder. add water to make exactly 100 mL and filter.0% and not more than 101. Part II luble in water and practically insoluble in ethanol or in ether. Monobasic Calcium Phosphate Hydrate is slightly deliquescent.5 mL of 0.0% of Monobasic Calcium Phosphate Hydrate [Ca(H2PO4)2·H2O]. Monobasic Calcium Phosphate Hydrate dissolves in dilute hydrochloric acid or in dilute nitric acid.7211 mg of CaHPO4 Purity (1) Clarity and color of solution⎯Dissolve 1. Assay Proceed as directed in the Assay under Dibasic Calcium Phosphate Hydrate. Monobasic Calcium Phosphate Hydrate Assay Weigh accurately about 0. Ca(H2PO4)2·H2O: 252. (3) Carbonate.07 Each mL of 0.02 mol/L disodium ethylenediaminetetraacetate VS = 2. Then add 1. (4) Sulfate⎯Dissolve 1.0 g of Monobasic Calcium Phosphate Hydrate in 20 mL of water and 1 mL of hydrochloric acid.041 mg of Ca(H2PO4)·2H2O Monobasic Calcium Phosphate.0% and not more than 101.25 mL of 0. silica gel. (5). Loss on Drying Not more than 1. Barium and Arsenic⎯Proceed as directed in the Purity (4).0 g of Monobasic Calcium Phosphate Hydrate with 3 mL of water and add 100 mL of water and 1 drop of methyl orange TS: a red color develops. Identification Proceed as directed in the Identification under Dibasic Calcium Phosphate Hydrate.200%). Anhydrous Dibasic Calcium Phosphate is practically insoluble in water.01 mol/L hydrochloric acid (not more than 0.0 g of Monobasic Calcium Phosphate Hydrate in 5 mL of dilute hydrochloric acid and perform the test (not more than 2 ppm). 200 3 hours).4 g of Monobasic Calcium Phosphate Hydrate.0 % of dibasic calcium phosphate (CaHPO4). Packaging and Storage Preserve in well-closed containers. when dried. (6) and (7) under Dibasic Calcium Phosphate Hydrate. 24 hours).0 g of Monobasic Calcium Phosphate Hydrate in 19 mL of water and 2 mL of diluted hydrochloric acid (3 in 4) and heat on a water-bath for 5 minutes with occasional shaking: the solution is clear and colorless.0 g of Monobasic Calcium Phosphate Hydrate in 20 mL of water and 12 mL of dilute nitric acid. is odorless and tasteless. Monobasic Calcium Phosphate Hydrate is sparingly so- Calcium Oxide . (5) Heavy metals⎯Proceed as directed in the Purity (5) under Dibasic Calcium Phosphate Hydrate. Packaging and Storage Preserve in tight containers.02 mol/L disodium ethylendiaminetetraacetate VS = 5. Anhydrous Dibasic Calcium Phosphate CaHPO4: 136. (2) Dibasic phosphate and acid⎯Triturate 1. crystalline powder or granule. (3) Chloride⎯Dissolve 1. odorless and has acid taste. Perform the test using 50 mL of this solution as the test solution. contains not less than 98. Anhydrous Dibasic Calcium Phosphate dissolves in dilute hydrochloric acid or in dilute nitric acid. Pipet exactly 20 mL of this solution and proceed as directed in the Assay under Dibasic Calcium Phosphate Hydrate.1152 Monographs. o C. 0% (1 g.1215 mg of CaO Packaging and Storage Preserve in tight containers. add water to make 200 mL. Loss on Ignition Not more than 10. Calcium Stearate is practically insoluble in water. Calcium Stearate Calcium Stearate mainly consists of calcium salts of stearic acid (C18H36O2) and palmitic acid (C16H36O2). cool. Cool and add water to make exactly 250 mL. Identification (1) Shake vigorously 3 g of Calcium Stearate with 20 mL of diluted hydrochloric acid (1 in 2) and 30 mL of ether for 3 minutes and allow to stand: the separated aqueous layer responds to the Qualitative Tests (1). 2 mL of 8 mol/L potassium hydroxide TS and 0.02 mol/L disodium ethylenediaminetetraacetate VS.7 g of Calcium Oxide.08). Calcium Stearate feels smooth when touched and is adhesive to the skin. neutralize with ammonia TS. filter through a glass filler (G4). cool. Pipet 10 mL of the solution. wash the residue with boiling water until no turbidity is produced when silver nitrate TS is added to the last washing and dry at 105 °C to a constant weight: the residue is not more than 10. (2) Carbonate⎯Disintegrate 1. allow to stand and separate the water layer. 3 hours) .0% and not more than 101. Prepare the control solution by evaporating 2 mL of hydrochloric acid on a water-bath to dryness and by adding 2 mL of dilute acetic acid. warm the residue with 20 mL of water and 2 mL of dilute acetic acid for 2 minutes. Boil for 1 minute to 2 minutes. add 5 mL of diluted hydrochloric acid (1 in 2) and 20 mL of chloroform. 900 °C.0% of calcium oxide (CaO).02 mol/L disodium ethylenediaminetetraacetate VS = 1. Mix the powder with about 5 times its mass of water: the mixture is alkaline. mix thoroughly and filter. (2) Wash the ether layer obtained in (1) with 20 mL and 10 mL of dilute hydrochloric acid and 20 mL of water successively and evaporate the ether on a waterbath: the residue melts at a temperature not below 54 °C (Method 2). Identification (1) Moisten Calcium Oxide with water: heat is generated and a white powder is obtained. heat the mixture on a waterbath for 2 hours. Evaporate 50 mL of the filtrate with 0. Description Calcium Oxide is a hard. allow to stand for a while. 2.0 mg. Perform the test (not more than 2 ppm). add water to make 50 mL and perform the test. One gram of Calcium Oxide dissolves almost completely in 2500 mL of water. add 50 mL of water. until the color of the solution changes from red-purple to blue. Description Calcium Stearate is a white.KP VIII 1153 Quick Lime CaO: 56. contains not less than 98. when ignited.0 g of Calcium Stearate. evaporate on a water-bath to dryness. light. add 100 mL of water and drop-wise hydrochloric acid with stirring until the solution becomes acidic and further add 1 mL of hydrochloric acid. containing powder and odorless.0 g of Calcium Oxide in 75 mL of water by adding dropwise hydrochloric acid and further add 1 mL of hydrochloric acid.0 g of Calcium Oxide with a small amount of water.0 mL of standard lead solution and add water to make 50 mL (not more than 20 ppm). (2) Dissolve 1 g of Calcium Oxide in 20 mL of water by adding a few drops of acetic acid: the solution responds to the Qualitative Tests for calcium salt. shake vigorously for 3 minutes. add drop-wise an excess of hot ammonium oxalate TS.4% and not more than 7. characteristic odor. add 2 mL of hydrochloric acid. and dissolve in 50 mL of water and 8 mL of diluted hydrochloric acid (1 in 3) by heating. in ethanol or in ether. (3) Magnesium and alkali metals⎯Dissolve 1.0 g of Calcium Stearate with caution at first and then ignite gradually to ash. Each mL of 0. white mass. After cooling. constant weight). Purity (1) Heavy metals⎯Heat gently 1. 105 °C. Calcium Stearate is odorless or has a faint.1 g of NN indicator and titrate with 0. previously ignited at 900 °C to a constant weight and cooled in a desiccator (silica gel). Loss on Drying Not more than 4. bulky powder. Assay Weigh accurately about 0. (2) and (4) for calcium salt. Calcium Stearate. contains not less than 6.1% of calcium (Ca: 40. cool. Combine the filtrate and the washings. (2) Arsenic⎯Take 1. filter and wash the residue with 15 mL of water.0% (1 g. mix thoroughly with 50 mL of water.5 mL of sulfuric acid to dryness and ignite the residue at 600 °C to a constant weight: the residue is not more than 15 mg. Boil the solution for 5 minutes. remove most of the supernatant milky liquid by decantation and add an excess of dilute hydrochloric acid to the residue: no vigorous foam is produced. Purity (1) Acid-insoluble substances⎯Disintegrate 5.08 Calcium Oxide. when dried. Calcium Oxide slowly absorbs moisture and carbon dioxide from air. Calcium Oxide is very slightly soluble in boiling water and practically insoluble in ethanol.0 g of Calcium Oxide with a small amount of water. Amount (%) of free acids = 0.13). Description Cellacefate is a white powder or granules. calculated on the anhydrous basis. add 5 drops of phenolphthalein TS and titrate with 0.0% of carboxybenzoyl group (COC6H4COOH: 149.0 g of Cel- lacefate according to Method 2 and perform the test.1 mol/L sodium hydroxide consumed B : Amount (%) of free acids obtained in the Free acids under the Purity W : Amount (g) of Cellacefate taken. combine the washings and the filtrate and titrate with 0. pH 10.0% of acetyl group (-COCH3: 43.0%.0 g of Cellacefate. calculated as phthalic acid (C8H6O4: 166. add 50 mL of water and exactly 25 mL of 0.1 mol/L sodium hydroxide VS (indicator: 3 drops of phenolphthalein TS). Perform a blank determination and make any necessary correction. heat gently with caution at first and then ignite gradually to ash. 4 drops of eriochrome black T TS and 5 drops of methyl yellow TS and titrate rapidly the excess disodium ethylenediamine tetraacetate with 0.1 mol/L hydrochloric acid VS. determine the density. Amount (%) of carboxybenzoyl group(C8H5O3) 1. Part II Assay Weigh accurately about 0. Perform a blank determination and make any necessary correction.5 g of Cellacefate.0 g of Cellacefate. Cellacefate Cellulose Acetate Phthalate Cellacefate is a reaction product of phthalic anhydride and partially acetylated cellulose.795 × B W = ×100 100 − B A : Amount (mL) of 0. as η = ρν: not less than 45 mPa·s and not more than 90 mPa·s. Perform a blank determination and make any necessary correction.5% and not more than 26. Water Not more than 5.0% and not more than 40. add 10 mL of dilute hydrochloric acid to the residue. place in a glass-stoppered Erlenmeyer flask. (2) Free acids⎯Weigh accurately about 3. 10 mL and 5 mL volumes of hot water. put in a glass-stoppered Erlenmeyer flask. warm for 10 minutes on a water-bath and transfer the contents to a flask with the aid of 10 mL. (2) Acetyl group⎯Weigh accurately about 0. After cooling. calculated on the anhydrous and free acid-free basis.1% (1 g) Assay (1) Carboxybenzoyl group⎯Weigh accurately about 1. W : Amount (g) of Cellacefate taken.05 mol/L magnesium chloride VS. Wash both the flask and residue twice with 10 mL volumes each of diluted methanol (1 in 2). Viscosity Weigh accurately a portion of Cellacefate. Prepare the control solution with 2. direct titration. dissolve in 85 g of a mixture of acetone and water (249: 1 in mass) and perform the test at 25 ± 0. Separately.1 mol/L sodium hydroxide consumed. dissolve in 50 mL of a mixture of ethanol and acetone (3:2) and titrate with 0.05 mol/L disodium ethylenediamine tetraacetate VS = 2. Purity (1) Heavy metals⎯Proceed with 2.1 mol/L sodium hydroxide VS and boil for 30 minutes under a reflux condenser.1 mol/L sodium hydroxide VS (indicator: 2 drops of phenolphthalein TS). Perform the blank determination with 120 mL of diluted methanol (1 in 2) and make any necessary correction: the amount of free acids is not more than 3.1154 Monographs. until the green color of the solution disappears and a red color develops. Residue on Ignition Not more than 0.0% (1 g.491× A − 1. 10 mL of ammonia-ammonium chloride buffer solution. stopper tightly and filter after shaking for 2 hours. Cellacefate contains not less than 21. previously dried.8306 × A W A : Amount (mL) of 0.7. equivalent to 15 g calculated on the anhydrous basis. using a mixture of dehydrated methanol and dichloromethane (3 : 2) instead of methanol for Karl Fischer method). Cellacefate is freely soluble in acetone and practically insoluble in water.05 mol/L disodium ethylenediamine tetraacetate VS.0 mL of standard lead solution (not more than 10 ppm).2 o C as directed in Method 1 under the Viscosity Determination to obtain the kinematic viscosity ν. η.0039 mg of Ca Packaging and Storage Preserve in well-closed containers. Identification Determine the infrared spectra of Cellacefate and Cellacefate RS as directed in the potassium bromide disk method under the Infrared Spectrophotometry : both spectra exhibit similar intensities of absorption at the same wavenumbers. ρ.5 g of Calcium Stearate. Cool. add 100 mL of diluted methanol (1 in 2).12).05) and not less than 30. Each mL of 0. . volumetric titration. of Cellacefate as directed under the Determination of Specific Gravity and Density and calculate the viscosity. calculated on the anhydrous basis. Add sodium hydroxide TS until the solution becomes slightly turbid and then add 25 mL of 0. in methanol or in dehydrated ethanol. Carboxymethylcellulose becomes viscose in sodium hydroxide TS.4305 × A (C2H3O) = W A : Amount(mL) of 0.0% (1 g.5 mL of 0. Description Carboxymethylcellulose is white powder. Carboxymethylcellulose is hygroscopic. Loss on Drying Not more than 8.1 g of Carboxymethylcellulose with 10 mL of water. stir well and filter through a filter paper for quantitative analysis. obtained by shaking 1 g of Carboxymethylcellulose with 100 mL of water. (3) Silicate⎯Weigh accurately about 1. cover with a watch glass and boil gently for 30 minutes. pH─The pH of a suspension. Wash the precipitate three times with 10 mL volumes of water by centrifuging each time. 105 4 hours) o C.1 mol/L sodium hydroxide consumed.720%). To 1 drop of this solution.5182 × B) = − 0.0 mL of this solution and add 6 mL of dilute nitric acid and water to make 50 mL. dissolve in 5 mL of sodium hydroxide TS and add 20 mL of water. (4) Heavy metals⎯Proceed with 1. To 1 mL of the test solution. Residue on Ignition Not more than 1. ignite in a platinum crucible. . Prepare the control solution with 0.5%. Perform the test.5 mL of concentrated chromotropic acid TS and heat on a water-bath for 10 minutes: a redpurple color develops. Carboxymethylcellulose swells with water to form suspension.5 mL of hydrochloric acid on a waterbath until a flocculent precipitate is produced. Carboxymethylcellulose is practically insoluble in ethanol and in ether.40 mL of 0. centrifuge and take the supernatant liquid. centrifuge and take the supernatant liquid. flocculent precipitate is produced. Heat this solution with 2.8 g of Carboxymethylcellulose with 50 mL of water.01 mol/L hydrochloric acid (not more than 0. Carboxymethylcellulose Carmellose CMC Carboxymethylcellulose is a polycarboxymethylether of cellulose. Purity (1) Chloride⎯Shake well 0. corrected after the blank determination W : Amount(g) of Cellacefate taken. Prepare the control solution with 2.0 g of Carboxymethylcellulose according to Method 2 and perform the test. Prepare the control solution with 1. Perform the test. shake. Remove the watch glass and evaporate on a water-bath to dryness with the aid of a current of air. calculated on the anhydrous basis Amount (%) of acetyl group(C2H3O) 100 × ( P − 0. Filter this solution. discard 5 mL of the first filtrate. prepare the test solution according to Method 3 and perform the test (not more than 2 ppm). add 20 mL of dilute hydrochloric acid.0 g of Carboxymethylcellulose.5 and 5. is between 3.5% (after drying.5772 × C (100 − B) B : Amount (%) of free acids obtained in the Free acids under the Purity C : Content (%) of carboxybenzoyl group P : Content (%) of free acids and bound acetyl group (C2H3O) Packaging and Storage Preserve in tight containers. Pipet 25. Cool.0 mL of standard lead solution (not more than 20 ppm). add water to make 5 mL. dissolve in 10 mL of sodium hydroxide TS and add water to make 100 mL.005 mol/L sulfuric acid (not more than 0. dry the residue together with the filter paper when no turbidity is produced on the addition of silver nitrate TS to the last washing and ignite to constant weight: the residue is not more than 0. Continue heating further for 1 hour. add 0. (2) Shake 5 mL of the test solution obtained in (1) with 10 mL of acetone: a white. allow to stand for 10 minutes and use this solution as the test solution. add 10 mL of hot water. 1 g) Packaging and Storage Preserve in tight containers. is odorless and tasteless. Wash the precipitate three times with 10 mL volumes of water by centrifuging each time.KP VIII 1155 Amount (%) of free acids and bound acetyl group 0. Wash the residue with hot water. combine the supernatant liquid and the washings and add water to make 100 mL. (5) Arsenic⎯Take 1. Identification (1) Shake well 0.0 g of Carboxymethylcellulose. take 25 mL of the subsequent filtrate and add 1 mL of dilute hydrochloric acid and add water to make 50 mL.40 g of Carboxymethylcellulose with 25 mL of water. (2) Sulfate⎯Shake well 0.0. combine the supernatant liquid and the washings and add water to make 100 mL.360%). (3) Shake 5 mL of the test solution obtained in (1) with 1 mL of ferric chloride TS: a brown. cool. flocculent precipitate is produced. add 2 mL of sodium hydroxide TS. Heat 20 mL of this solution with 10 mL of dilute nitric acid on a water-bath until a flocculent precipitate is produced. Separate the supernatant liquid. to the bottom of a glass column. add 10 mL of hot water. dissolve and cool: the pH of this solution is between 6. proceed in the same manner. 15 mm in inner diameter and 2 mm in thickness. The solution has no more color than the following standard stain. heat gently until it becomes fluid. add 5 mL of sulfuric acid and heat until white fumes are evolved. To 1 mL of the test solution. stir well and filter through a filter paper for quantitative analysis. heat to produce a flocculent precipitate on a water-bath. Carboxymethylcellulose Sodium is hygroscopic.0. in ethanol.0 g of Carboxymethylcellulose Sodium. (6) Arsenic⎯Take 1. Take 10 mL of this solution.45 mL of 0. then trans- . centrifuging each time. add water to make 200 mL and use 50 mL of this solutions as the test solution. boil gently on a water-bath for 5 minutes and filter.0 g of Carboxymethylcellulose Sodium in 20 mL of warm water with stirring.5% of sodium (Na: 22. combine the supernatant liquid and the washings. wash the precipitate three times with 10 mL volumes of water. dry together with the filter paper after no turbidity is produced on the addition of silver nitrate TS to the last washing and then ignite to constant weight: the residue is not more than 0. add 5 mL of nitric acid and heat again.99).005 mol/L sulfuric acid (not more than 0. add water to make 50 mL and use this solution as the test solution. Carboxymethylcellulose Sodium. Repeat this operation until the solution becomes colorless or pale yellow. Part II Carboxymethylcellulose Sodium CMC Sodium Carboxymethylcellulose Sodium is the sodium salt of a polycarboxymethylether of cellulose. Perform the test. (2) To 10 mL of the test solution obtained in test (1). Evaporate the filtrate to dryness and add 20 mL of water to the residue: the solution responds to the Qualitative Tests for sodium salt. Continue heating for further 1 hour.0 mL of standard lead solution (not more than 20 ppm). Carboxymethylcellulose Sodium is practically insoluble in methanol. add 20 mL of methanol and 2 mL of dilute hydrochloric acid. centrifuging each time. Add 2 mL of barium chloride TS. add 20 mL of nitric acid. (3) To 3 g of Carboxymethylcellulose Sodium. Repeat the operation 3 times and calculate the mean value: it is not larger than that calculated from the same operation. 250 mm in height. 2 mm in thickness to the bottom of a glass column. add 1 mL of cupric sulfate TS: a blue flocculent precipitate is produced.5 g of Carboxymethylcellulose Sodium in 50 mL of water and use this solution as the test stock solution. 5 mL of ethanol and add water to make 50 mL.5% and not more than 8. (2) Chloride⎯Dissolve 0. in glacial acetic acid or in ether. Wash the residue with hot water. Standard stain⎯Without using Carboxymethylcellulose Sodium. us- ing the following control solution.5 mL of concentrated chromotropic acid TS and heat on a water-bath for 10 minutes: a red-purple color develops. add 0. Separate the supernatant liquid.50 mL of 0.0 g of Carboxymethylcellulose Sodium according to Method 2 and perform the test. Description Carboxymethylcellulose Sodium is white to yellowish white powder or granules and has no taste. wash the precipitate three times with 10 mL volumes of water. Take 5 mL of this solution and use this solution as the test solution and perform the test.005mol/L sulfuric acid. mix well and allow to stand for 10 minutes. Control solution⎯Take 5. Shake well this solution before use. when dried. After cooling. This is used as an outer tube. Remove the watch glass and evaporate on a water-bath to dryness with the aid of a current of air. cool and centrifuge. cover with a watch glass and boil gently for 30 minutes.5%.0 g of Carboxymethylcellulose Sodium. pH Add 1. Prepare the control solution with 0. Purity (1) Clarity and color of solution⎯Firmly attach a glass plate of good quality. determine the height of the solution up to the lower edge of the inner tube when the distinction of the lines becomes impossible. cool and use this solution as the test solution.40 mL of 0.0 g of Carboxymethylcellulose Sodium in small volumes to 100 mL of warm water with stirring.0 g of Carboxymethylcellulose Sodium in 100 mL of water.960%). Moving the inner tube up and down observing from the upper part. add 20 mL of dilute hydrochloric acid. pour this solution into the outer tube and place on a piece of white paper on which 15 parallel black line. Prepare the control solution with 0. Carboxymethylcellulose Sodium forms a viscid solution in water or warm water. 25 mm in inner diameter and 2 mm in thickness. Dissolve 1.1156 Monographs. Cool. cool. ignite in a platinum crucible. Similarly prepare an inner tube by attaching a glass plate of good quality. (4) Silicate⎯Weigh accurately about 1.640%). add 15 mL of a saturated solution of ammonium oxalate and heat until white fumes are evolved again. cool and add water to make 25 mL. Shake 10 mL of the test solution with 10 mL of dilute nitric acid. 2 mm in thickness.01mol/L hydrochloric acid (not more than 0. contains not less than 6. add water to make 5 mL.5 and 8. heat to produce a flocculent precipitate on a water-bath. combine the supernatant liquid and the washings and add water to make 50 mL. (5) Heavy metals⎯Proceed with 1. 1 mm in width and 1 mm in interval are drawn. 300 mm in height. if necessary. add 1 mL of dilute hydrochloric acid. Identification (1) Dissolve 2. Perform the test. To 1 drop of this solution. (3) Sulfate⎯Shake throughly 1 mL of hydrochloric acid to 10 mL of the test stock solution obtained in (2). Prepare the control solution with 2. cool and centrifuge. 5 g of Carboxymethylcellulose Sodium. Assay Weigh accurately about 0. Purity (1) Alkali⎯Shake thoroughly 1.1 g of Carboxymethylcellulose Calcium with 10 mL of water. (ii) Take a quantity of the fitrate and add an equal volume of barium chloride TS: a fine.5 g of Carboxymethylcellulose Sodium. Method of Preparation Prepare as directed under Tablets. It meets the require- Assay Weigh accurately not less than 20 Carboxyme- thylcellulose Sodium Tablets and powder.2990 mg of Na Packaging and Storage Preserve in tight containers. (iii) The filtrate obtained from (i) responds to the Qualitative Tests for sodium salt.0. To 1 mL of the test solution. equivalent to about 1 g of Carboxymethylcellulose Sodium. is between 4. Perform a blank determination and make any necessary correction. To 1 drop of this solution. add 2 mL of sodium hydroxide TS. Cool and titrate with 0.5 mL of concentrated chromotropic acid TS and heat on a water-bath for 10 minutes: a red-purple color develops. Weigh accurately a volume of the powder. Identification (1) Shake thoroughly 0. with Carboxymethylcellulose Sodium. Perform a blank determination and make any necessary correction. o C. (7) Starch⎯Add step-wise 2 drops of iodine TS to 10 mL of the test solution obtained in (2): no blue color develops. Disintegration It meets the requirement of Disintegration tests. 105 4 hours). if necessary.1 mol/L perchloric acid (potentiometric titration. (2) Shake 5 mL of the test solution obtained in (1) with 10 mL of acetone: a white. previously dried.99).5% of the labeled amount of carboxymethylcellulose Sodium (Na: 22.1 mol/L perchloric acid = 2.5% and not more than 9. Test time should be 2 hours. (i) Take 30 mL of the filtrate and add 3 mL of hydrochloric acid: a white precipitate is produced. add 0. End point Detection Method in Titrimetry). Carmellose Calcium is hygroscopic. Carboxymethylcellulose Calcium Carmellose Calcium CMC Calcium Carboxymethylcellulose Calcium is the calcium salt of a polycarboxymethylether of cellulose.2990 mg of Na Packaging and Storage Preserve in tight containers. Carboxymethylcellulose Sodium Tablets CMC Sodium Tablets Carboxymethylcellulose Sodium Tablets contain equivalent to not less than 6. Carboxymethylcellulose Calcium swells with water to form a suspension.0 g of Carboxymethylcellulose Calcium with 50 mL of water. dissolve the residue in 10 mL of water and 5 mL of acetic acid and filter. Uniformity of Dosage Units ment. allow to stand for 10 minutes and use this solution as the test solution. (3) Shake 5 mL of the test solution obtained in (1) with 1 mL of ferric chloride TS: a brown. add 80 mL of glacial acetic acid. Loss on Drying Not more than 10.5 and 6. cool and neutralize with ammonia TS: the solution responds to the Qualitative Tests (1) and (3) for calcium salt.KP VIII 1157 fer 5 mL of this solution to a generator bottle. Each mL of 0. Carboxymethylcellulose Calcium is practically insoluble in ethanol or in ether. (4) Ignite 1 g of Carboxymethylcellulose Calcium to ash. cool and titrate with 0. add water to make 5 mL. freshly boiled and cooled and add 2 drops of phenolph- .1 mol/L perchloric acid (potentiometric titration). connect with a reflux condenser and heat on an oil bath maintained at 130 o C for 2 hours.1mol/L perchloric acid = 2. in 50 mL of water and filter: the filtrate responds to the following tests. Each mL of 0.0% (1 g. flocculent precipitate is produced. flocculent precipitate is produced. white precipitate is formed. add 80 mL of glacial acetic acid. obtained by shaking 1 g of Carboxymethylcellulose Calcium with 100 mL of water. Boil the filtrate. add exactly 2 mL of standard arsenic solution and proceed as directed for the test with the test solution (not more than 10 ppm). heat the mixture on a water-bath for 2 hours. equivalent to about 0. pH⎯The pH of a suspension. Identification Dissolve a quantity of powdered Carboxymethylcellulose Sodium Tablets. Description Carboxymethylcellulose Calcium is white to yellowish white powder and is odorless. and compare the turbidity. Part II thalein TS: no red color develops. Melting Point Between 47 °C and 53 °C.8 g of Carboxymethylcellulose Calcium with 50 mL of water. Cera Carnauba Purity Proceed as directed in the Purity under Stearyl Alcohol.0 and 20. 105 4 hours).0% (after drying. add 50 mL of ethanol and 25. Iodine Value Between 5 and 14 (Dissolve Carnauba Wax in by shaking a glass-stoppered flask in warm water). centrifuge and take out the supernatant liquid.0. white flakes. Residue on Ignition Between 10. The turbidity from the test solution is not more dense than the turbidity from the control solution (not more than 1. Hydroxyl Value Between 210 and 232.0% (1 g. C.05% (2 g). Acid Value Not more than 1. Melting point─Between 80 o C and 86 o C .0.44). Packaging and Storage Preserve in well-closed containers. Ester Value Not more than 2.42 mL of 0. characteristic odor and is tasteless. Use a mixture of xylene and ethanol (2 : 1) as a solvent.005mol/L sulfuric acid. Add 1 mL of 3 mol/L hydrochloric acid and 3 mL each of brium chloride TS to the test solution and the standard solution. combine the supernatant and the washings and add water to make 100 mL. Prepare the control solution with 0. 1 g) Packaging and Storage Preserve in tight containers. Cool. in dehydrated ethanol or in ether. Prepare the control solution with 2.0 g of Carboxymethylcellulose Calcium according to Method 2 and perform the test. (2) Chloride⎯Shake thoroughly 0. Carnauba Wax has slight.0 mL of standard lead solution (not more than 20 ppm).40 mL of 0.1158 Monographs. characteristic odor and is tasteless.990 and 1. (4) Heavy metals⎯Proceed with 1. combine the supernatant and washings and add water to make 100 mL.0. very slightly soluble in acetic anhydride and practically insoluble in water. add water to make 50 mL. centrifuge and take the supernatant liquid.0 mL of 0. o Carnauba Wax is practically insoluble in water. Perform the test using 25 mL of this solution as the test solution and prepare the control solution with 0.0%). Description Carnauba Wax is pale yellow to pale brown. Take 25 mL of this solution. Cetanol Cetanol is a mixture of solid alcohols and consists chiefly of cetanol (C16H34O: 242.36%). 20 Specific gravity─ d 20 : Between 0. . water to make 50 mL and use this solution as the test solution. or masses. Acid Value Not more than 10. Saponification Value Between 78 and 95. Perform the test. Weigh accurately about 3 g of Carnauba Wax in a 300-mL flask. hard and brittle mass or white to pale yellow powder.0. Loss on Drying Not more than 10. (3) Sulfate⎯Heat 10 mL of the test stock solution obtained in (2) with 1 mL of hydrochloric acid on a water-bath until a flocculent precipitate is produced. ethanol. Take 25 mL of this solution and add 6 mL of dilute nitric acid. Heat 20 mL of the test stock solution with 10 mL of dilute nitric acid on a water-bath until a flocculent precipitate is produced. After cooling.5 mol/L potassium hydroxide-ethanol VS and proceed as directed in the Saponification value under the Fats and Fatty Oils. Allow to stand for 10 minutes. Residue on Ignition Not more than 0. ether or xylene. dissolve in 10 mL of sodium hydroxide TS. Wash the precipitate three times with 10 mL volumes of water by centrifuging each time. granules. Cetanol is very soluble in pyridine. Packaging and Storage Preserve in well-closed containers. Wash the precipitate three times with 10 mL volumes of water by centrifuging each time. Carnauba Wax Iodine Value Not more than 2. The time of heating should be 2 hours and the titration should be done by warming. Proceed as directed in the Melting Point under Stearyl Alcohol. Description Cetanol occurs as unctuous. and mix. Carnauba Wax is the wax obtained from the leaves of Copernicia cerifera Mart (Palmae). freely soluble in ethanol. add water to make 100 mL and use this solution as the test stock solution. Cetanol has a faint. add 25 mL of xylene and dissolve by warming.01mol/L hydrochloric acid (not more than 0. To this solution.002. 105 °C. (2) Water-soluble substances⎯Mix 6. Evaporate a 15.5 mL of water. is obtained. Perform a blank determination and make any necessary correction.0 mg. loss on drying and bulk density values with the range. add 0. pH Mix 10 g of Powdered Cellulose with 90 mL of freshly boiled and cooled water and allow to stand for 1 hour with occasional stirring: the pH of the supernatant liquid is between 5. Filter with the aid of vacuum. Evaporate the eluate to dryness in an evaporation dish. Place about 10 mg of Powdered Cellulose on a watch glass and disperse in 2 mL of this solution: the substance develops a blue-violet color. 400 and about 20 cm in inside diameter). previously dried and weighed dry at 105°C for 30 minutes and cool in a desiccator : the residue is not more than 15. Microcrystalline Cellulose is practically insoluble in water. transfer to a 125 mL Erlenmeyer flask. Transfer 100 mL of the dispersion to a 100-mL mass cylinder and allow to stand for 3 hours: a white. which does not form a supernatant liquid at the surface. Microcrystalline Cellulose swells with sodium hydroxide TS on heating.0 mL of standard lead solution (not more than 10 ppm).KP VIII 1159 Powdered Cellulose Powdered Cellulose is purified.5 g of iodine and shake for 15 minutes. to obtain a clear filtrate. 2 hours).0 and 7.0 g of Powdered Cellulose with 90 mL of freshly boiled and cooled water and allow to stand for 10 minutes with occasional stirring.0 mg.3 g of Microcrystalline Cellulose. Microbial Limits The total aerobic microbial count is not more than 1000 per g. Salmonella species.0 g of Powdered Cellulose according to Method 2 and perform the test. add 25. Identification (1) Dissolve 20 g of zinc chloride and 6. mix 45 g with 255 mL of water. opaque. Perform the test with this solu- . mix 30 g of Microcrystalline Cellulose with 270 mL of water: otherwise. Staphylococcus aureus and Pseudomonas aeruginosa are not observed.3% (1 g. if necessary. transfer 100 mL of the dispersion to a 100 mL mass cylinder and allow to stand for 1 hour: a supernatant liquid appears above the layer of the cellulose and the supernatant liquid produces a precipitate. Perform the mixing for 5 minutes in a high-speed (18000 revolutions per minute or more) power blender. Description Powdered Cellulose is a white powder. mechanically disintegrated α-cellulose obtained as a pulp from fibrous plant materials.0 mL each of water and 1 mol/L cupriethylenediamine TS. add 0. (3) Weigh accurately about 0. to a 125-mL Erlenmeyer flask and add 25. the addition of sulfuric acid being omitted from the procedure). P. (3) Transfer 1. Place about 10 mg of Microcrystalline Cellulose on a watch glass and disperse in 2 mL of this solution: the substance develops a blue-violet color. previously weighed. Prepare the control solution with 2. Description Microcrystalline Cellulose is a white crystalline powder having fluidity. (2) Sieve 20 g of Microcrystalline Cellulose for 5 minutes on an air-jet sieve equipped with a screen (No. and pass 50 mL of peroxide-free ether through the column.5 g of iodine and shake for 15 minutes.0 g of Powdered Cellulose in a column.5 g of potassium iodide in 10. calculated on the dried basis.25 g of Powdered Cellulose. in ethanol or in ether.5 g of potassium iodide in 10. dry at 105 °C for 1 hour and cool in a desiccators : the residue is not more than 15. Microcrystalline Cellulose Microcrystalline Cellulose is purified. The label indicates the mean degree of polymerization value with the range. obtained as a pulp from fibrous plant material. Loss on Drying Not more than 6. partially depolymerized α-cellulose. Residue on Ignition Not more than 0.5 mL of water. bubble-free dispersion. to dryness without charring. accurately weighed. Perform a blank determination and make any necessary correction. Purity (1) Heavy metals⎯Proceed with 2. in ethanol or in ether.0 mL volumes of the filtrate in an evaporation dish. Packaging and Storage Preserve in tight containers. discard the first 10 mL of the filtrate and pass the subsequent filtrate through the same filter.5. (3) Ether-soluble substances⎯Place 10. If more than 5% is retained on the screen.0 mL each of water and 1 mol/L cupriethylenediamine TS and proceed as directed in the Identification (3) under Microcrystalline Cellulose : the mean degree of polymerization. is not less than 440 and is within the labeled specification.0% (1 g. with mineral acids. Powdered Cellulose is practically insoluble in water. insert the stopper and shake on a suitable mechanical shaker to dissolve. Immediately purge the solution with nitrogen. The label indicates the degree of polymerization. about 20 mm in inner diameter. (2) Mix 30 g of Powdered Cellulose with 270 mL of water in a high-speed (18000 revolutions per minute or more) blender for 5 minutes. the total combined fungi and yeast count is not more than 100 per g and Escherichia coli. Identification (1) Dissolve 20 g of zinc chloride and 6. about 20 mm in inner diameter. Residue on Ignition Not more than 0.744 g of powdered potassium chloride. Conductivity (1) Standard potassium chloride solution⎯Weigh accurately 0. Perform a blank determination and make any necessary correction. Gx : conductivity measured (μS). Perform a blank determination and make any necessary correction. with standard potassium chloride solution and fill up with the standard potassium chloride solution.0 mL of standard lead solution (not more than 10 ppm).x 0 . aration of the potassium chloride conductivity calibration standard solution (μS·cm-1) (25°C). Evaporate the eluate to dryness in a previously dried and tared evaporation dish. Prepare the control solution with 2. -1 x T (µS·cm ) = JG T -1 x 0 (µS·cm ) = JG 0 Loss on Drying Not more than 7. Bulk Density (1) Apparatus⎯Use a volumeter shown in the figure. Take exactly 100 mL of this solution.0 and 7.9 μS·cm-1. Separately.0 g of Microcrystalline Cellulose with 80 mL of water for 10 minutes. p is not more than 350 and within the labeled range. add water at 20 ± 1 °C to make exactly 1000 mL and determine the conductivity: the conductivity constant of this solution. ν0. (3) Ether-soluble substances⎯Place 10. and pass 50 mL of peroxide-free ether through the column. the conductivity meter consists of detector and indicator. After washing well the cell with water.0 g of Microcrystalline Cellulose in a column.1160 Monographs.1 cm-1. 0 Use the supernatant obtained in the pH test as the test solution. dry at 105 °C for 1 hour. of Micro- ν ν0 Obtain the product.1 °C. by the following expressions: the value x T .03. .1% (2 g). previously washed well with water. The detector consists of a cell including electrodes in it. kept at 25 ± 0. p= 95[η ]C amount (g) of the test calculated on the dried basis pH Shake 5. cool in a desiccator (silica gel) and weigh: the residue is not more than 12.0 g of Microcrystalline Cellulose with 40 mL of freshly boiled and cooled water for 20 minutes and centrifuge: the pH of the supernatant liquid is between 5. by the following formula. The cell constant. after a stable reading of ± 0 3% is obtained. Dry the residue at 105 °C for 30 minutes. previously dried at 500 °C to 600 °C for 4 hours. 0.0% and within a range as specified on the label (1 g. repeat the determination in same manner and measure the conductivity of the standard potassium chloride solution. 0.0 mg. ν.1 °C.0. is not more than 75 μS·cm-1. Determine the conductivity and the standard potassium chloride solution is kept at 25 ± 0. J . previously weighed. η crystalline Cellulose by the formula: η rel = rel. at 25 ± 0.0 mg. and dissolve in water at 20 ± 1 °C to make exactly 1000 mL. and weigh accurately: the residue is not more than 5. GT (µS). using a capillary viscometer having K. (3) Procedure⎯Wash 2 to 3 times the cell. of limiting viscosity [ η ] (mL/g) and concentration C (g/100 mL) from the value ηrel of the Table shown somewhere below. (2) Water-soluble substances⎯Shake 5. G0 (µS). (2) Apparatus⎯Use an appropriate conductivity meter having the cell constant of between 0. [ η ]C. Evaporate the clear filtrate in a beaker. χKCl. 105 °C. p. Replace the standard potassium chloride solution. allow to cool in a desiccator. x KCl : conductivity constant of the potassium chlo- ride conductivity calibration standard solution (μS·cm1 ) (25°C) x H O : conductivity constant of water used for prep2 Purity (1) Heavy metals⎯Proceed with 2. Part II tion according to Method 1 under the Viscosity Determination using a capillary viscometer having the viscometer constant (K). to dryness without charring.01 and determine the kinematic viscosity. 3 hours). at 25 °C is 146. Determine the conductivity of water used for the preparation of the test solution. rinse the cell with the test solution 2 to 3 times. is calculated by the following: J= xKCl + x H2O G x0 J : cell constant (cm-1). When calculated the degree of polymerization. Calculate the relative viscosity. Usually. perform the test with a mixture of 25. filter with the aid of vacuum through filter paper into a vacuum flask. fill up with the test solution and determine the conductivity of the test solution. in the same manner as above and calculate the conductivity constants. The cell with a temperature compensation circuit is preferable.01 and 0.1 °C and determine the kinematic viscosity. Gx (µS).0 mL each of water and 1 mol/L cupriethylenediamine TS in the same manner as above. x T (μS·cm-1) and x 0 (μS·cm-1).0 g of Microcrystalline Cellulose according to Method 2 and perform the test. 566 0.544 0.358 0.0 mm in inner diameter.152 0.098 0.580 0.01 0.558 0.050 1.089 1.207 0.445 0.115 0.959 1.260 1.743 0.125 0.769 0.876 0.971 1.649 0.460 0.078 1.067 1.4 2.622 0.268 0.7 2.391 0.116 1.302 0.846 0.602 0.929 0.039 1.900 0.270 1. Salmonella species.242 0.573 0. From a position apart 5.225 1.935 0.143 0.03 0.656 0.976 1.888 0.840 0.894 0.399 0. Put a No.072 1.636 0.9 0.230 1. at a rate suitable to prevent clogging. slowly pour Microcrystalline Cellulose through the sieve.028 1.09 1.7 1.276 0.061 1.809 0. which has a capacity of 25. having four glass baffle plates inside which the sample powder slides as it passes.250 0.170 0.245 1.858 0.300 0.407 0.3 2.225 0.453 0.5 2.00 0.215 1.690 0.2 1.1 1.111 1.788 0.965 1.953 1. At the bottom of the baffle box is a funnel that collects the powder.174 1. (2) Procedure⎯Weigh accurately the mass of a brass or stainless steel cup.736 0.285 1.0 ± 2.918 0.437 0.762 0.1 2.529 0.775 0.180 0.670 0.324 0.205 1.319 0. weigh the filled cup and weigh accurately the content of the cup and then calculate the bulk density by the following expression: the bulk density is within the labeled specification.468 0.4 1.827 0.169 1.697 0.536 0.815 0.033 1.161 0.988 1.2 2.1 cm from the top edge of the funnel.07 0.717 0. Level the excess powder with the aid of a slide glass.240 1.318 0.285 0.6 1.6 sieve (2000 μm) on top of the volumeter.414 0. until the cup overflows.782 2.334 0.795 0. 8.189 0.756 0.044 1.265 1.730 0.295 0.04 0.220 1.305 0.515 0.105 1.484 0.235 1.131 1.0 2.137 1.821 0.022 1.906 0. the total aerobic microbial count is not more than 1000 per g.179 1.06 0.011 1.677 0.522 0.595 0.329 0.190 1. Table for Conversion of Relative Viscosity (ηrel) into the Product of Limiting Viscosity and Concentration ([η]C) [η]C ηrel 0.05 mL and an inside diameter of 30.551 0.615 0.383 0.163 1. the total combined fungi and yeast count is not more than 100 per g and Escherichia coli.8 2.293 0.121 1.158 1.106 0.422 0.9 0. and put the cup directly below the funnel of the volumeter.994 1.608 0.491 0.8 1.126 1.255 1.367 0.375 0.02 0.350 0.210 1.587 0.882 0. A funnel is mounted over a baffle box.342 0.195 1.100 1.333 .723 0.250 1.864 0. Staphylococcus aureus and Pseudomonas aeruginosa are not observed. and allows it to pour in- Packaging and Storage Preserve in tight containers.499 0.6 2.083 1.802 0.275 1.749 0.200 1.006 1.912 0.430 0.704 0.683 0.5 1.924 0.233 0.476 0.983 1.0 ± 0.134 0.290 0.184 1.948 1.056 1.259 0.08 0.870 0.642 0.000 1.833 0.280 1.198 0.094 1.663 0.941 1.153 1.216 0.147 1.852 0.05 0.710 0.310 0.314 0.3 1.507 0.017 1.629 0. Bulk density (g/cm 3 ) = A 25 A: Measured mass of the content of the cup (g) Microbial Limit When tested.142 1.326 0.310 0.KP VIII 1161 to a sample receiving cup mounted directly below it. 0 6.3 3.467 2.481 2.603 2.922 2.087 1.658 1.550 2.433 2.605 2.584 2.1 8.826 1.811 1.870 1.765 1.116 5.575 1.769 2.726 2.786 2.979 2.785 1.521 2.2 4.240 2.583 1.700 2.395 1.591 1.968 2.800 2.937 2.546 1.446 1.167 2.640 2.043 2.264 2.060 2.013 2.1 5.911 1.6 3.230 2.805 2.590 2.110 1.249 2.946 2.957 2.840 2.376 1.715 1.773 1.215 2.431 2.972 2.604 1.436 1.158 2.860 2.750 2.842 2.695 2.300 2.828 2.666 1.568 2.767 2.1 7.764 2.505 2.630 2.390 2.683 2.884 2.273 2.455 1.904 1.7 7.996 2.8 6.489 2.427 1.723 1.8 5.525 1.218 2.511 2.873 2.721 2.093 1.735 1.8 4.341 2.002 .003 2.950 1.662 1.297 2.3 2.954 1.642 1.154 2.050 2.306 2.400 2.513 1.959 2.432 1.1162 Monographs.558 2.957 1.367 2.414 1.3 4.574 2.516 2.913 2.2 5.790 2.792 1.771 2.645 2.566 1.2 7.344 2.571 2.928 2.683 1.975 2.724 2.974 2.3 6.3 5.418 1.939 1.312 2.246 2.294 2.5 4.453 2.698 2.673 2.781 1.795 2.621 1.1 6.646 1.558 1.955 2.362 1.550 1.877 2.896 1.000 2.600 1.700 1.073 2.518 2.387 2.500 2.675 2.373 2.990 2.762 4.658 2.200 2.985 2.458 2.867 1.758 1.0 7.804 1.774 2.961 2.459 1.926 2.856 1.236 2.731 2.070 2.668 2.902 2.911 2.7 3.090 1.777 1.821 2.7 6.386 1.291 2.743 2.113 1.671 1.4 6.702 2.874 1.615 2.4 5.173 2.324 2.5 3.135 2.815 1.405 1.508 2.986 2.844 2.010 2.100 1.504 1.816 2.464 2.881 2.576 2.428 2.914 1.963 2.9 1.1 3.097 1.830 1.145 2.856 2.665 2.329 2.943 1.618 2.332 2.037 2.909 2.2 8.107 1.579 2.080 2.863 2.879 2.719 1.989 2.3 7.597 2.587 1.719 2.483 2.492 2.918 2.6 7.209 2.279 2.687 1.176 2.464 1.521 1.833 2.532 2.841 1.160 2.826 2.562 1.608 2.384 2.976 2.517 1.053 2.833 1.885 1.845 1.186 2.500 1.183 2.376 2.800 1.379 2.900 2.760 2.206 2.979 3.285 2.529 2.762 2.781 2.950 2.132 2.6 6.851 2.456 2.887 2.9 2.746 2.717 2.2 6.870 2.648 2.729 2.1 4.8 3.371 1.497 2.925 1.122 2.952 2.408 2.472 2.233 2.047 2.691 1.357 1.353 2.796 1.414 2.470 2.255 2.655 2.939 2.996 2.678 2.650 1.450 1.148 2.315 2.9 2.4 3.895 2.361 2.425 2.554 1.077 2.270 2.807 2.529 1.920 2.748 2.494 2.417 6.4 7.352 1.905 2.878 1.750 1.849 2.057 2.409 1.224 2.627 2.944 2.125 2.600 2.9 2.350 2.653 2.982 2.436 2.129 2.258 2.779 2.738 2.393 2.0 3.020 2.875 2.477 1.921 1.347 2.524 2.221 2.889 2.637 1.083 2.994 2.5 5.685 2.447 2.195 2.103 1.898 2.819 2.932 1.907 1.595 1.422 2.693 2.561 2.381 1.000 2.776 2.798 2.0 8.5 6.382 2.727 1.987 2.0 5.030 2.6 4.508 1.848 1.946 1.142 2.714 2.823 2.893 2.704 1.119 2.405 2.547 2.063 2.865 2.396 2.852 1.326 2.924 2.566 2.7 4.555 2.635 2.170 2.610 2.915 8.650 2.687 2.540 2.180 2.355 2.808 1.309 2.542 2.736 2.475 2.746 1.486 2.695 1.625 1.625 2.190 2.680 7.690 2.033 2.620 2.966 2.637 2.822 1.814 2.542 1.0 4.400 1.998 2.151 2.343 1.203 2.553 2.889 1.390 1.579 1.303 2.769 1.139 2.2 3.654 1.164 2.411 2.961 1.537 2.793 2.970 2. Part II 3.670 2.968 2.660 2.675 1.757 2.837 1.613 2.733 2.007 2.891 2.482 1.710 2.197 2.468 1.338 1.608 1.882 1.267 2.040 2.513 2.364 2.403 2.633 2.783 2.338 2.837 2.942 2.755 2.893 1.900 1.617 1.9 1.370 2.581 2.473 1.419 2.348 1.948 2.587 2.858 2.754 1.707 2.931 2.537 1.643 2.570 1.854 2.964 2.261 2.802 2.679 1.933 2.318 2.592 2.461 2.705 2.712 2.859 1.423 1.252 2.819 1.612 1.981 3.595 2.526 2.789 1.533 1.830 2.486 1.918 1.491 1.4 4.868 2.8 7.992 2.478 2.545 2.847 2.742 1.983 2.623 2.367 1.788 2.863 1.439 2.282 2.023 2.7 5.935 2.739 1.441 1.971 2.712 1.442 2.936 1.358 2.212 2.812 2.444 2.809 2.731 1.227 2.503 2.708 1.335 2.835 2.563 2.067 2.993 2.929 1.5 7.752 2.633 1.320 2.907 2.288 2.027 2.017 2.534 2.243 2.496 1.740 2.192 2.663 2.450 2.629 1.6 5.276 2. 37 3.29 4.096 3.64 3.162 3.38 4.72 3.206 3.02 4.35 4.110 3.5 8.010 3.098 3.10 4.004 3. then gradually decolorizes.3 9.252 3.156 3.060 3. Chlorobutanol slowly volatilize in air.298 3.196 3.300 3.148 3.142 3.60 3.62 3.140 3.112 3.229 3.120 3.244 3.88 4.176 3.037 3.219 3.192 3. Chlorobutanol Identification (1) Add dilute hydrochloric acid to Chlorinated Lime: a gas.150 3.58 3.69 3.27 4.61 3.291 3.256 3.062 3.242 3.266 3.50 3.223 3.015 3.23 4.56 4.0 9.122 3.273 3.174 3.37 4.138 3.217 3.80 3.231 3.166 3.20 4.25 4.182 3.320 3.277 3.154 3.204 3.74 3.106 3.188 3.050 3. Perform a blank deter- CH3 Cl3C C OH CH3 C4H7Cl3O: 177.254 3. in ethanol or in ether and slightly soluble in water.027 3.09 4.63 3.17 4.44 4. Transfer to a 500-mL volumetric flask with the aid of water and add water to make 500 mL.13 4.200 3.41 4.250 3.68 3.092 3.302 3.34 3.114 3.64 3.71 3.96 4.07 4.53 4.52 4.168 3. Add 10 mL of dilute hydrochloric acid and titrate the liberated iodine with 0.30 4. which has the odor of chlorine.152 3.158 3.128 3. (2) Shake 1 g of Chlorinated Lime with 10 mL of water and filter: the filtrate responds to the Qualitative Tests (2) and (3) for calcium salt.4 9.46 Chlorobutanol contains not less than 98. calculated on the anhydrous basis.235 3.22 4.275 3.194 3.136 3. Description Chlorinated Lime is a white powder and has a chlorine-like odor.067 3.5453 mg of Cl Chlorinated Lime contains not less than 30.48 3.269 3.321 10 11 12 13 14 15 16 17 18 19 3.170 3.214 3.264 3.146 3.184 3.9 3.132 3.025 3.8 9.044 3.83 3.064 3.0 and not more than 101.295 3.8 8.0% of Chlorobutanol (C4H7Cl3O).93 4.048 3.130 3.97 4.116 3.215 3.313 3.164 3.017 3.58 3.36 3.281 3.316 3.248 3.287 3.309 3. Chlorinated Lime dissolves partially in water.021 3.24 4. tight containers in a cold place.39 3.212 3.55 3.293 3.06 4.124 3.9 3.04 4.268 3.094 3.39 4.33 4.058 3.41 3.7 9.233 3. Chlorinated Lime Each mL of 0.46 3.59 3.31 4.241 3.079 3.190 3.56 3.056 3.077 3.279 3.144 3.66 3.052 3.46 4.50 4.210 3.260 3.61 3.18 4.208 3.15 4.227 3. The solution changes red litmus paper to blue.258 3.172 3.KP VIII 1163 8.134 3.108 3.60 3.085 3.054 3.89 4.040 3.283 3.45 4.042 3.104 3.297 3.087 3.012 3.36 4.289 3.52 3.006 3.029 3.307 3.237 3.14 4.305 3.55 4.304 3.246 3.100 3.106 9.198 3.45).271 3.11 4.7 8.089 3.42 4.019 3.1 mol/L sodium thiosulfate VS (indicator: 3 mL of starch TS).239 3.118 3.311 3.63 3.102 3. Chlorobutanol is very soluble in methanol.186 3.66 mination and make any necessary correction.033 3.008 3.5 9.0 g of Chlorinated Lime.202 3.43 4.03 4.76 3.45 3.046 3.85 3.318 3.035 3. Description Chlorobutanol is colorless or white crystal and has camphor-like odor.1 mol/L sodium thiosulfate VS = 3.178 3.180 3.99 4.92 4.285 3.77 3.80 3. .53 3.49 4.54 4.075 3.225 3.32 3.4 8.1 9.2 9.073 3.031 3.28 4.86 4.79 3.47 4.48 4.19 4.069 3.65 3.00 4.43 3.34 4.262 3.6 9.90 4.071 3.023 3. Assay Weigh accurately about 5. evolves and the gas changes moistened starchpotassium iodide paper to blue.0% of available chlorine (Cl: 35.6 8.083 3.95 4. transfer to a mortar and triturate thoroughly with 50 mL of water.160 3. Melting point─Not lower than about 76 o C .221 3. Packaging and Storage Preserve in light.resistant.57 3.081 3. Water Content Not more than 6.915 mg of C4H7Cl3O Packaging and Storage Preserve in tight containers. (2) Dissolve 5 mg of Cholesterol in 2 mL of chloroform. 0. direct titration). Loss on Drying Not more than 0. ethanol or ether. H HO C27H46O: 386. Cinnamon Oil H H Cholesterol is freely soluble in chloroform or in ether. Purity (1) Acid⎯Shake thoroughly 0. Add 10 mL of sodium hydroxide TS. add 1 mL of acetic anhydride and 1 drop of sulfuric acid and shake: a red color is produced and it changes to green through blue. Specific Optical Rotation o [α ] 25 D : Between -34 and -38 o (after drying. Assay Weigh accurately about 0.1 mol/L ammonium thiocyanate VS (indicator: 2 mL of ferric ammonium sulfate TS). Prepare the control solution with 1. add 10 mL of water and titrate with 0. Purity (1) Clarity of solution⎯Place 0. then slowly add 3 mL of iodine TS: a yellow precipitate is produced and the odor of iodoform is perceptible. Perform a blank determination and make any necessary correction. transfer to a 200-mL Erlenmeyer flask and dissolve in 10 mL of ethanol. soluble in dioxane.30 mL.0 g of Cholesterol in a flask. add 5 mL of sodium hydroxide TS.5 g of Cholesterol in a glass-stoppered flask.1 mol/L silver nitrate VS and shake well.10% (1 g). 60 o C .10% (1 g). add 3 to 4 drops of aniline and warm gently: the disagreeable odor of phenyl isocyanide (poisonous) is perceptible. pungent taste.071%). cool. Perform the test. Cool. sparingly soluble in dehydrated ethanol and practically insoluble in water. in vacuum. 100 mm) Melting Point Between 147 o C and 150 o C.1 mol/L sodium hydroxide VS consumed is not more than 0.0 mL of 0.0% (0. . boil under a reflux condenser for 10 minutes.05 mol/L sulfuric acid VS (indicator: 2 drops of phenolphthalein TS).65 Description Cholesterol is white to pale yellow crystal granule. Cholesterol gradually changes to a yellow to pale yellow-brown color by light.1 g of Chlorobutanol. 10 mL.2 g. (2) Take 0. Cinnamon Oil is the essential oil distilled with steam from the leaves and twigs or bark of Cnnamomum cassia Blume or from the bark of Cinnamomum zeylanicum Nees (Lauraceae). Each mL of 0. dissolve in 50 mL of warm ethanol and allow to stand at room temperature for 2 hours: no turbidity or deposit is produced. Titrate the excess silver nitrate with 0. Cholesterol H3C CH3 H3C H3C CH3 H H Identification (1) Dissolve 10 mg of Cholesterol in 1 mL of chloroform.01 mol/L hydrochloric acid VS by adding 25 mL of dilute ethanol. (2) Chloride⎯Dissolve 0.10 g of the pulverized Chlorobutanol with 5 mL of water: the solution is neutral. volumetric titration. shake well the mixture. add 40 mL of dilute nitric acid and 25. add 1 mL of sodium hydroxide TS. add 1 mL of sulfuric acid and shake: a red color develops in the chloroform layer and the sulfuric acid layer shows a green fluorescence.30% (1 g. Description Cinnamon Oil is a yellow to brown liquid. has a characteristic. 6 mL of dilute nitric acid and add water to make 50 mL (not more than 0.5 g of Chlorobutanol in 25 mL of dilute ethanol and add 6 mL of dilute nitric acid and water to make 50 mL. Cinnamon Oil is clearly miscible with ethanol. Part II Identification (1) Take 5 mL of a solution of Chlorobutanol (1 in 200). Cinnamon Oil is practically insoluble in water. Residue on Ignition Not more than 0. dioxane.0 mL of 0. Perform a blank determination and make any necessary correction: the volume of 0.1164 Monographs.1 mol/L sodium hydroxide VS and shake for 1 minute.1 g of Chlorobutanol. add 10. aromatic odor and a sweet. Evaporate the ether and boil for 5 minutes. Cinnamon Oil contains not less than 60% of the total aldehydes. Packaging and Storage tight containers. Add 3 mL of nitrobenzene and shake vigorously until the precipitate is coagulated.2 g. is odorless or has slight odor and is tasteless. Preserve in light-resistant. Residue on Ignition Not more than 0. (2) Acid⎯Place 1. 4 hours).0 mL of 0.1 mol/L silver nitrate VS = 5. dissolve in 10 mL of ether. Preserve in light-resistant. Coconut Oil Clove Oil Clove Oil is the volatile oil distilled with steam from the flower buds or leaves of Syzygium aromaticum Merrill et Perry (Myrtaceae). add 20 mL of boiling water. Saponification Value Between 246 and 264. warm for 10 minutes on a water-bath with occasional shaking. Packaging and Storage Preserve in tight containers.5　 (100 mm) Specific Gravity 20 : Between 1. add 70 mL of sodium bisulfite TS and heat the mixture on a water-bath with frequent shaking to dissolve completely. add sodium bisulfite TS to raise the lower level of the oily layer within the graduate volume of the neck.537.0 mL of clove Oil according to Method 2.0 mL of Clove Oil in a Cassia flask. Assay Pipet 5.0 mL of Cinnamon Oil with 5 mL of ethanol. To this solution.2. Total eugenol (%) = [10 . Acid Value Not more than 0. Specific Optical Rotation [α ] 20 D : Between 0 and - Coconut oil is the fixed oil obtained from the seeds of Cocos nucifera Linné (Palmae). characteristic odor and mild taste. has a slight.040 and 1.0 mL of standard lead solution (not more than 40 ppm). Identification Shake 4 drops of Cinnamon Oil with 4 drops of nitric acid: the mixture forms white to pale yellow crystals at a temperature below 5 o C .(volume of separated oily layer)] × 20 Packaging and Storage tight containers. add 70 mL of sodium hydroxide TS. shake vigorously. Unsaponifiable Matter Not more than 1.527 and 1. Clove Oil contains not less than 80. Description Clove Oil is colorless or pale yellowbrown. Refractive Index nD20 : Between 1. clear liquid. Coconut Oil is practically insoluble in water.0vol% of total eugenol. shake for 5 minutes. Total aldehydes (%) = [5. Coconut Oil is freely soluble in ether and in petroleum ether. (2) Water-soluble phenol　Take 1. (2) Dissolve 2 drops of Clove Oil in 4 mL of ethanol and add 1 to 2 drops of ferric chloride TS: a green color is produced. Melting point⎯Between 20 °C and 28 °C (Method 2). Purity (1) Rosin⎯Mix 1. saturated ethanol solution of lead acetate: no precipitate is produced. Clove Oil acquires a brown color upon aging or by air. and perform the test. It has characteristic aroma and burning taste. Cinnamon Oil darkens and becomes viscous. then add 3 mL of freshly prepared. Preserve in light-resistant. Assay Take 10. Description Coconut Oil is a white to pale yellow mass. filter the aqueous layer after cooling and add 1 to 2 drops of ferric chloride TS: a yellow-green. (3) Heavy metals　Proceed with 1.0 mL of diluted ethanol (7 in 10): the solution is clear. Corn Oil .(volume of separated oily layer)] × 10 Packaging and Storage tight containers. d 20 Purity (1) Clarity of solution　Dissolve 1. Prepare the control solution with 4. Coconut Oil congeals to a hard and brittle solid. add 10 mL of calcium hydroxide TS and shake vigorously: the oil forms a flocculent mass and a white to pale yellow color develops. (2) Heavy metals⎯Proceed with 1. or colorless or pale yellow.0 mL of Standard Lead Solution (not more than 40ppm).KP VIII 1165 Upon aging or long exposure to air. Prepare the control solution with 4.0%.068.0 . Measure the volume (mL) of the separated oily layer. Iodine Value Between 7 and 11.010 and 1. 1. At a temperature below 15 °C.0 mL of Clove Oil in 2. Identification (1) Take 5 drops of Clove Oil. color develops. clear oil. Allow to stand for 2 hours and measure the volume (mL) of the separated oily layer. Clove Oil is miscible with ethanol or with ether.0 g of Cinnamon Oil according to Method 2 and perform the test. add sodium hydroxide TS to the volume after cooling and allow to stand for 18 hours.0 mL of Clove Oil. Clove Oil is slightly soluble in water. but no blue or violet. 20 Specific gravity⎯ d 20 : Between 1.065.0 mL of Cinnamon Oil into a cassia flask. 2. Corn Starch is observed a black cross. Corn Oil is miscible with ether or with petroleum ether. d 20 Purity (1) Bases and hydrocarbons⎯Shake 1.915 and 0. or irregularly orbicular or spherical simple grains of about 25 to 35 μm in diameter.0 mL of creosote. Corn Oil is slightly soluble in ethanol and practically insoluble in water. Creosote is slightly soluble in water. Part II Corn Oil is the fixed oil obtained from the embryo of Zea mays Linné (Gramineae). pH Put 5.0% (1 g. At -7 o C . and allow to cool: a subtle white-turbid. (2) To 1 g of Corn Starch add 50 mL of water.076. Saturated solution of Cresote is neutral. Creosote is miscible with ethanol or with ether.0 mL of Creosote with 9 mL of sodium hydroxide TS: the solution is clear and does not darken.0 and 7. Description Corn Starch is a white to pale yellowish white mass or powder. shake and allow to stand: no blue or muddy brown color develops in the upper layer of the mixture and no red color develops in the lower layer. add 2 mL of petroleum benzin and 2 mL of barium hydroxide TS. Description Dextrin is a white or pale yellow. (2) Creosote made from phenol or coal-tar⎯Shake creosote with an equal volume of collodion: no coagulum is produced. Corn Starch Corn Starch is a starch granules obtained from the seeds of Zea mays Linné (Gramineae). Residue on Ignition Not more than 0. boil for 1 minute.05 mL of diluted iodine TS (1 in 10): an orange-red to deep blue color is formed and the color disappears by heating. Iodine Value Between 103 and 130. Identification Take 10 mL of a saturated solution of Creosote and add 1 drop of ferric chloride TS: a purple color develops and the solution becomes rapidly turbid and changes through blue and muddy green to brown.921. Creosote gradually changes in color by light or by air. its intersection point on hilum when grains are put between two nicol prisms fixed at right angle to each other. add 25. Cresote is highly refractive. Corn Starch is practically insoluble in water or in dehydrated ethanol. Add further 50 mL of water: the solution is practically clear. Preserve in light-resistant. and allow to stand for 15 minutes: the pH of the solution is between 4.0. . Identification (1) Under a microscope. appears as irregularly polygonal simple grains of about 2 to 23 μm in diameter.0 mL of freshly boiled and cooled water. (3) To 1 mL of the pasty liquid obtained in (2) add 0. Distilling Range Between 200 not less than 85%. mix gently for 1 minute. clear liquid. o C. Packaging and Storage tight containers. Hilum appears as distinct cave or 2 to 5 radial clefts. Description Creosote is colorless or pale yellow.1166 Monographs.0 g of Corn Starch in a non-metal vessel. Specific Gravity 20 : Not less than 1. Packaging and Storage Preserve in tight containers. Creosote has characteristic odor and buring taste. (3) Other impurities⎯Take 1. pale yellow oil. Unsaponifiable Matter Not more than 1. Creosote Creosote is a mixture of phenols obtained from wood tar. Description Corn Oil is a clear. concentric striation absent. 130 90 minutes). pasty liquid is formed. o C and 220 o C.5%. Corn Oil congeals to an unguentary mass. Saponification Value Between 187 and 195. Corn Starch. 25 Specific gravity⎯ d 25 : Between 0. is odorless or has slight odor and mild taste. Acid Value Not more than 0. Dextrin Purity Proceed as directed in the Purity under Wheat Starch.6% (1 g) Packaging and Storage Preserve in well-closed containers. Loss on Drying Not more than 15. preserved in a mixture of water and glycerin (1 : 1). 0 g of Dextrin.1 mol/L sodium hydroxide TS: a red color develop.5% (0.0% and not more than 101. Prepare the control solution with 2. dissolve by heating. add 1 drop of iodine TS: a pale red-brown or pale red-purple color develops. and does not irritate the tongue. add 1 mL of dilute hydrochloric acid and add water to make 50 mL and perform the test.35 mL of 0. Loss on Drying Not more than 10% (0.0 g of Dibasic Sodium Phosphate Hydrate. Dibasic Sodium Phosphate Hydrate Na2HPO4·12H2O: 358. (7) Heavy metals⎯Proceed with 0.1 g of Dextrin. then at 105 o C for 5 hours). add water to make 50 mL. Purity (1) Clarity and color of solution⎯Dissolve 1. Purity (1) Clarity and color of solution⎯Take 2. add water to make 100 mL and filter. characteristic odor and a sweet taste. Identification Take 0.038%) (4) Carbonate⎯Take 2. shake and filter. (2) Acid⎯Take 1.01 mol/L hydrochloric acid (not more than 0. the turbidity is not more than that of the following control solution.005 mol/L sulfuric acid.14 Dibasic Sodium Phosphate Hydrate. add 1 mL of acetic acid and filter. Prepare the control solution with 0. 4 hours).0 g of Dextrin in a Nessler tube and 40 mL of water.0 and 9.0% and 61. Residue on Ignition Not more than 0.5 g. clear and even if turbid. when dried. Dibasic Sodium Phosphate Hydrate is freely soluble in water and practically insoluble in ethanol or in ether.0% (10 g.KP VIII 1167 amorphous powder or granule. 105 o C .0 mL of 0.50 mL of 0.96) Description Dibasic Sodium Phosphate Hydrate is colorless or white crystal and is odorless. dissolve by heating.013%). (2) Chloride⎯Dissolve 1. Perform the test. if necessary.0 g of Dibasic Sodium Phosphate Hydrate according to Method 1 and perform the test (not more than 2 ppm). Packaging and Storage Preserve in well-closed containers. and add 2 mL of hydrochloric acid: no foam is produced.40 mL of 0. boil. Perform the test using this solution as the test solution. Control solution⎯Take 1. Prepare the control solution with 0.5 g of Dextrin according to Method 2 and perform the test. To 5 mL of the filtrate. dissolve by heating. Loss on drying Between 57. Dibasic Sodium Phosphate Hydrate effloresces in warm. add 5 mL of water.0 mL of standard lead solution by adding 2 mL of dilute acetic acid and water to make 50 mL (not more than 10 ppm). has a slight. (3) Sulfate⎯Dissolve 0. (5) Heavy metals⎯Dissolve 2. add 5 drops of calcium chloride TS: no turbidity is produced immediately.0 g of Dibasic Sodium Phosphate Hydrate in 50 mL of water: the pH of this solution is between 9. dissolve by heating. contains not less than 98. soluble in water and practically insoluble in ethanol or in ether. add 5 mL of water. Prepare the control solution with 0. add 100 mL of water.30 mL of 0.01 mol/L hydrochloric acid VS (not more than 0. To 5 mL of the filtrate.40 mL of 0.0 g of Dibasic Sodium Phosphate Hydrate in 7 mL of dilute nitric acid.5 g of Dibasic Sodium Phosphate Hydrate in 2 mL of dilute hydrochloric acid and add water to make 50 mL. Perform the test using this solution as the test solution.0 g of Dibasic Sodium Phosphate Hydrate in 20 mL of water: the solution is clear and colorless. 46 mL of water and 2 mL of barium chloride TS. Perform the test using this solution as the test solution. Prepare the control solution with 0. cool.005 mol/L sulfuric acid VS (not more than 0.5 mL of standard lead solution (not more than 50 ppm). at 40 o C for 3 hours at first. . Dextrin is freely soluble in boiling water. cool.5 g). add 5 drops of ammonium oxalate TS: no turbidity is immediately produced. allow to stand for 10 minutes and shake before use.014%). add 80 mL of water.0 g of Dextrin. dry air.005 mol/L sulfuric acid (not more than 0.0% of Dibasic Sodium Phosphate (Na2HPO4: 141.4.019%). Identification A solution of Dibasic Sodium Phosphate Hydrate (1 in 10) responds to the Qualitative Tests (1) and (2) for sodium salt and the Qualitative Tests for phosphate. (5) Oxalate⎯Take 1. add 20 mL of water. cool and add 1 drop of phenolphthalein TS and 0. add 1 mL of dilute hydrochloric acid. cool and add water to make 50 mL: the solution is colorless or pale yellow. (6) Calcium⎯Take 5 mL of the filtrate obtained in (5). cool. (6) Arsenic⎯Prepare the test solution with 1.0 g of Dibasic Sodium Phosphate Hydrate in 4 mL of acetic acid and add water to make 50 mL.0 g of Dextrin. pH Dissolve 1. Prepare the control solution with 2. (3) Chloride⎯Take 2. (4) Sulfate⎯Take 45 mL of the filtrate obtained in (3). Take 40 mL of the filtrate and add 6 mL of dilute nitric acid and add water to make 50 mL. Separately.07 Ethanol contains not less than 95. the peak area of acetal. as directed in the liquid film method disk method under the Infrared Spectrophotometry. and use this solution as the standard solution (2).816.9vol% (by specific gravity) of Ethanol (C2H6O) at 15 o C . and maintain at a constant temperature of about 240 o C for 10 minutes.0 mL of Ethanol add water to make 20 mL. in 50 mL of water. add Ethanol to make exactly 50 mL and use this solution as the standard solution (4). d15 Purity (1) Clarity of solution—Ethanol is clear and colorless. the sum of acetaldehyde and acetal as acetaldehyde is not more than 10 vol ppm. Part II Assay Dissolve about 3. (3) Volatile impurities—Pipet exactly 500 mL of Ethanol. Identification Determine the infrared spectra of Ethanol and Ethanol RS. Description Ethanol is clear. coated with 6% cyanopropyl phenyl-94% dimethyl silicone polymer for gas chromatography in 1. C E obtained with Ethanol. Column temperature: Inject at a constant temperature of about 40 o C . then raise up to 240 o C at the rate of 10 o C per minute. pipet 100 μL of this solution. A T with the standard solution (2). Titrate with 0. and the amount of benzene is not more than 2 vol ppm. To 1.01 mol/L sodium hydroxide VS to this solution: a light red color develops. The total area of the peaks other than the peak mentioned above and the peak having the area not more than 3% of 4-methylpentan-2-ol is not more than the peak area of 4-methylpentan-2-ol. and the peak area of methanol with the standard solution (1).32 mm in inside diameter and 30 m in length. Ethanol is miscible with water.1 mL of a solution prepared by addition of 7. to exactly 50 μL each of anhydrous methanol and acetaldehyde add Ethanol to make exactly 50 mL. Ethanol is flammable and burns with a pale blue flame on ignition. When calculate the amounts of the volatile impurities by the following equation.5 mol/L sulfuric acid VS keeping at 15 o C until the color of the solution changes from green to dark-greenish red-purple (indicator: 3 to 4 drops of methyl orange-xylenecyanol FF TS). Perform the test with exactly 1μL each of the sample solution and the standard solutions (1).0 mL of ethanol and 20 mL of water to 1.809 and 0. A E . Seperately. BT : the peak area of methanol is not more than 1/2 times the peak area of methanol with the standard solution (1). respectively: both spectra exhibit similar intensities of absorption at the same wavenumbers. Pipet exactly 5 mL of this solution. Separately.5 mol/L sulfuric acid VS = 141. and use this solution as the standard solution (1). Operation conditions Detector: A hydrogen flame-ionization detector Column: A fused silica tube 0. colorless liquid. add Ethanol to make exactly 50 mL. Specific Gravity 15 : Between 0.1vol% and not more than 96. to exactly 150 μL of acetal add Ethanol to make exactly 50 mL. (3) and (4) as directed under Gas Chromatography according to the following conditions. Total amount (vol ppm) of acetaldehyde and acetal = [(10 × A E ) /(A T − A E )] + [(30 × C E ) /(C T − C E )] Amount (vol ppm) of benzene = 2 B E /(B T − B E ) If necessary. (2).1168 Monographs. Each mL of 0. benzene. previously dried. to exactly 100 μL of benzene add Ethanol to make exactly 100 mL. and allow to stand for 5 minutes: the resulting liquid is clear. To exactly 100 μL of this solution add Ethanol to make exactly 10 mL. identify the peak of benzene by using a different stationary liquid phase and suitable chromatographic conditions. BE and acetal. Separately.0 g of Dibasic Sodium Phosphate Hydrate.96 mg of Na2HPO4 Packaging and Storage Preserve in tight containers. Ethanol is volatile. (2) Acid or alkali –To 20 mL of Ethanol add 20 mL of freshly boiled and cooled water and 0. to 100 μL of anhydrous methanol add Ethanol to make exactly 50 mL.8 μm thickness. Add 1. To exactly 100 μL of this solution add Ethanol to make exactly 10 mL. add 150 μL of 4-methylpentan-2-ol. Ethanol CH3CH2OH Alcohol C2H6O: 46. the peak area of aldehyde.0 mL of phenolphthalein: it is colorless. previously dried and accurately weighed.0 mL of 0. and use this solution as the standard solution (3). maintain the temperature for 12 minutes. and determine the peak areas of acetaldehyde. has characteristic odor and burning taste. Carrier gas: Helium Flow rate: 35 cm/sec Split ratio: about 1 : 20 System suitability System performance : When the procedure is run with 1 μL of the standard solution (2) under the above oper- . CT with the standard solution (3) and the peak area of benzene. and use this solution as the sample solution. with occasional shaking: no color is produced in the ether layer and the aqueous layer. Disodium Edetate Hydrate Ether . clear. shake gently.KP VIII 1169 ating conditions. and shake well: no color is produced in the ether layer and in the aqueous layer. with the formation of peroxides.0 mg. Anhydrous Ethanol is volatile. may explode violently. Description Anhydrous Ethanol is a clear. Packaging and Storage Preserve in light-resistant. Anhydrous Ethanol CH3CH2OH Dehydrated Ethanol Dehydrated Alcohol C2H6O: 46. shake for 1 minute.5 mL of phenolphthalein TS in a glass-stoppered flask. stopper the flask. and allow to evaporate spontaneously to a volume of about 1 mL: no foreign odor is perceptible.5 mg. (4) Other impurities (absorbance)—Perform the test with Ethanol as directed under Ultraviolet-visible spectrophotometry: the absorbances at 240 nm. CH3CH2OCH2CH3 Diethyl ether C4H10O: 74.02 mol/L sodium hydroxide VS with shaking: a red color develops. (4) Peroxide—Place 10 mL of Ether in a Nessler tube. Ether cannot be used for anesthesia. colorless liquid. Boiling point⎯Between 78 o C and 79 o C .10. and add 0.07 Anhydrous Ethanol contains not less than 99. The absorption spectrum determined in a 5 cm cell using water as a blank shows a flat absoption curve between 235 nm and 340 nm. (3) Aldehyde—Place 10 mL of Ether in a Nessler tube. Store with avoidance of fire. Description Ether is a colorless. mobile liquid. Ether contains a small quantity of ethanol and water. then add 1 mL of starch TS. Add 25 mL of Ether. Specific Gravity 20 : Between 0. add 1 mL of freshly prepared solution of potassium iodide (1 in 10). add 1 mL of potassium hydroxide TS. Store at not exceeding 25 o C with avoidance of fire.12 Ether contains not less than 96. Ether is soluble in water. Ether is highly volatile and flammable.40. evaporate in a tared dish on a water bath.5. tight containers. Store with avoidance of fire. Boiling point—Between 35 o C and 37 o C . (5) Residue on evaporation—Pipet exactly 100 mL of Ethanol. Anhydrous Ethanol is miscible with water. Ether is slowly oxidized by the action of air and light. has characteristic odor.794 ~0.02 mol/L sodium hydroxide VS dropwise to produce a red color which persists after shaking for 30 seconds.5vol% (by specific gravity) of ethanol (C2H6O) at 15 o C .40 mL of 0. tight containers. d15 Purity Proceed as directed in the Purity under Ethanol. and dry for 1 hour at 105 o C : the mass of the residue does not exceed 2. respectively. and 0. Packaging and Storage Preserve in light-resistant. without filled up. between 250 nm and 260 nm and between 270 nm and 340 nm are not more than 0. tight containers. 0. Ether is miscible with ethanol. acetaldehyde and methanol are eluted in this order with the resolution between these peaks being not less than 1. d 20 Purity (1) Foreign odor—Place 10 mL of Ether in an evaporation dish.30. and add 0.0% (by specific gravity) of ether (C4H10O).718 and 0.797. odorless filter paper to evaporate the ether: no foreign odor is perceptible. Drop this residue onto a piece of clean. and allow the mixture to stand for 2 hours. protecting from light. (2) Acid—Place 10 mL of diluted ethanol (4 in 5) and 0.0% and not more than 98. Anhydrous Ethanol is flammable and burns with a pale blue flame on ignition.721. Vapor of Ether. Packaging and Storage Preserve in light-resistant. and dry the residue at 105 o C for 1 hour: the residue is not more than 1. Identification Proceed as directed in the Identification under Ethanol. (5) Residue on evaporation—Evaporate 140 mL of Ether. when mixed with air and ignited. Specific Gravity 15 : 0. Part II HOOCH2C CH2COOH NCH2CH2N NaOOCH2C 2 H2O CH2COONa Disodium Ethylenediaminetetraacetate EDTA Sodium C10H14N2Na2O8·2H2O: 372.0 g of Disodium Edetate Hydrate according to Method 2 and perform the test. Ethylenediamine is gradually affected by air.5 g of Disodium Edetate Hydrate in 20 mL of water and add 1 mL of dilute hydrochloric acid: a white precipitate is produced. wash with 50 mL of water and dry at 105 o C for 1 hour: the precipitate melts between 240 o C and 244 o C (with decomposition).0% of disodium edetate hydrate (C10H14N2Na2O8·2H2O).7 and titrate with 0. Prepare the control solution with 2.0% (1 g). pH 6. 20 Specific gravity⎯ d 20 : About 0. Assay Weigh accurately about 1. with ethanol or with ether. Place 15 mL of 0. Transfer 20 mL of the test solution to a glassstoppered test tube.5 mol/L sodium hydroxide VS in a 100-mL measuring cylinder. Mix well with 5 mL of pyridine-pyrazolone TS and allow to stand between 20 o C and 30 o C for 50 minutes: the solution is not more intense than the following control solution. dissolve in 100 mL of water.5 mol/L sodium hydroxide VS and add water to make exactly 1000 mL. dissolve in 50 mL of water. (4) Arsenic⎯Prepare the test solution with 1.0 g of Disodium Edetate Hydrate in 100 mL of water: the pH of this solution is between 4. is odorless and has a slightly acidic taste.224mg of C10H14N2Na2O8. (3) Take 40 mg of Ethylenediamine. Residue on Ignition Between 37. Dissolve the precipitate in 8 mL of ethanol by warming.0 g of Disodium Edatate Hydrate.0 g of Disodium Edetate Hydrate in 50 mL of water: the solution is clear and colorless.0% and not more than 101. Preserve in well-closed Ethylenediamine H 2 NCH 2 CH 2 NH 2 C2H8N2: 60. Ethylenediamine is miscible with water. Identification (1) A solution of Ethylenediamine (1 in 500) is alkaline. Description Disodium Edetate Hydrate is white crystal or crystalline powder.3 and 4.2H2O Packaging and Storage containers. Ethylenediamine has a caustic nature and an irritating property. wash with water. which is used as a receiver and immerse the top end of the condenser into the solution. . (2) Dissolve 0.0 g of Disodium Edetate Hydrate to a round-bottomed flask. colorless to pale yellow liquid. collect the white precipitate formed and wash with water. Identification (1) Dissolve 10 mg of Disodium Edetate Hydrate in 5 mL of water.0 mL of diluted chloramine TS (1 in 5). promptly add 8 mL of water. neutralize with dilute acetic acid and add 5 mL of phosphate buffer solution. (3) A solution of Disodium Edetate Hydrate (1 in 20) responds to the Qualitative Tests (1) for sodium salt. add 2 mL of a solution of potassium chromate (1 in 200) and 2 mL of arsenic trioxide TS and heat on a water-bath for 2 minutes: a purple color develops. (2) Cyanide⎯Transfer 1.0 mL of standard cyanide solution. Purity (1) Clarity and color of solution⎯Dissolve 1. warm for 2 to 3 minutes with occasional shaking. add 2 mL of ammonia-ammonium chloride buffer solution. Immediately stopper the tube.0 mL of standard lead solution (not more than 10 ppm). has an ammonia-like odor.1mol/L zinc VS = 37. cool.898. Distil the mixture until the distillate measures 100 mL and use this solution as the test solution. pH Dissolve 1.10 Ethylenediamine contains not less than 97. and 1. mix gently and allow to stand for a few minutes. filter the crystals. Control solution⎯Pipet exactly 1. add 1 drop of phenolphthalein TS.24 Disodium Edetate contains not less than 99. add 6 drops of benzoyl chloride and 2 mL of a solution of sodium hydroxide (1 in 10).1170 Monographs.0 g of Disodium Edetate Hydrate according to Method 1 and perform the test (not more than 2 ppm).0% of ethylenediamine (C2H8N2). Description Ethylenediamine is clear. add 10 mL of phosphoric acid and distil. Collect the precipitate. (3) Heavy metals⎯Proceed with 2. Disodium Edetate Hydrate is soluble in water and practically insoluble in ethanol or in ether.0 and 39.1 mol/L zinc VS until the color of the solution changes from blue to red. pH 10.0% and not more than 101. transfer 20 mL of this solution to a glass-stoppered test tube and proceed as directed for the test solution. (2) Take 2 mL of cupric sulfate TS and add 2 drops of Ethylenediamine: a blue-purple color develops.7.8. add 15 mL of 0. and dry at 105 o C for 1 hour: the melting point is between 247 o C and 251 o C . (Indicator: 40 mg of eriochrome black T-sodium chloride indicator) Each mL of 0. Eucalyptus Oil Eucalyptus Oil is the essential oil distilled with steam from the leaves of Eucalyptus globulus Labillardiere or allied plants (Myrtaceae).0% of cineole (C10H18O: 154.0 mL of Eucalyptus Oil with 5 mL of diluted ethanol (7 in 10): the solution is clear. weigh accurately about 0. Specific Gravity 20 : Between 0. (2) Heavy metals⎯Proceed with 1. Packaging and Storage tight containers. System suitability⎯ System performance: Dissolve 0. Description Exsiccated Gypsum is a white to grayish white powder and is odorless and tasteless. Carrier gas: Nitrogen.0 mL of Standard Lead Solution (not more than 40 ppm). Distilling Range Between 114 not less than 95vol%. about 3 mm in inside diameter and about 5 m in length.KP VIII 1171 Purity (1) Heavy metals⎯Place 1. When the procedure is run with 2 μL of the standard solution under the above operating conditions. o C and 119 o C. Pipet exactly 5 mL of this solution.1 g of Eucalyptus Oil and dissolve in hexane to make exactly 25 mL. Refractive Index nD20 : Between 1. of the peak area of cienol to that of the internal standard of each solutions. To 1 mL of this solution. Each mL of 1 mol/L hydrochloric acid VS = 30.0 mg.1 g of Cineol RS. Operating conditions Detector: A hydrogen flame-ionization detector. limonene and cineol are eluted in this order with a resolution between their peaks being not less than 1. Assay Weigh accurately about 0. and perform test. Exsiccated Gypsum Exsiccated Gypsum possibly corresponds to the formula CaSO4· 1/2H2O. heat on a water-bath to dryness and dry to a constant weight at 105 o C : the residue is not more than 3. respectively. Prepare the control solution with 2.0 mL of standard lead solution (not more than 20 ppm). tight and almost well-filled containers. (2) Residue on evaporation⎯Pipet exactly 5 mL of Ethylenediamine. Assay Weigh accurately about 0.049 mg of C2H8N2 Packaging and Storage Preserve in light-resistant. Flow rate: Adjust the flow rate so that the retention time of cineol is about 11 minutes. having alkylene glycol phthalate ester for gas chromatography coated at the ratio of 10% on silanized siliceous earth for gas chromatography (150 μm to 180 μm in particle diameter).458 and 1.927. has characteristic.7 g of Ethylenediamine in a glass-stoppered Erlenmeyer flask containing 25 mL of water. Amount (mg) of Cienol (C10H18O) = amount (mg) of Q Cienol RS × T QS Internal standard solution⎯A solution of anisol in hexane (1 in 250). colorless or pale yellow liquid.0 mL of Eucalyptus Oil according to Method 2. ignite at a low temperature until charred. then add hexane to make exactly 100 mL and use this solution as the test solution.5. Column: A glass column. Eucalyptus Oil contains not less than 70. add exactly 5 mL of the internal standard solution.0 g of Ethylenediamine in a porcelain crucible. aromatic odor and pungent taste. Description Eucalyptus Oil is clear. . evaporate to dryness on a water-bath. proceed according to Method 2 and perform the test.907 and 0. add hexane to make 20 mL. for the test solution and the standard solution. add 50 mL of water and titrate with 1 mol/L hydrochloric acid VS (indicator: 3 drops of bromphenol blue TS).1 g each of cineol and limonene in 25 mL of hexane. d 20 Purity (1) Clarity of solution⎯Mix 1. Perform the test with 2 μL each of the test solution and the standard solution as directed under the Gas Chromatography according to the following operating conditions.25). proceed as directed in the test solution and use this solution as the standard solution. Separately. Calculate the ratios. Exsiccated Gypsum is slightly soluble in water and practically insoluble in ethanol. Prepare the control solution with 4. Eucalyptus Oil is neutral. Preserve in light-resistant.470. cover loosely. Identification Shake 1 mL of Eucalyptus Oil vigorously with 1 mL of phosphoric acid and allow to stand: the solution congeals within 30 minutes. Column temperature: A constant temperature of about 120 o C . QT and QS . Exsiccated Gypsum absorbs moisture slowly on standing in air to lose its solidifying property. Identification (1) Dilute 2 mL of Formalin with 10 mL of water in a test tube and add 1 mL of silver nitrate-ammonia TS: a gray precipitate is produced. stir immediately for 3 minutes and allow to stand: the period necessary for water no longer to separate. (Illiciaceae).955 and 0. d 20 Purity (1) Clarity of solution⎯Take 1. Add water to make exactly 100 mL. add about 1 g of Formalin and weigh accurately again. Purity Acid⎯Dilute 20 mL of Formalin with 20 mL of water and add 5. Identification Dissolve 0.30 g of Fennel Oil in 20 mL of hexane. To this solution. Spot 5 μL of the test solution on a plate of silicagel with fluoroscenti indicator for thin-layer chromatography.0 mL of standard lead solution (not more than 40 ppm). Formalin is miscible with water or with ethanol. Part II When Exsiccated Gypsum is heated to yield an anhydrous compound at a temperature above 200 °C.0% of formaldehyde (CH2O: 30.0 mL of Fennel Oil and add 3 mL of ethanol: the solution is clear.0 mL of 0. Fennel Oil is miscible with ethanol or with ether.0 g of Exsiccated Gypsum. Preserve in light-resistant. after evaporation) Assay Weigh accurately a weighing bottle containing 5 mL of water. (2) Add 2 droops of Formalin to 5 mL of sulfuric acid in which 0. Fennel Oil Oleum Foeniculi Funnel Oil is the essential oil distilled with steam from the fruit of Foeniculum vulgare Miller (Umbelliferae) or of Illicium verum Hooker fil. Residue on Ignition Not more than 0. Solidification Take 10. Packaging and Storage Preserve in light resistant.1 mol/L sodium hydroxide VS and 2 drops of bromothymol blue TS: a blue color develops. To this mixture.528 and 1. Description Formalin is a clear and colorless liquid. or a silver mirror is formed on the wall of the test tube. tight containers. Formalin may become cloudy. Purity Alkali⎯Take 3.0% and not more than 38. and sue this solution as the test solution. add exactly 50 mL of 0. dark red color develops. white crystals or crystalline masses may often separate from the Fennel Oil. add 10 mL of water.1172 Monographs.4. Specific Gravity 20 : Between 0.05 mol/L iodine VS and 20 mL of potassium hydroxide TS and allow to stand for 15 minutes at an ordinary temperature.560.05 mol/L iodine VS = 1.1 g of salicylic acid has been dissolved. pipet 1 mL of this solution.0 mL of Fennel Oil according to Method 2 and perform the test. Refractive Index nD20 : Between 1.03). Examine under ultraviolet light (mail wavelength : 254 nm) : a main spot with a dark purple color appears at the Rf value of about 0. aromatic odor and sweet taste with slightly bitter aftertaste. Fennel Oil has characteristic. (2) Heavy metals⎯Proceed with 1. add hexane to make exactly 10 mL. and air-dry the plate. When stored for a long time. . Formalin Formalin contains not less than 35. Exsiccated Gypsum loses its solidifying property. When cold.995.5013 mg of CH2O Packaging and Storage tight containers. Vapor is irritating to the mucous membrane. Packaging and Storage Preserve in tight containers. Description Fennel Oil is colorless to pale yellow liquid. Fennel Oil is practically insoluble in water. is not more than 10 minutes from the time when water was first added.06% (5 mL. Pipet exactly 10 mL of this solution. Identification Shake 1 g of Exsiccated Gypsum with 20 mL of water for 5 minutes and filter: the filtrate responds to the Qualitative tests (2) and (3) for calcium salt and to the Qualitative Tests for sulfate. add 10 mL of water and 1 drop of phenolphthalein TS and shake vigorously: no red color develops. especially in a cold place. Each mL of 0.1 mol/L sodium thiosulfate VS (indicator: 1 mL of starch TS ). upon pressing with a finger. Perform a blank determination and make any necessary correction. add 15 mL of dilute sulfuric acid and titrate the excess iodine with 0. Perform the test with the test solution as directed under Thin-layer Chromatography. Develop the plate with a mixture of hexane and ethyl acetate (20 : 1) to a distance of about 10 cm. Prepare the control solution with 4. add 7 mL of ethanol: the solution remains clear. and warm the solution: a persistent. Formalin contains 5% to 13% of methanol to prevent polymerization.0 g of Exsiccated Gypsum in a glass-stoppered test tube. Collect the precipitates. Place the test solution in a test water bottle of the atomic absorption spectrophotometer. To this solution. Perform the test with 5 mL of this solution: the solution is not more intense than the following standard stain. Gelatin does not dissolve in water.5 g of dibasic sodium phosphate and allow to cool. granules or powder. neutralize with ammonia TS.0 g of Gelatin in a roundbottomed flask. Take about 1 g of Gelatin. (2) Sulfite　Take 20. add 20 mL of diluted sulfuric acid (1 in 2) and 100 mL of a solution of potassium permanganate (3 in 50). accurately weighed. Cool. ligament or tendon of animals.5 mg.0 and 9. add a solution of hydroxylamine hydrochloride (1 in 5) until the precipitate of manganese dioxide disappears. The raw collagen is obtained by acid or alkali treatment of the bone. heat until the excess of bromine is expelled.1 ppm). add further 5 mL of a solution of potassium permanganate (3 in 50). is clear. or only slightly opalescent and has no more color than Color Matching Fluid A. Determine the absorbance AT of the test solution at 253. heat gently under a reflux condenser and boil for 2 hours. . (2) Take 5 mL of a solution of Gelatin (1 in 5000) and add tannic acid TS drop-wise: the solution becomes turbid. Standard stain　Proceed with 15 mL of Standard Arsenic Solution. Loss on Drying Not more than 15. If the solution becomes clear during boiling. but slowly swells and softens when immersed in it. add water to make exactly 150 mL and use the solution as the test solution.0% (0.5 g). place 2. but the residue obtained from Gelatin for use in the preparation of capsules and tablets is not more than 75 mg. 5 mL of phosphoric acid and 1 g of sodium bicarbonate. dissolve in 150 mL of hot water and add 3 to 5 drops of silicone resin. allow to stand for 30 minutes with occasional shaking. (4) Arsenic　Take 15. evaporate to dryness on a water-bath with occasional shaking and dry the residue at 110 o C for 3 hours. add 30 mL of magnesia TS. immediately distil the solution.7 nm when the indication of the recorder has risen rapidly and become constant. Perform the test as directed under the Atomic Absorption Spectrophotometry (Cold vapor type). Packaging and Storage Preserve in tight containers. shreds. 5 to 10 times its own mass. o reduce the temperature of the solution to about 60 C . Attach a condenser. add 10 mL of stannous chloride-sulfuric acid TS. Determine the absorbance AS of the standard solution: AT is not more than AS (not more than 0. Add 15 mL of bromine TS. Purity (1) Foreign odor and water-insoluble substances　Dissolve 1. Acidify the distillate with hydrochloric acid. boil again and repeat the abovementioned procedure until the precipitate of manganese dioxide remains for about 20 minutes.1). is odorless and tasteless.0%. Gelatin derived from an acid-treated collagen exhibits an isoelectric point between pH 7. Wash the precipitates five times with 10 mL volumes of diluted ammonia TS (1 in 4) and dissolve in diluted hydrochloric acid (1 in 4) to make exactly 50 mL.0 mL of standard mercury solution a decomposition flask.0. Description Gelatin is colorless or white to pale yellow-brown sheets. in the same manner (not more than 1 ppm).0 g of Gelatin in a decomposition flask. Add 20 mL of water. skin. previously dried at 110 o C for 3 hours. add 1. add 20 mL of diluted sulfuric acid (1 in 2) and 100 mL of a solution of potassium permanganate (3 in 50) and proceed in the same manner as for the test solution.0 g of Gelatin in 40 mL of water by heating: the solution has no disagreeable odor. Prepare the control solution with 2. Identification (1) Take 5 mL of a solution of Gelatin (1 in 100) and add chromium trioxide TS or picric acid TS drop-wise: a precipitate is produced.0 and Gelatin derived from an alkali-treated collagen exhibits an isoelectric point between pH 4. gradually absorbing water. add 2 mL of barium chloride TS and heat on a water-bath until the color of iodine TS is discharged. in a weighed 200 mL beaked containing 10 g of sea sand (No. immersing the end of the condenser into a receiver containing 50 mL of iodine TS and continue the distillation until 50 mL of distillate is obtained. (3) Heavy metals　Proceed with 0.0 g of Gelatin in a flask. (5) Mercury　Place 2. Gelatin is very soluble in hot water and practically insoluble in ethanol or in ether. Separately.5 and 5. Perform a blank determination and make any necessary correction. connect the bottle immediately to the atomic absorption spectrophotometer and circulate air.KP VIII 1173 Gelatin Gelatin is a product prepared from aqueous extract of raw collagen by heating.5 g of Gelatin according to Method 2 and perform the test. add 60 mL of diluted hydrochloric acid (1 in 5) and heat until solution is dissolved. instead of Gelatin.5 mL of standard lead solution (not more than 50 ppm). Residue on Ignition Not more than 2. wash with water and ignite: the residue is not more than 4. allow to stand for 1 hour and collect the precipitates. Use chloroform instead of cyclohexane. is odorless and has a sweet taste.5 mg. Purified Gelatin derived from an acid-treated collagen exhibits an isoelectric point between pH 7.1 g of Glyceryl Monostearate in 2 mL of ethanol by warming. or tendon of animals. Residue on Ignition Not more than 2.0 g of Glyceryl Monostearate. waxy masses. 5 to 10 times its own mass.0.and βglyceryl monostearate and other fatty acid esters of glycerin. wash with water and ignite: the residue is not more than 1. Loss on Drying Not more than 15. Preserve in light-resistant. pellets or powder and is odorless and tasteless. Description Purified Gelatin is colorless to light yellow sheets. Glycine is freely soluble in water or in formic acid and practically insoluble in ethanol or in ether. Identification (1) Heat 0. (2) Sulfite　Take 20. Identification Proceed as directed in the Identification under Gelatin. thin flakes. add 2 mL of barium chloride TS and heat on a water-bath until the color of iodine TS is discharged.0 g of Purified Gelatin in a round-bottomed flask.0 mL of standard lead solution (not more than 20 ppm).0 g of Purified Gelatin according to Method 2 and perform the test. (4) Arsenic　Proceed as directed in the Purity Arsenic under Gelatin. Purity Acidity or alkalinity⎯Take 1. Glyceryl Monostearate is a mixture of α. Purified Gelatin is very soluble in hot water and practically insoluble in ethanol or in ether. or granules. heat with 5 mL of dilute sulfuric acid on a water-bath for 30 minutes and cool: a white to yellow solid is produced. Identification Determine the infrared spectra of Glycine and Glycine RS.2 g of Glyceryl Monostearat with 0. Packaging and Storage Preserve in tight containers.07 Glycine. (5) Mercury　Proceed as directed in the Purity Mercury under Gelatin. soluble in chloroform sparingly soluble in ether and practically insoluble in water or ethanol. Collect the precipitates.1174 Monographs.0% (0. Glyceryl Monostearate is slowly affected by light. Acidify the distillate by dropwise addition of hydrochloric acid. immediately distil the solution. Iodine Value Not more than 3. contains not less than 98. Proceed as directed in the Loss on drying under Gelatin. is a white crystal or crystalline powder. Purity (1) Foreign odor and Water-insoluble substances　Dissolve 1. Part II Purified Gelatin Glyceryl Monostearate Purified Gelatin is a product prepared from aqueous extract of raw collagen by heating.0. Saponification Value Between 157 and 170. colorless and disagreeable odor when the layer of the solution is 20 mm in depth. The raw collagen is obtained by acid or alkali treatment of the bone. Glycine H2NCH2COOH Aminoacetic Acid C2H5NO2: 75.0 and Purified Gelatin derived from an alkali-treated collagen has an isoelectric point at pH 4.10% (1 g). shreds.5 to 5. (2) Dissolve 0. add 20 mL of boiling water and cool with swirling: the solution is neutral.5% and not more than 101. previously dried. has a characteristic odor and taste.0%. as directed in . Prepare the control solution with 2. This separated solid dissolves when shaken with 3 mL of ether.0% of glycine (C2H5NO2).0 g of Purified Gelatin in 40 mL of water by heating: the solution is clear. skin.0 and 9. 5 mL of phosphoric acid and 1 g of sodium bicarbonate. when dried. Description Glycine. but slowly swells and softens when immersed in water and absorbs water.5 g). Acid Value Not more than 15. dissolve in 150 mL of hot water and add 3 to 5 drops of silicone resin. Purified Gelatin does not dissolve in water. immersing the end of the condenser into a receiver containing 50 mL of iodine TS and continue the distillation until 50 mL of distillate is obtained. ligament. Glyceryl Monostearate is very soluble in hot ethanol. Residue on Ignition Not more than 0. Attach a condenser. (3) Heavy metals　Proceed with 1. Melting Point Not less than 55 o C (Method 2). Packaging and Storage tight containers.5 g of potassium bisulfate until thoroughly charred: the irritative odor of acrolein is perceptible. Perform a blank determination and make any necessary correction. Description Glyceryl Monostearate is white to pale yellow. KP VIII 1175 the potassium bromide disk method under the Infrared Spectrophotometry: both spectra exhibit similar intensities of absorption at the same wavenumbers. If any difference appears between the spectra, dissolve each with water, evaporate the water to dryness, and repeat the test with the residue. termination and make any necessary correction. Each mL of 0.1 mol/L perchloric acid VS = 7.507 mg of C2H5NO2 Packaging and Storage Preserve in well-closed containers. pH Dissolve 1.0 g of Glycine in 20 mL of water: the pH of this solution is between 5.6 and 6.6. Purity (1) Clarity and color of solution⎯Dissolve 1.0 g of Glycine in 20 mL of water: the solution is clear and colorless. (2) Chloride⎯Proceed with 1.5 g of Glycine and perform the test. Prepare the control solution with 0.30 mL of 0.01 mol/L hydrochloric acid VS (not more than 0.021%). (3) Sulfate⎯Proceed with 0.6 of Glycine and perform the test, Prepare the control solution with 0.35 mL of 0.005 mol/L sulfuric acid VS (not more than 0.028%). (4) Ammonium⎯ Proceed with 0.25 g of Glycine and perform the test. Prepare the control solution with 5.0 mL of standard ammonium solution (not more than 0.02%). (5) Heavy metals⎯Proceed with 1.0 g of Glycine according to Method 4 and perform the test. Prepare the control solution with 2.0 mL of standard lead solution (not more than 20 ppm). (6) Arsenic⎯Prepare the test solution with 1.0 g of Glycine according to Method 1 and perform the test (not more than 2 ppm). (7) Related substances⎯Dissolve 0.10 g of Glycine in 25 mL of water and use this solution as the test solution. Pipet 1.0 mL of the test solution and add water to make exactly 50 mL. Pipet 5.0 mL of this solution, add water to make exactly 20 mL and use this solution as the standard solution. Perform the test with the test solution and the standard solution as directed under the Thinlayer Chromatography. Spot 5 μL each of the test solution and the standard solution on a plate of silica gel for thin-layer chromatography. Develop the plate with a mixture of n-butanol, water and glacial acetic acid (3 : 1 : 1) to a distance of about 10 cm and dry the plate at 80 o C for 30 minutes. Spray evenly a solution of ninhydrin in acetone (1 in 50) and heat at 80 o C for 5 minutes: the spots other than the principal spot from the test solution are not more intense than the spot from the standard solution. Loss on Drying Not more than 0.3% (1 g, 105 3 hours). o C, Residue on Ignition Not more than 0.10% (1 g). Assay Weigh accurately about 0.15 g of Glycine, previously dried, dissolve in 3 mL of formic acid, add 50 mL of glacial acetic acid and titrate with 0.1 mol/L perchloric acid VS (potentiometric titration, Endpoint Detection Method in Titrimetry). Perform a blank de- Honey Mel Honey is the saccharine substances obtained from the honeycomb of Apis mellifera Linné or Apis indica Radoszkowski (Apidae). Description Honey is a pale yellow to pale yellowbrown, syrupy liquid. Usually Honey is transparent, but often opaque with separated crystals. Honey has a characteristic odor and a sweet taste. Specific Gravity Mix 50.0 g of Honey with 100 mL 20 , is not less than 1.111. of water: d 20 Purity (1) Acid—Weigh 10 g of Honey, dissolve in 50 mL of water and neutralize with l mol/L potassium hydroxide TS (indicator: 2 drops of phenolphthalein TS): not more than 0.5 mL is required. (2) Sulfate—Mix 1.0 g of Honey with 2.0 mL of water and filter. To the filtrate, add 2 drops of barium chloride TS: the solution does not change immediately. (3) Ammonia-coloring substances—Mix 1.0 g of Honey with 2.0 mL of water and filter. To the filtrate, add 2 mL of ammonia TS: the solution does not change immediately. (4) Resorcin-coloring substances—Weigh 5.0 g of Honey, add 15 mL of ether, mix by shaking, filter and evaporate the ether solution at ordinary temperature. To the residue, add l to 2 drops of resorcin TS: a yellowred color may develop in the solution of resorcin and in the residue and a red to red-purple color which does not persist more than l hour. (5) Starch or dextrin—(i) Shake 7.5 g of Honey with 15 mL of water, warm the mixture on a water-bath and add 0.5 mL of tannic acid TS. After cooling, filter and to 1.0 mL of the filtrate, add 1.0 mL of dehydrated ethanol containing 2 drops of hydrochloric acid: no turbidity is produced. (ii) Weigh 2.0 g of Honey, add 10 mL of water, warm in a water-bath, mix and allow to coo1. Shake 1.0 mL of the mixture with l drop of iodine TS: no blue, green or red-brown color develops. (6) Foreign matter—Mix 1.0 g of Honey with 2.0 mL of water, centrifuge the mixture and examine the precipitate microscopically: no foreign substance except pollen grains is observable. Ash Not more than 0.4%. 1176 Monographs, Part II Packaging and Storage Preserve in tight containers. Hydrogenated Oil Hydrogenated Oil is the fat obtained by hydrogenation of fish oil or of other oils originating from animal or vegetable. Description Hydrogenated Oil is a white mass or powder, has a characteristic odor and a mild taste. Hydrogenated Oil is freely soluble in ether, very slightly soluble in ethanol and practically insoluble in water. Only the oil obtained by hydrogenation of castor oil is slightly soluble in ether, very slightly soluble in ethanol and practically insoluble in water. Acid Value Not more than 2.0. Purity (1) Moisture and coloration⎯Proceed as directed in the Purity (1) under Beef Tallow. (2) Alkali⎯Proceed as directed in the Purity (2) under Beef Tallow. (3) Chloride⎯Proceed as directed in the Purity (3) under Beef Tallow. (4) Heavy metals⎯Take 2.0 g of Hydrogenated Oil, add 5 mL of dilute hydrochloric acid and 10 ml of water, heat on a water-bath for 5 minutes with occasionally shaking. Filter after cooling, make slightly alkaline with 5 ml of ammonia TS to the filtrate and add 3 drops of sodium sulfide: the solution does not change. (5) Nickel⎯Place 5.0 g of Hydrogenated Oil in a quartz or porcelain crucible, heat slightly with caution at the beginning and after carbonization, incinerate by strong heating (500 ± 20 °C). After cooling, add 1 mL of hydrochloric acid, evaporate on a water-bath to dryness, dissolve the residue in 3 mL of dilute hydrochloric acid and add 7 mL of water. Add 1 mL of bromine TS and 1 mL of a solution of citric acid (1 in 5), make alkaline with 5 mL of ammonia TS and cool in running water. To this solution, add 1 mL of dimethyl-glyoxime TS, add water to make 20 mL and use this solution as the test solution. Allow to stand for 5 minutes: the solution has no more color than the following control solution. Control solution⎯Evaporate 1 mL of hydrochloric acid on a water-bath to dryness, add 1 mL of standard nickel solution and 3 mL of dilute hydrochloric acid and add 6 mL of water. Proceed as directed in the test solution, add water to make 20 mL and allow to stand for 5 minutes. Residue on Ignition Not more than 0.1% (5 g). Packaging and Storage Preserve in well-closed containers. Hydroxypropylcellulose Hydroxypropylcellulose is a hydroxypropyl ether of cellulose. Hydroxypropylcellulose, when dried, contains not less than 53.4% and not more than 77.5% of hydroxypropoxyl group (-OC3H6OH: 75.09). Description Hydroxypropylcellulose is a white to yellowish white powder and is odorless. Hydroxypropylcellulose practically insoluble in ether. Hydroxypropylcellulose forms a viscous liquid upon addition of water or ethanol. Identification (1) Take 1 g of Hydroxypropylcellulose, add 100 mL of water, heat on a water-bath at 70 o C for 5 minutes with stirring and cool while shaking. Allow to stand at room temperature until it becomes more homogeneous and viscous and use this solution as the test solution. To 2 mL of the test solution, add 1 mL of anthrone TS gently: a blue to green color develops at the zone of contact. (2) Heat the test solution obtained in (1): white turbidity or white precipitate is produced and the turbidity or the precipitate disappears when cooled. (3) Take 1 g of Hyddroxypropylcellulose, add 100 mL of ethanol and allow to stand after stirring: a homogeneous and viscous liquid is produced. pH Dissolve 1.0 g of Hydroxypropylcellulose in 50 mL of freshly boiled and cooled water: the pH of the solution is between 5.0 and 7.5. Purity (1) Clarity of solution⎯Use an outer glass cylinder, about 25 cm in height, 25 mm in internal diameter and 2 mm in thickness, with a high-quality glass plate, 2 mm in thickness at the bottom and inner glass cylinder, about 30 cm in height, 15 mm in internal diameter and 2 mm in thickness, with high-quality glass plate, 2 mm in thickness at the bottom. In the outer cylinder place a solution prepared by adding 1.0 g of Hydroxypropylcellulose to 100 mL of water, heat while stirring on a water-bath at 70 o C and then cool to room temperature. Place this cylinder in a sheet of white paper on which 15 parallel, black, 1-mm lines in width are drawn at 1-mm intervals. Place the inner cylinder and move it up and down while viewing downward through the bottom of the inner cylinder and measure the minimum height of the solution between the bottom of the outer cylinder and the lower end of the inner cylinder at the time when the lines on the paper cannot be differentiated: the average value obtained from three repeated procedures is greater than that obtained form the following control solution treated in the same manner. Control solution⎯5.50 mL of 0.005 mol/L sulfuric acid VS, add 1 mL of dilute hydrochloric acid, 5 mL of ethanol and water to make 50 mL. To this solution, add 2 mL of barium chloride TS, mix, allow to stand for 10 minutes and shake well before use. KP VIII 1177 (2) Chloride⎯Add 1.0 g of Hydroxypropylcellulose to 30 mL of water, heat on a water-bath with stirring for 30 minutes and filter while being hot. Wash the residue with three 15 mL volumes of hot water, combine the washings with the filtrate and add water to make 100 mL after cooling. To 10 mL of the test solution, add 6 mL of dilute nitric acid and water to make 50 mL and perform the test using this solution as the test solution. Prepare the contrrol solution with 0.40 mL of 0.01 mol/L hydrochloric acid VS (not more than 0.142%). (3) Sulfate⎯To 20 mL of the test solution obtained in (2), add 1 mL of dilute hydrochloric acid and water to make 50 mL and perform the test using this solution as the test solution. Prepare the control solution with 0.40 mL of 0.05 mol/L sulfuric acid VS (not more than 0.048%). (4) Heavy metals⎯Proceed with 1.0 g of Hydroxypropylcellulose according to Method 2 and perform the test. Prepare the control solution with 2.0 mL of standard lead solution (not more than 20 ppm). (5) Arsenic⎯Prepare the test solution with 1.0 g of Hydroxypropylcellulose according to Method 3 and perform the test (not more than 2 ppm). Loss on Drying Not more than 5.0% (1 g, 105 o C , 4 hours). Residue on Ignition Not more than 0.5% (1 g). (1) Apparatus⎯Reaction flask: A 5-mL Assay screw-cap pressure-tight glass bottle, having an inverted conical bottom inside, 20 mm in outside diameter, 50 mm in height up to the neck and 2 mL in capacity up to a height of about 30 mm, equipped with a pressure-tight septum of heat-resisting resin and also with an inside stopper or sealer of fluoroplastic. Heater: A square aluminum block, 60 mm to 80 mm in thickness, having holes, 20.6 mm in diameter and 32 mm in depth, capable of maintaining the inside temperature within ± 1 o C . (2) Procedure⎯Weigh accurately about 65 mg of Hydroxypropylcellulose, previously dried, transfer to the reaction flask, add 65 mg of adipic acid, 2.0 mL of the internal standard solution and 2.0 mL of hydroiodic acid, stopper the flask tightly and weigh accurately. Shake the flask for 30 seconds, heat at 150 o C on the heater for 30 minutes with repeated shaking at 5 minute intervals and continue heating for an additional 30 minutes. Allow the flask to cool and again weigh acurately. If the mass loss is less than 10 mg, use the upper layer of the mixture as the test solution. Separately, take 65 mg of adipic acid, 2.0 mL of hydroiodic acid in another reaction flask, stopper tightly and weigh accurately. Add 50 μL of iospropyl iodide RS and again weigh accurately. Shake the reaction flask for 30 seconds and use the upper layer of the content as the standard solution. Perform the test as directd under the Gas Chromatography with 1 μL each of the test solution and the standard solution according to the following operating conditions and, calculate the ratios, QT and QS , of the peak area of isopropyl iodide to that of the internal standard for the test solution and the standard solution, respectively. Amount (%) of hydroxypropoxyl group (C 3 H 7 O 2 ) = WS QT × × 44.17 QS amount (mg) of the sample WS : Amount(mg) of isopropyl iodide in the standard solution. Internal standard solution⎯A solution of n-octane in o-xylene (4 in 100). Operating conditions Detector: A thermal conductivity detector or hydrogen flame-ionization detector. Column: A column, about 3 mm in inside diameter and about 3 m in length, packed with siliceous earth for gas chromatography (180 μm to 250 μm in particle diameter), coated with methyl silicone polymer for gas chromatography at the ratio of 20%. Column temperature: A constant temperature of about 100 °C. Carrier gas: Helium (for thermal-conductivity detector), helium or nitrogen (for hydrogen flameionization detector). Flow rate: Adjust the flow rate so that the retention time of the internal standard is about 10 minutes. Selection of column: When the procedure is run with 1 μL of the standard solution according to the above operating conditions, isopropyl iodide and the internal standard are eluted in this order and separated completely from each other. Packaging and Storage Preserve in well-closed containers. Low Substituted Hydroxypropylcellulose Low Substituted Hydorxypropylcellulose is a low substituted hydroxypropylether of cellulose. Low Substituted Hydroxypropylcellulose, when dried, contains not less than 5.0% and no more than 16.0% of hydroxypropoxyl group (-OC3H6OH: 75.09). Description Low Substituted Hydroxypropylcellulose is white to yellowish white powder or granules, is tasteless, odorless or has slight, characteristic odor. Low Substituted Hydroxypropylcellulose is practically insoluble in ethanol or in ether. Low Substituted Hydroxypropylcellulose dissolves in a solution of sodium hydroxide (1 in 10) and becomes 1178 Monographs, Part II viscous solution. Low Substituted Hydroxypropylcellulose swells in water, in sodium carbonate TS or in 2 mol/L hydrochloric acid TS. Identification (1) Take 20 mg of Low Substituted Hydroxypropylcellulose, add 2 mL of water, shake and produce a turbid solution. Add 1 mL of anthrone TS gently: a blue to blue-green color develops at the zone of contact. (2) Take 0.1 g of Low Substituted Hydroxypropylcellulose, add 10 mL of water, stir and produce a turbid solution. Add 1 g of sodium hydroxide, shake until it becomes homogeneous and use this solution as the test solution. To 0.1 mL of the test solution, add 9 mL of diluted sulfuric acid (9 in 10), shake well, heat in a waterbath for exactly 3 minutes, immediately cool in an icebath, add carefully 0.6 mL of ninhydrin TS, shake well and allow to stand at 25 o C : a red color develops at first and it changes to purple within 100 minutes. (3) Take 5 mL of the test solution obtained in (2), add 10 mL of a mixture of acetone and methanol (4 : 1) and shake: a white, flocculent precipitate is produced. pH Take 1.0 g of Low Substituted Hydroxypropylcellulose, add 100 mL of freshly boiled and cooled water and shake: the pH of the solution is between 5.0 and 7.5. Purity (1) Chloride⎯Take 0.5 g of Low Substituted Hydroxypropylcellulose, add 30 mL of hot water, stir well, heat on a water-bath for 10 minutes and filter the supernatant liquid by decantation while being hot. Wash the residue thoroughly with 50 mL of hot water, combine the washings with the filtrate and add water to make 100 mL after cooling. To 5 mL of this solution, add 6 mL of dilute nitric acid and water to make 50 mL and perform the test using this solution as the test solution. Prepare the control solution with 0.25 mL of 0.01 mol/L hydrochloric acid (not more than 0.335%). (2) Heavy metals⎯Prceed with 2.0 g of Low Substituted Hydroxypropylcellulose according to Method 2 and perform the test. Prepare the control solution with 2.0 mL of standard lead solution (not more than 10 ppm). (3) Arsenic⎯Prepare the test solution with 1.0 g of Low Substituted Hydroxypropylcellulose, according to Method 3 and perform the test (not more than 2 ppm). Loss on Drying Not more than 6.0% (1 g, 105 o C , 1 hour). Residue on Ignition Not more than 1.0% (1 g). Assay Proceed as directed in the Assay under Hydroxypropylcellulose, but add 15 μL of iospropyl iodide RS instead of 50 μL of iospropyl iodide RS, and perform the test with 2 μL each of the test solution and the standard solution instead of 1 μL each and use a so- lution of n-octane in o-xylene (1 in 50) as the internal standard solution. Amount (%) of hydroxypropoxyl group (C 3 H 7 O 2 ) = WS QT × × 44.17 QS amount (mg) of the sample Packaging and Storage Preserve in tight containers. Hypromellose Hydroxypropylmethylcellulose Hypromellose is a methyl and hydroxypropyl mixed ether of cellulose. There are four substitution types of Hypromellose, which are 1828, 2208, 2906, and 2910. Hypromellose contains methoxy group (-OCH3: 31.03) and hydroxypropoxy group (-OCH3H6OH: 75.09) as shown in the following table, calculated on the dried basis. The viscosity of Hypromellose is shown in millipascal second (mPa⋅s) on the label, together with its substitution type. Substitution Type 1828 2208 2906 2910 Methoxy Group (%) Hydroxypropoxy Group (%) Min. Max. Min. Max. 16.5 19.0 27.0 28.0 20.0 24.0 30.0 30.0 23.0 4.0 4.0 7.0 32.0 12.0 7.5 12.0 Description Hypromellose is a white to yellowish white, powder or granule. Hypromellose is practically insoluble in dehydrated ethanol. Hypromellose swells with water and becomes a clear or slightly turbid, viscous solution. Identification (1) Disperse evely 1.0 g of Hypromellose over the surface of 100 mL of water in a beaker, while gently tapping the top of the beaker, if necessary, and allown the beaker to stand: it aggregates on the surface of water. (2) Add 1.0 g of Hypromellose to 100 mL of hot water and stir: it becomes a suspension. Cool the suspension to 10 o C , and stir: the resulting liquid is a clear or a slightly cloudy, viscous fluid. (3) Take 0.1 mL of the final solution obtained in (2), add 9 mL of diluted sulfuric acid (9 in 10), shake, heat in a water-bath for exactly 3 minutes, immediately cool in an ice-bath, add carefully 0.6 mL of ninhydrin TS, shake and allow to stand at 25 o C : a light red color develops at first and it changes to purple within 100 minutes. and heat until the volume of the solution becomes 2 to 3 mL. dilute the solution with 2 to 3 mL of water. 2 mL of acetate buffer solution. Repeat this procesure until the solution no longer changes to black. Centrifuge the test solution if necessary to expel any entrapped air bubbles. boil gently until dense white fumes are evolved. After cooling. and heat until the solution changes to black. add hot water to make 500. Repeat this operation 2 times more.KP VIII 1179 (4) Pour and spread out 2 to 3 mL of the viscous fluid obtained in (2) on to a glass plate and allow the water to evaporate : a transparent film results. 105 o C . equivalent to 10. is not less than 50 o C . Repeat this procedure until to use total 18 mL of the mixture of nitric acid and sulfuric acid (5 : 4). Operating conditions Apparatus: Brookfield type viscometer LV model Rotor no.5 and water to make 50 mL. add 18 mL of the mixture of nitric acid and sulfuric acid (5 : 4) and an amount of nitric acid equal to that used for the preparation of the test solution. according to the following operating conditions: not less than 75% and not more than 140% of the labeled viscosity. After cooling. Rotor no. stopper the bottle.0 mL of standard lead solution in a 100mL Kjeldahl flask. add water to make 25 mL. then proceed in the same manner for the preparation of the test solution.5% (1. Separately. Method 2: Apply to Hypromellose having a labeled viscosity of not less than 600 mPa·s.000 g. if necessary. stir by mechanical means at 350.0 to 4. Purity Heavy metals⎯Put 1. and use this solution as the test solution. put 2. and prepare the test solution in the same manner as directed in Method 1. Perform the test with the test solution at at 20 ± 1 o C as directed in Method 2 under the Viscosity Determination.0 and 8. separately. Add cooled water. Viscosity Method 1: Apply to Hypromellose having a labeled viscosity of less than 600 mPa·s. and use this solution as the test solution. using a single cylinder-type rotational viscometer. respectively. to make 200. about 50 mm in height. and conversion factor: use as shown in the following table. and stop the rotation for 2 minutes. transfer to a Nessler tube. After cooling. Labeled viscosity (mPa·s) Not less than 600 and less than 1400 Not less than 1400 and less than 3500 Not less than 3500 and less than 9500 Not less than 9500 and less than 99500 Not less than 99500 Operation of apparatus: Read value after 2 minutes of rotation. In the case where hydrogen peroxide (30) is added for the preparation of the test solution. Put exactly Hypromellose. Put exactly Hypromellose. add 1 mL of hydrogen peroxide(30).0% (1 g. wide-mouth bottle. rotation frequency. add the same amount of hydrogen peroxide (3). 1 hours). calculated on the dried basis.00 g. pH 3. add a sufficient amount of a mixture of nitric acid and sulfuric acid (5:4) to wet the sample.to 450-revolutions per minute for 10 to 20 minutes to get a homogeneous dispersion.. 4 60 100 4 6 1000 4 3 2000 Assay (1) Apparatus⎯Reaction bottle : A 5-mL screw-cap pressure-tight glass vial. and add water to make 40 mL.0 g). equipped with a pressure-tight septum of . when a white turbidity of the solution starts to increase. Rotation frequency /min Conversion factor 3 60 20 Loss on Drying Not more than 5.0 g. wide-mouth bottle. equivalent to 4. in a tared. and heat until the solution changes to black.0 with ammonia solution (28). then heat until the volume of the solution becomes 2 to 3 mL.0 g. If necessary. oserve vertically both tubes on a white background: the color obtained with the test solution is not more intense than that with the control solution (not more than 20 ppm). and heat until dense white fumes are evolved. depending on the labeled viscosity. add 5 mL of water. pH Allow the test sample obtained in the Viscosity to stand at 20 ± 2 o C for 5 minutes: the pH of the solution thus obtained is between 5. After allowing to stand for 5 minutes. Perform the test with the test solution at at 20 ± 1 o C as directed in Method 1 under the Viscosity Determination: not less than 80% and not more than 120% of the labeled viscosity. take off the sample attached on the walls of the bottle. in a tared. add 2 mL of nitric acid. and dissolve by continuing the stirring in a water bath not exceeding 10 o C for 20 to 40 minutes while stirring. 3 12 100 Residue on Ignition Not more than 1. and heat strongly until dense white fumes are evolved. (5) Take exactly 50 mL of water.0. Adjust the test solution and the control solution to pH 3. After cooling. if the solution reveals yellow color by addition of 5 mL of water. calculated on the dried basis. To this solutions add 1. and heat gently.0 g of Hypromellose a 100-mL Kjeldahl flask. After cooling. add 10 mL of water. having the neck 20 mm in outside diameter and 13 mm in inside diameter.0 g. and average three observed values. put them in the dispersed solution. and use so obtained solution as the control solution. add exactly 50 mL of the final solution obtained in (2) and warm to rise the temperature at a rate of 2 to 5 o C per minute while stirring: the temperature of congealing.2 mL of thisacetamide-alkaline glycerin TS. add hot water to make 200. about 20 mm in outside diameter. Add 45 μL of methyl iodide RS and 15 to 22 μL of isopropyl iodide RS through the septum using micro-syringe with weighing accurately each time. and continue heating for an additional 30 minutes. 3 to 4 mm in inside diameter and 1.0 27.12). Hypromellulose Phthalate contains methoxy group (OCH3: 31. in dehydrated ethanol. Heater: A square-shaped aluminum block. add 60 to 100 mg of adipic acid. Stir or shake for 60 minutes while heating so that the temperature of the bottle content is 130 ± 2 o C . transfer to the reaction bottle. methyl iodide. or helium or nitrogen for hydrogen flame ionization detector.03). and capable of stirring the content of the reaction bottle by means of magnetic stirrer or of reciprocal shaker about 100 times per minute.8 to 3 m in length. Shake thoroughly the reaction bottle and use the upper layer of the content as the standard solution. (2) Procedure⎯Weigh accurately about 65 mg of Hypromellulose.1180 Monographs. and each type contains indicated amount of carboxybenzoyl group in the following table. Column: A glass column. from the standard solution to that of the internal standard from the standard solution. Internal standard solution⎯A solution of n-octane in o-xylene (1 in 25). which can be fixed tightly to vial with aluminum cap. in acenitrile. isopropyl iodide and the internal standard are eluted in this order. Operating conditions Detector: A thermal conductivity detector or hydrogen flame-ionization detector. calculated on the dried basis.09) and carboxybenzoyl group (-COC6H4COOH: 149. Column temperature: A constant temperature of about 100 °C.17 QSb W WSa : Amount (mg) of methyl iodide RS WSb : Amount (mg) of isopropyl iodide RS W : Amount (mg) of the sample. Description Hypromellulose Phthalate is white powder or granule. In the case when the stirrer or shaker is not available. stopper the bottle tightly. Carrier gas: Helium for thermal conductivity detector. put 60 to 100 mg of adipic acid. adopted to the reaction bottles.. having holes 20 mm in diameter and 32 mm in depth. Hypromellulose Phthalate is practically insoluble in water. with complete separation of these peaks. 2.0 220824 21. Carboxybenzoyl group (%) Substitution type Minimum Maximum 200731 27.0 The substitution type of Hypromellulose Phthalate is shown together with its kinetic viscosity in square mm per second (mm2/s). of the peak area of methyl iodide from the test solution to that of the internal standard and QSa and QSb .0 mL of hydroiodic acid in a reaction bottle. 2. peakd with siliceous earth for gas chromatography (125 μm to 150 μm in diameter). QTa and QTb . If the mass loss is less than 0. coated with methyl silicone polymer at the ratio of 10 to 20%.0 mL of hydroiodic acid. or equivalent. heat for 30 minutes with repeated shaking at 5-minute intervals by hand. respectively. 200731 and 220824. Part II butyl-rubber with surface processed with fluoroplastics.0 35. Allow the flask to cool and again weigh accurately. of the peak area of methyl iodide and isopropyl iodide. and in hexane.50% or there is no evidence of a leak. Perform the test with 1 to 2 μL each of the test solution and the standard solution as directed under the Gas Chromatography according to the following operating conditions and calculate the ratios. Hypromellulose Phthalate becomes a viscous liquid when a mixture of methanol and dichloromethane (1 : 1) or a mixture of dehydrated ethanol and acetone (1 : . on the label. use the upper layer of the content as the test solution. Separately. immediately and weigh accurately. hydroxypropoxy group (-OC3H6OH: 75.0 mL of the internal standard solution and 2. Packaging and Storage Preserve in well-closed containers. Flow rate: Adjust the flow rate so that the retention time of the internal standard is about 10 minutes. is odorless and tasteless. calculated on the anhydrous basis. System suitability System performance: When the procedure is run with 1 to 2 μL of the standard solution under the above operating conditions.0 mL of the internal standard solution and 2. Content (%) of methoxyl group (CH 3 O) Q W = Ta × Sa × 21.864 QSa W Content (%) of hydroxypropoxyl group (C 3 H 7 O 2 ) Q W = Tb × Sb × 44. There are two substitution types. stopper immediately and weigh accurately. Hypromellose Phthalate Hydroxypropylmethylcellulose Phthalate Hypromellulose Phthalate is a monophthalic acid ester of hydpomellulose. sonicate for dissolving partially.2% (1 g) Assay Weigh accurately about 1. packed with octadecylsilylated silica gel (3 μm to l0 μm in particle diameter).1 o C according to Method 1 under the Viscosity Determination: not less than 80% and not more than 120% of the labeled unit. Mobile phase: A mixture of 0. until the gel-like precipitate formed becomes granular. Determine the viscosity at 20 ± 0. calculated on the anhydrous basis. add acetonitrile to make exactly 250 mL and use this solution as the standard solution.1 mol/L cyanoacetic acid and acetonitrile (17 : 3). as directed in the potassium bromide disk method under Infrared Spectrophotometry: both spectra exhibit similar intensities of absorption at the same wavenumbers.13) is not more than 1. weigh accurately about 12. in 90 g of a mixture of methanol and dichloromethane in equal mass ratio by mixing and shaking. Purity (1) Chloride⎯Dissolve 1.1 mol/L of sodium hydroxide VS (indicator: 2 drops of phenolphthalein TS). AT and AS .0 mL of standard lead solution (not more than 10 ppm) (3) Phthalic acid⎯Weigh accurately about 2. Separately. direct titration.07%).1 × V 2 × 149. Operating conditions Detector: An ultraviolet absorption photometer (wavelength: 235 nm). Perform the test with 50 mL of the filtrate. add 1 drop of phenolphthalein TS and add dilute nitric acid drop-wise.1 × P − W 166. add 10 mL of water. and water to make 50 mL (not more than 0. and filter. with stirring. with vigorous stirring. centrifuge and separate the supernatant liquid and wash the residue with three 20 mL portions of water by centrifuging each time. Hypromellulose Phthalate dissolves in sodium hydroxide TS. W : Amount(mg) of the sample. until the red color is discharged. W : Amount (g) of the sample.0%. Residue on Ignition Not more than 0. Column temperature: A constant temperature of about 20 o C .01× 149.2 mol/L sodium hydroxide. combine the supernatant liquid and the washings. ethanol and water (2 : 2 : 1). then add 25 mL of water. Viscosity Dissolve 10 g of Hypromellulose Phthalate previously dried at 105 o C for 1 hour. (2) Heavy metals⎯Proceed with 2. Packaging and Storage Preserve in tight containers. Flow rate: 2. add acetonitrile to make exactly 100 mL and use this solution as the test solution. dissolve in 50 mL of a mixture of acetone. using a mixture of dehydrated ethanol and dichloromethane (3 : 2) instead of methanol for Karl Fischer method).0 g of Hypromellulose Phthalate.2 mol/L sodium hydroxide TS and 7 mL of dilute nitric acid. respectively: the content of phthalic acid (C8H6O4: 166. Prepare the control solution as follows: take 0. calculrated on anhydrous basis.KP VIII 1181 1) is added.0% (1g.0g of Hypromellulose Phthalate. and heat on a water-bath. titrate with 0. Column: A stainless steel column. add about 50 mL of acetonitrile.0 g of Hypromellulose Phthalate in 40 mL of 0. the relative deviation of the peak area of phthalic acid is not more than 1. Content (%) of phthalic acid (C 8 H 6 O 4 ) = C AT × × 10 W AS C : Concentration(μg/mL) of phthalic acid in the standard solution. . Prepare the control solution with 2. System suitabilty System reproducibility: When the test is repeated 6 times with 10 μL of the standard solution under the above operating conditions. sonicate again to dissolve further. Perform a blank determination and make necessary correction.0%. add water to make 200 mL. Add an additional 20 mL of dilute nitric acid with stirring.0 g of Hypromellulose Phthalate according to Method 2 and perform the test.0 mL/minute. Amount (%) of carboxybenzoyl group (C8 H 5 O 3 ) = 0.1 P : Content (%) of phthalic acid under Purity (3) Phthalic acid. add 10 mL of 0. V : Volume (mL) of 0.01 mol/L hydrochloric acid.1 mol/L sodium hydroxide used in titration.5 mg of phthalic acid.50 mL of 0. of phthalic acid for the test solution and the standard solution. after cooling. Identification Determine the infrared absorption spectra of Hypromellulose Phthalate and Hypromellulose Phthalate RS. Water Not more than 5. Perform the test with 10 μL each of the test solution and the standard solution as directed under the Liquid Chromatography according to the following operating conditions and determine the peak areas. 4 mm in inside diameter and about 25 cm in length. After cooling. add about 125 mL of acetonitrile. dissolve with shaking.5. (2) Acid-soluble substances⎯Add 20 mL of dilute hydrochloric acid to 1. Cool.036%). (2) and (4) for aluminum salt. add 100 mL of water. Add drop-wise strong ammonia water to this solution until a slight precipitate occurs. Identification (1) Heat 1 g of Kaolin with 10 mL of water and 5 mL of sulfuric acid in a porcelain dish and evaporate the mixture nearly to dryness. (3) Carbonate⎯Stir 1.45 g of hydroxylamine hydrochloride and heat. Purity (1) Chloride—Perform the test with 1. Combine the filtrate and the washings and add water to make 150 mL. add 0.0 g of Lactic Acid. if necessary and wash with 10 mL of water. Lactic Acid contains not less than 85. stir and decant to leave sand. centrifuge and separate the supernatant liquid. (2) Sulfate—Perform the test with 2. Prepare the control solu- tion with 2.010%).0% and not more than 92. Wash the precipitate twice with 10 mL of water. Kaolin is practically insoluble in water. 20 Specific gravity— d 20 : About 1.08 Lactic Acid is a mixture of lactic acid and lactic anhydride.0 g of Lactic Acid.15 g of hydroxylamine hydrochloride. Kaolin darkens and becomes plastic.15 g of sodium acetate. (3) Heavy metals—Take 2.0 g of Lactic Acid.0% of lactic acid (C3H6O3). Repeat this procedure several times with 100 mL volumes of water: no sandy residue remains.005 mol/L sulfuric acid VS (not more than 0. in dehydrated ethanol or in ether. Description Lactic Acid is a clear. add 0. viscous liquid. Part II Kaolin Kaolin is a native. 600 5 hours).40 mL of 0. Prepare the control solution as follows: To 2. unpleasant odor. (7) Foreign matter⎯Place 5 g of Kaolin in a breaker.0 and 7. Prepare the control solution with 1. conetrifuge each time and combine the supernatant liquid and the washings. Lactic Acid is hygroscopic. add 10 mL of water and 1 drop of phenolphthalein TS. boil for 2 to 3 minutes and filter: the color of the residue is gray.5 g of tartaric acid.5 mL of standard lead solution add 0.01 mol/L hydrochloric acid VS (not more than 0. Perform the test using 50 mL of this solution as the test solution. Evaporate 10 mL of the filtrate to dryness and ignite between 450 o C and 550 o C to a constant weight: the ignited residue is not more than 10 mg. Loss on Ignition Not more than 15. odorless or has faint. add 20 mL of water. Packaging and Storage Preserve in well-closed containers. Add 0.5 g of Kaolin gently with 50 mL of water and 5 mL of hydrochloric acid for 20 minutes with frequent agitation. hydrous aluminum silicate. cool. agitate thoroughly and filter: the pH of the filtrate is between 4. (6) Arsenic⎯Add 5 mL of water and 1 mL of sulfuric acid to 1. prepare the test solution with this solution according to Method 2 and perform the test according to Method B. responds to the Qualitative Tests (1).0% (1 g. (2) The filtrate obtained in (1).0 g of Kaolin and agitate thoroughly: the resultant mass has no remarkable fluidity. Lactic Acid OH H3C C COOH H 2-Hydroxypropionic acid and enantiomer C3H6O3: 90.0 g of Kaolin. Identification A solution of Lactic Acid in water (1 in 50) changes blue litmus paper to red and responds to the Qualitative Tests for lactate.0 mL of 0. colorless or light yellow. filter. Kaolin is insoluble in dilute hydrochloric acid or in sodium hydroxide TS. o C.0 g of Kaolin with 5 mL of water and add 10 mL of diluted sulfuric acid (1 in 2): no foam is produced. agitate for 15 minutes and filter. and add ammonia TS dropwise until a pale red color ap- . Add water to make 5 mL after cooling and perform the test (not more than 2 ppm). Description Kaolin is white or nearly white.0 g of Kaolin and heat on a water-bath until white fumes begin to evolve.1182 Monographs. then add dilute hydrochloric acid drop-wise while agitating strongly to complete solution.0 mL of standard iron solution (not more than 500 ppm). Purity (1) Acidity or alkalinity⎯Add 25 mL of water to 1. After cooling. fragmentary mass or powder and has slightly clay-like odor. 2 mL of acetic acid and add water to make 50 mL (not more than 50 ppm).5 mL of water to 5. ethanol or ether. Lactic Acid is miscible with water. Plasticity Add 7. When moistended with water. Cool.45 g of sodium acetate and 6 mL of dilute acetic acid. 0. Prepare the control solution with 0.20. (4) Heavy metals⎯Boil 1.0 g of Kaolin. (5) Iron⎯Add 10 mL of dilute hydrochloric acid to 40 mg of Kaolin and heat for 10 minutes with shaking in a water-bath. add 1.10%(1 g). and dilute with water to make 50 mL (not more than 10 ppm). (5) Sugars—Take 1. Weigh accurately about 10 g of Lactose Hydrate.9 o . Control solution—Pipet exactly 1. To the solution. After standing for 30 minutes. Boil the mixture for 2 minutes: no change occurs.5 mol/L sulfuric acid VS immediately (indicator: 2 drops of phenolphthalein TS). Specific Optical Rotation [α ]20 D : Between +54. powder or granulated powder. Description Lactose Hydrate is a white crystal. 80 o C . Prepare the control solution with 2. Loss on Drying Not more than 0. Add 2 mL of dilute acetic acid and water to make 50 mL. Assay Weigh accurately about 3 g of Lactic Acid. add accurately measured 40 mL of 1 mol/L sodium hydroxide VS. and perform the test using this solution as the test solution.0 g of Lactic Acid. (10) Readily carbonizable substances— Superimpose slowly 5 mL of Lactic Acid. add 1. any make any necessary correction. Lactose is odorless.8. add dropwisely a solution of sodium hydroxide (1 in 10) with shaking until a pale red color develops. .0 mL of this solution to a Nessler tube. invert a watch glass over the flask. Residue on Ignition Not more than 0. (4) Iron—Prepare the test solution with 4. and the total count of fungi and yeast is not more than 50 per g. dissolve in 80 mL of water warmed to 50 o C . Prepare the control solution with 2. and 0. as directed in the potassium bromide disk method under the Infrared Spectrophotometry and compare the spectrum with the reference spectrum or the spectrum of: both spectra exhibit similar intensities of absorption at the same wavenumbers.0 mL of standard lead solution and 2 mL of dilute acetic acid. add 1 drop of dilute acetic acid.0 mL of standard cyanide solution. Each mL of 1 mol/L sodium hydroxide VS = 90. and heat in a water-bath for 10 minutes. and allow to stand at 15 o C for 15 minutes: no dark color develops at the zone of contact. followed by 40 mL of calcium hydroxide TS.08 mg of C3H6O3 Packaging and Storage Preserve in tight containers.0 mL of water. mix gently. and allow to stand for 5 minutes. Titrate the excess sodium hydroxide with 0. (7) Glycerin or mannitol—Shake 10 mL of Lactic Acid with 12 mL of ether: no turbidity is produced.31 Lactose Hydrate is a disaccharide obtained from milk. allow to cool and add 0. upon 5 mL of sulfuric acid for Readily carbonizable substances.25 mL of chloramine TS. and perform the test according to Method A. add 10 mL of water and 1 drop of phenolphthalein TS.0% for the granulated powder). calculated on the anhydrous basis.2 mL of ammonia TS. consist of one unit of glucose and one unit of galactose. add 10 mL of water.0 g of Lactic Acid to a Nessler tube. Lactose Hydrate is freely soluble in water and practically insoluble in ethanol. and neutralize with sodium hydroxide TS. Cool.KP VIII 1183 pears.0 mL of standard iron solution (not more than 5 ppm).5% (1 g. previously kept at 15 o C . oxalic acid .4 and +55. previously dried. and add water to make exactly 20 mL.0 g of Lactic Acid according to Method 1. (6) Citric acid. Salmonella and Escherichia coli should not be observed. The label states that the granulated powder is Lactose Hydrate.0 g of Lactic Acid. transfer in a Erlenmeyer flask. and heat in a water-bath for 10 minutes. (9) Cyanide—Transfer 1. Microbial Limit The total viable aerobic microbial count is not more than 100 per g of Lactose Hydrate.10% (1 g). Residue on Ignition Not more than 0. pH 6.5 mL of a solution of sodium hydroxide (1 in 10) and water to make 20 mL. Perform a blank determination. add 10 mL of phosphate buffer solution. Identification Determine the infrared spectra of Lactose Hydrate and Lactose Hydrate RS. Transfer 1. add dropwisely dilute acetic acid until a red color of the solution disappears. and proceed as directed in the test solution. add 15 mL of pyridine-pyrazolone TS and water to make 50 mL. phosphoric acid and tartaric acid—Take 1. 2 hours) (not more than 1. Lactose Hydrate CH2OH HO H OH OH H OH O H OH H H H O H HO H OH H2O H O CH2OH C12H22O11·H2O: 360. and allow to stand at 25 o C for 30 minutes: the solution is not more intense than the following control solution. add 10 mL of water and 1 drop of phenolphthalein TS. (8) Volatile fatty acids—Warm Lactic Acid: any acetic acid-like or butyric acid-like odor is not produced. add water to make exactly 100 mL and determine the optical rotation of this solution in a 100 mm cell. stopper immediately. Purity Proceed as directed in the Purity under Anhydrous Lactose. Boil the mixture with 10 mL of Fehling's TS for 5 minutes: no red precipitate is produced. previously kept at 15 o C . 40 mL of 0. a ratio of the retenion time of α-lactose to that of β-lactose is about 0.5% (1 g. Carrier gas: Helium. allow to cool and add 0. and shake well. Column: A column. Content (%) of β-lactose = Ab × 100 Aa + Ab Operating conditions— Detector: A hydrogen flame-ionization detector. add 0. volumetric titration.0 g of Anhydrous Lactose in 10 mL of hot water: the solution is clear and colorless or nearly colorless.25 at between 210 nm and 220 nm and not more than 0. cool.0 and 5. about 4 mm in inside diameter and about 0. Add 1. (3) Heavy metals⎯Proceed with 4.3 mL of phenolphthalein TS: the solution is colorless. of α-lactose and β-lactose. Part II Water Between 4.07 at between 270 nm and 300 nm.8 mL of a mixture of pyridine and trimethylsilylimidazole (72:28). Test injection port temperature: About 275 o C . Identification Determine the infrared spectra of Anhydrous Lactose and Anhydrous Lactose RS. After standing for 30 minutes and water to make exactly 100 mL and determine the optical rotation of this solution in a 100 mm cell. Weigh accurately about 10 g of Anhydrous Lactose.0.30 Anhydrous Lactose is β-lactose or mixture of β-lactose and α-lactose. Specific Optical Rotation [α ]20 D : Between +54. respectively and calculate the content (%) of β-lactose in Anhydrous Lactose by the following equation.5 and 5. add 0. Flow rate: A constant flow rate of about 40 mL per minute. Description Anhydrous Lactose is a white crystal or powder. (4) Proteins and light absorbing substances⎯Dissolve 1. using water as the blank: not more than 0. . Perform the test with 2 μL of the test solution as directed under the Gas Chromatography according to the following operating conditions and determine peak areas Aa and Ab .7 with the resolution between their peaks being not less than 3. Anhydrous Lactose is freely soluble in water and practically insoluble in ethanol.1184 Monographs. Column temperature: A constant temperature of about 215 o C . System suitability⎯ System performance: Prepare a solution with 1 mg of the mixture of α-lactose and β-lactose (1 : 1) in the same manner as for preparing the test solution.9 m in length.1 mol/L sodium hydroxide VS: a red color develops.5% for the granulated powder). Microbial Limits The total aerobic microbial count is not more than 100 per g of Anhydrous Lactose. as directed in the potassium bromide disk method under the Infrared Spectrophotometry: both spectra exhibit similar intensities of absotption at the same wave numbers. The relative quantities of α-lactose and β-lactose in Anhydrous Lactose are indicated as the isomer ratio. direct titration) Use a mixture of methanol for Karl Fischer method and formamide for Karl Fischer method (2 : 1) instead of methanol for Karl Fischer method. Anhydrous Lactose CH2OH HO H OH OH H OH O H OH H H H H O O H HO H OH CH2OH C12H22O11: 342. Purity (1) Clarity and color of solution⎯Dissolve 1.04. dissolve in 80 mL of water warmed to 50 o C . Packaging and Storage Preserve in well-closed containers.0 g of Anhydrous Lactose according to Method 2 and perform the test. mix. add 0. Determine the absorbance at 400 nm of this solution as directed under the Ultraviolet-visible Spectrophotometry. packed with siliceous earth for gas chromatography coated at the ratio of 3% with 25% phenyl-25% cyanopropyl-methylsilicone polymer for gas chromatography. When the procedure is run with 2 μL of this solution under the above operating conditions.45 mL of dimethylsulfoxide. Prepare the control solution with 2 mL of standard lead solution (not more than 5 ppm).9 o .0 g of Anhydrous Lactose in water to make 100 mL and use this solution as the test solution. stopper.4 and +55. Isomer Ratio Place 1 mg of Anhydrous Lactose in an about 5 mL screw capped reaction vial for gas chromatography. as directed under the Ultraviolet-visible Spectrophotometry. (between 4. Determine the absorbances. using water as the blank: not more than 0. the total fungus (fungi and yeast) count is not more than 50 per g.2 mL of ammonia TS. (2) Acid or alkali⎯Dissolve 6 g of Anhydrous Lactose in 25 mL of freshly boiled and cooled water by heating. previously dried. allow to stand for 20 minutes and use this solution as the test solution. To this solution. and Salmonella species and Escherichia coli are not observed. (3) and (4) under Purified Lanolin. Residue on Evaporation Weigh accurately about 12. Chloride. 80 hours). Purity (1) Acid or alkali. silica gel) for 24 hours and weigh. Purity (1) Acidity or alkality⎯Take 5 g of Purified . 2 Water Not more than 1.5% (1 g. then weigh accurately about 0.b) × 1.0% and not more than 75. characteristic but not rancid odor. Wash the separatory funnel and the filter paper twice with 20 mL volumes of ether. Iodine Value Between 18 and 36.1 mol/L sodium thiosulfate VS (indicator: 1 mL of starch TS). Heat a suitable amount of Hydrous Lanolin on a water-bath to remove its almost moisture. transfer the separated aqueous layer to another separatory funnel. Proceed with 1 mL of the cyclohexane solution in the Identification under Purified Lanolin. Add 20 mL of a solution of potassium iodide (1 in 10) and 100 mL of water.1% (1 g). shake and combine the ether layer and ether in the first separatory funnel.269 Iodine value = amount (g) of sample a: Volume (mL) of 0. Residue on Ignition Not more than 0. ointment-like substance and has a faint.5 g of Hydrous Lanolin.0% of Purified Lanolin (as determined by the test for Residue on evaporation). Hydrous Lanolin is Purified Lanolin to which water is added. Identification Superimpose carefully 1 mL of a solution of Purified Lanolin in cyclohexane solution (1 in 50) on 2 mL of sulfuric acid: a red-brown color develops at the zone of contact and the sulfuric acid layer shows a green fluorescence. If a clear solution is not obtained. When melted by heating on a water-bath. Acid Value Not more than 1. Iodine Value Between 18 and 36. dissolve in 50 mL of ether. ointment like substance and has a slight. using a mixture of methanol for Karl Fischer Method and formamide for Karl Fischer Method (2 : 1) instead of methanol for Karl Fischer Method). well-closed containers while occasional shaking. Description Hydrous Lanolin is a yellowish white. Identification Dissolve 1 g of Hydrous Lanolin in 1 mL of cyclohexane and remove the separated water. Acid Value Not more than 1. add more cyclohexane to make clear and allow the mixture to stand for 1 hour between 20 °C and 30 °C in a light-resistant. volumetric titration. Ammonia and Water-soluble organic substances⎯Proceed as directed in Purity (1).8 g of Purified Lanolin in a glass-stoppered 500 mL flask and add 10 mL of cyclohexane to dissolve and add 25. evaporate on a water-bath until the odor of ether is no longer perceptible.0. o C. viscous.0 mL of Hanus’s TS and mix well.0% (1 g. very slightly soluble in ethanol. Perform a blank determination in the same manner and make any necessary correction. Weigh accurately about 0. it separates into a clear oily layer and a clear water layer.8 g of the treated Hydrous Lanolin in a glass-stoppered 500 mL flask and proceed as directed in the Iodine value under Purified Lanolin.KP VIII 1185 Loss on Drying Not more than 0. Packaging and Storage Preserve in well-closed containers. Melting point⎯Between 37 o C and 43 o C . combine the washings with the filtrate. It is very soluble in ether or in cyclohexane. Purified Lanolin Hydrous Lanolin Purified Lanolin is the purified product of the fat-like substance obtained from the wool of Ovis aries Linné (Bovidae).1 mol/L sodium thiosulfate VS consumed in the blank determination. (a . Hydrous Lanolin contains not less than 70. b: Volume (mL) of 0.1 mol/L sodium thiosulfate VS consumed in the titration. but miscible without separation with about twice volumes of water and retaining ointment-like viscosity. place in a separatory funnel. freely soluble in tetrahydrofuran or in toluene. (2) Petrolatum⎯Dry the residue after evaporation and proceed as directed in Purity (5) under Purified Lanolin. add 10 mL of ether. filter paper. direct titration. which is not rancid.0. Hydrous Lanolin is soluble in ether or in cyclohexane. shake and titrate the liberated iodine with 0. with the separation of water. characteristic odor. (2). Melting point⎯About 39 o C . dry in a dessicator (in vacuum. Shake the ether layer with 3 g of anhydrous sodium sulfate and filter through dry Description Purified Lanolin is a pale yellow to yellowish brown. Purified Lanolin is partially insoluble in water. Packaging and Storage Preserve in well-closed containers at not more than 30 o C . cool and examine under ultraviolet light (main wavelength: 365 nm): no fluorescent spot is observed in the same level with the spot of standard solution. add 40 mL of water. Ash Not more than 0. Spot 25 μL each of the test solution and the standard solution on a plate of silica gel for thin-layer chromatography. has a characteristic odor and a somewhat bitter and slightly irritative taste. boil for 10 minutes and cool.0 mL of 0. boil for 10 minutes and cool. Collect the separated crystals. add 5 drops of a solution of silver nitrate in ethanol (1 in 50): the turbidity of the mixture is not more intense than that of the following control solution. clear liquid or white. (2) Alkali⎯Take 2. Loss on Drying Not more than 0. stopper lightly with absorbent cotton and allow to stand at 20 o C for 18 hours. For this test use a thin-layer plate previously developed with isooctanol to the upper end. add 1 mL of sodium hydroxide TS and boil: the gas evolved does not turn moistened red litmus paper to blue. add 0. Congealing point of fatty acids⎯Between 36 o C and 42 o C .0 g of Purified Lanolin in 10 mL of a mixture of tetrahydrofuran and isooctane (1 : 1) and use this solution as the test solution. unctuous mass and has a faint. dried in air and heated at 110 o C for 60 minutes. domesticus Gray (Suidae). (3) Ammonia⎯Take 10 mL of the aqueous layer obtained in (1). Description Lauromacrogol is a colorless or pale yellow. characteristic odor and a bland taste. heat the plate at 80 o C for 5 minutes. 10 mm in thickness: the liquid is colorless to slightly yellow. To 20 mL of the filtrate. Develop the plate with isooctanol to a distance of about 10 cm and air-dry the plate. soft. Cool and add 1 drop of phenolphthalein TS to the separated water layer: the layer is colorless. Acid Value Not more than 2. Prepare the control solution with 1. Control solution⎯Take 1.0 g of Purified Lanolin. add 10 mL of water. Lard is freely soluble in ether or in petroleum ether. (5) Petrolatum⎯Dissolve 1. petrolatum-like or waxy solid. Add water to restore the previous mass and separate the aqueous layer: the aqueous layer is neutral. 2 hours). Saponificatioin Value Between 195 and 203. from which no water separates. add 6 mL of dilute nitric acid and water to make 50 mL. add 30 mL of ethanol. Observe the liquid in a layer.0 Iodine Value Between 46 and 70. Spray evenly diluted sulfuric acid (1 in 2) on the plate.1186 Monographs.0 mL of 0. Add dissolve 20 mg of vaseline in 10 mL of a mixture of tetrahydrofuran and isooctane (1 : 1) and use this solution as the standard solution. melt by warming on a water-bath and shake vigorously.5 g of Lard. Lauromacrogol Polyoxyethylene Lauryl Alcohol Ether Lauromacrogol is a polyoxyethylene ether prepared by the polymerization of ethylene oxide with lauryl alcohol. Perform the test with the test solution and the standard solution as directed under the Thin-layer Chromatography. To 20 mL of the filtrate. Part II Lanolin. add ethanol to make 20 mL and add 5 drops of a solution of silver nitrate in ethanol (1 in 50).036%). (4) Water-soluble organic substance⎯Take 5 mL of the aqueous layer obtained in (1). Lard Lard is the fat obtained from Sus scrofa Linné var. 105 o C . (2) Chloride⎯Take 2.0 g of Lard. Description Lard is a white.01 mol/L hydrochloric acid VS (not more than 0. use this solution as the test solution and perform the test.002 mol/L potassium permanganate VS and allow to stand for 5 minutes: the red color of the solution does not disappear. (3) Chloride⎯Take 1. very slightly soluble in ethanol and practically insoluble in water.5% (1 g. (4) Beef tallow⎯Dissolve 5 g of Lard in 20 mL of ether. Packaging and Storage Preserve in well-closed containers at not more than 30 o C . moisten with ethanol and examine under a microscope of 200 magnification: the crystals are in the form of rhomboidal plates grouped irregularly and do not contain prisms or needles grouped in fan-shaped clusters. Melting point⎯Between 36 o C and 42 o C (Method 2). Purity (1) Moisture and coloration⎯Melt 5 g of Lard by heating on a water-bath: it forms a clear liquid.01 mol/L hydrochloric acid VS. add 25 mL of water. Add water to restore the previous mass and filter.1% (proceed as directed in the Ash under the Crude Drugs Test) Packaging and Storage Preserve in well-closed containers at not more than 30 o C .25 mL of 0. in ether or in . Lauromacrogol is very soluble in ethanol. boil for 10 minutes under a reflux condenser and filter after cooling. add 20 mL of water and 2 mL of dilute acetic acid to the residue and heat for 2 minutes. Identification (1) Shake well 0. After washing the combined aqueous extract with 15 mL of peroxide-free ether.0 mL of heptane through the condenser and reflux for about 10 minutes. of the methyl stearate peak and the total of the areas. accurately weighed.): the test solution responds to the Qualitative Tests for magnesium salt. Add 4. and has no odor or a faint. mix and reflux for about 10 minutes to dissolve the solids. bulky powder. then shake with 5 mL of chloroform and allow to stand: the chloroform layer becomes blue. filter this solution through a filter paper. Lauromacrogol is freely soluble or dispersed as fine oily drops in water. shaking once or twice while heating. Prepare the control solution with 1. Purity (1) Acid or alkali⎯Heat 1. contains not less than 4. shake and allow the layers to separate. After cooling. transfer the contents of the flask to a separatory funnel. then incinerate at about 500 ± 25 °C. Packaging and Storage Preserve in tight containers.5 g of Lauromacrogol with 10 mL of water and 5 drops of bromine TS: the color of the solution does not disappear. After cooling. previously washed with heptane. add 2 mL of hydrochloric acid. After cooling. allow the layers to separate and transfer the aqueous layer to a flask. After cooling. (2) Chloride⎯Perform the test with 10. Extract the ether layer with two 4 mL volumes of water and combine these extracts to the main aqueous extract.0 g of Magnesium Stearate with 50 mL of peroxide-free ether. 20 mL of dilute nitric acid and 20 mL of water in a round-bottom flask and heat to dissolve completely under a reflux condenser.1 g of anhydrous sodium sulfate. Magnesium Stearate. light. Magnesium Stearate Magnesium Stearate consists chiefly of magnesium salts of stearic acid (C18-H36O2) and palmitic acid (C16H32O2). characteristic odor. shake.2 mL of 0.0% and not more than 5. (2) The retention times of the peaks corresponding to stearic acid and palmitic acid in the chromatogram of the test solution correspond to those in the chromatogram of the system suitability solution. mix and use this solution as the test solution. Perform the test with 1 μL of the test solution as directed under the Gas chromatography according to the following operating conditions and determine the area. add 2 mL of dilute acetic acid.1 mm fixed cell: it exhibits absorption at the wave numbers of about 1347 cm-1. Transfer the heptane layer through 0.0 mL of standard lead solution and water to make 50 mL (not more than 20 ppm). Prepare the control solution as follows: evaporate 2 mL of hydrochloric acid on a water-bath to dryness. Transfer 1.10%).35 g of Lauromacrogol in 10 mL of carbon tetrachloride and perform the test as directed in the Solution method under the Infrared Spectrophotometry using a 0. Add 5. To 10 mL of the filtrate. A Content (%) of stearic acid = B × 100 . (4) Heavy metals⎯Heat 1. dilute with heptane to volume. transfer to a 50-mL volumetric flask. Calculate the% of stearic acid in the fatty acid fraction of Magnesium Stearate by the following equation. Heat on a water nearly to boil.1 g of Magnesium Stearate.1 mol/L sodium hydroxide VS: the color of the solution changes.0 mL of the test solution obtained in the Identification (1).0 mL of the test solution obtained in the Identification (1).05 mL of 0.0% of magnesium (Mg: 24. as obtained in the Purity (5).01 mol/L sulfuric acid (not more than 1. (2) Unsaturated compound⎯Shake 0. add water to make exactly 50 mL. Purify (1) Acid⎯Transfer 10. To the filtrate. Residue on Ignition Not more than 0.0 g of Magnesium Stearate in 20 mL of freshly boiled and cooled water on a water-bath for 1 minute while shaking and filter after cooling.05 mL of bromothymol blue TS and add exactly 0.0 g of Lauromacrogol into a flask and add 50 mL of neutralized ethanol.20% (1 g). evaporate on a water-bath to dryness. mix and use this solution as the test solution (keep this solution for the tests of chloride and sulfate. add 0. Description Magnesium Stearate is a white. to another flask.KP VIII 1187 carbon tetrachloride. B.0 mL of boron trifluoride-methanol TS. to a small Erlenmeyer flask fitted with a reflux condenser.40 mL of 0. (2) Dissolve 0.0%). of all of fatty acid ester peaks.02 mol/L hydrochloric acid (not more than 0.0 mL of this solution to a 10-mL volumetric flask. add water to make 50 mL and perform the test. is smooth to the touch and sticky to the skin.5 g of Lauromacrogol with 10 mL of water and 5 mL of ammonium thiocyanate-cobalt nitrate TS. 1246 cm-1 and 1110 cm-1. 2. Cool and add 5 drops of phenolphthalein TS: a red color develops. (5) Relative content of stearic acid and palmitic acid⎯Transfer about 0. add 20 mL of saturated sodium chloride solution. Magnesium Stearate is practically insoluble in water or in ethanol. (3) Sulfate⎯Perform the test with 10. wash the filter paper with 15 mL of water and combine the washing with the filtrate. when dried. Identification (1) Mix 5.0 g of Magnesium Stearate weakly at first. Prepare the control solution with 10.31). A.1 mol/L hydrochloric acid or 0. Perform a blank determination and make any necessary correction. and with the resolution between these peaks of not less than 5. pH 10. to a 250 mL flask. in the chromatogram.0% and not less than 90. System reproducibility: When the test is repeated 6 times with 1 μL of the system suitability solution under the above operating conditions: the relative deviations of the peak area of methyl palmitate and methyl stearate are not more than 6. Operating conditions Detector: A hydrogen flame-ionization detector.0 mL of the system suitability solution and dilute to 10.1 mol/L disodium ethylenediamine tetraacetate = 2. 3 mL of ammonium chloride buffer solution. Column: A fused silica capillary column about 0. Add 5.1 mol/L zinc sulfate VS until the solution changes from blue to purple. then program to increase the temperature at the rate of 5 °C per minute to 240 °C and to maintain this temperature for 5 minutes. System performance: When the procedure is run with 1 μL of the system suitability solution according to the above operating conditions. The congealing point of the fatty acid is between 18 o C and 28 o C . 5 mL of strong ammonia water.0 g of Medicinal Soap in 85 mL of neutralized ethanol by warming on a water-bath. Purity (1) Acid or alkali⎯Dissolve 5.. the inside coated with a 0.0. filter off the precipitate and wash with warm water until the washing no longer shows acidity to methyl orange TS. Transfer the precipitate to a small beaker and heat on a water-bath to complete separation of water and transparent fatty acids.1188 Monographs. calculate the% of palmitic acid in Magnesium Stearate. 30.0 mL of boron trifluoride-methanol TS. Description Medicinal Soap is white to pale yellow powder or granule.0 mL of 0. each previously dried in a desiccator (silica gel) for 4 hours and place in a small Erlenmeyer flask fitted with a reflux condenser.0% and the relative deviations of the peak area ratios of methyl palmitate to methyl stearate is not more than 1. After cooling. and Salmonella species and Escherichia coli are not observed. add 50 mL of a mixture of n-butanol and dehydrated ethanol (1 : 1). with the relative retention time of methyl palmitate to methyl stearate being about 0. Each mL of 0. add 60 mL of dilute sulfuric acid slowly and warm in a water-bath for 20 minutes.0%. Fatty Acid Dissolve 25 g of Medicinal Soap in 300 mL of hot water. mix and proceed in the test manner as directed for the preparation of the test solution.0 mL with heptane. Combine the filtrate and the washings.5 μm layer of polyethylene glycol 15000-diepoxide for gas chromatography. Medicinal Soap is sparingly soluble in water and slightly soluble in ethanol. Pipet 1. Carrier gas: Helium. System suitability Test for required detectability: Weigh accurately about 50 mg each of Stearic Acid RS and Palmitic Acid RS. Assay Transfer about 0.4305 mg Mg Packaging and Storage Preserve in tight containers. Acid value is between 185 and 205 and Iodine value is between 82 and 92. Medicinal Soap Medicinal Soap is the sodium salts of fatty acids. filter while hot through absorbent cotton and wash the filter and the residue three times with 5 mL volumes of hot neutralized ethanol.20 mL of 0. 105 °C.1 mol/L disodium ethylenediamine tetraacetate VS and 1 to 2 drops of eriochrome black T TS and mix.0% (2 g. A solution of Medicinal Soap in water (1 in 100) is alkaline.0% of the total area of all fatty acid ester peaks. Filter the fatty acid into a small beaker while warm. The methyl stearate peak and the total of the methyl stearate and methyl palmitate peaks are not less than 40. (i) Add 3 drops of phenolphthalein TS and 0. Part II Similarly. titrate the excess disodium ethylenediamine tetraacetate with 0. Confirm that the peak area of methyl stearate obtained from 1 μL of this solution is equivalent to 5 to 15% of that from the system suitability solution. respectively. Use this solution as the system suitability solution. Flow rate: Adjust the flow rate so that the retention time of methyl stearate is about 32 minutes. Heat at 45 °C to 50 °C to make the solution clear and after cooling. Loss on Drying Not more than 6. and has characteristic odor free from rancidity. accurately weighed.32 mm in inside diameter and about 30 m in length. a constant weight). methyl palmitate and methyl stearate are eluted in this order.1 mol/L sodium hydroxide VS to 40 mL of . Column temperature: Maintain at 70 °C for about 2 minutes after injection. the total fungi count is not more than 500 per g.86. Microbial Limit The total aerobic microbial count is not more than 1000 per g. add hot neutralized ethanol to make exactly 100 mL and perform the following tests quickly using this solution as the test solution at 70 o C . Injection port temperature: A constant temperature of about 220 °C. Detector temperature: A constant temperature of about 260 °C. dry at 100 °C for 20 minutes and perform the test with this material as directed under the Fats and Fatty Oils.5 g of previously dried Magnesium Stearate. wash the residue with 100 mL of hot neutralized ethanol and dry at 105 o C for 4 hours: the residue is not more than 1. Add 10 mL of ethanol.0 and -36.5 mL of diluted ethanol (7 in 10) and shake: Mentha Oil dissolves clearly.27). or with ether. Preserve in well-closed Mentha Oil Mentha Oil is the essential oil which is distilled with steam from the aerial parts of Mentha arvensis Linné var. weigh accurately about 10. evaporate on a water-bath to dryness with thorough stirring and dry at 105 o C for 3 hours. add exactly 10 mL of the internal standard solution and use this solution as the standard solution.0 mL of Mentha Oil.0% of menthol (C10H20O: 156. clear liquid. Description Mentha Oil is a colorless or pale yellow. (ii) Add 3 drops of phenolphthalein TS and 0. Flow rate: Adjust the flow rate so that the retention time of the internal standard is about 10 minutes.5 g of Medicinal Soap in a tared beaker. of the peak area of menthol to that of the internal standard. Control solution⎯Take 0. Purity (1) Clarity and color of solution⎯Take 1. has a characteristic. QT and QS . Acid Value Not more than 1. Loss on Drying Not more than 5.05 mol/L sulfuric acid VS to 40 mL of the test solution: no red color develops. respectively. with warm ethanol. Column temperature: A constant temperature of about 150 o C . Operating conditions Detector: A hydrogen flame-ionization detector.0 mL of standard lead solution (not more than 20 ppm).0%. To the solution.0 g of Mentha Oil and dissolve in ethanol to make exactly 20 mL.0 o (100 mm). Perform the test with 1 μL each of the test solution and the standard solution as directed under the Gas Chromatography according to the following operating conditions. Calculate the ratios.0% in the case of the granules. for the test solution and the standard solution. piperascens Malinvaud (Labiatae) and from which solids are removed after cooling. pleasant aroma and a pungent taste.0 mL of this solution. Mentha Oil is miscible with ethanol. dissolve by warming in 100 mL of neutralized ethanol. add 10 mL of ethanol: the solution is clear or has no more turbidity. (4) Water-insoluble substances⎯Wash thoroughly the dried substances obtained in (3) with 200 mL of water and dry at 105 o C for 4 hours: the residue is not more than 0. add 1 mL of silver nitrate TS and allow to stand for 5 minutes. Refractive Index nD20 : Between 1. with dehydrated ethanol. Pipet 10.910.0 mL of this solution. (2) Heavy metals⎯Proceed with 1. Assay Weigh accurately about 5.0 mL of standard lead solution (not more than 40 ppm). Pipet 10. Prepare the control solution with 4. Packaging and Storage containers. (2) Heavy metals⎯Proceed with 1. Specific Gravity [α ]20 D : Between 0. Separately.0 g of Mentha Oil according to Method 2 and perform the test. and again weigh the beaker. 1). packed with 25% of polyethylene glycol 6000 for gas chromatography supported on acid washed 180 μm to 250 μm siliceous earth for gas chromatography.01 mol/L hydrochloric acid VS. Selection of column: Proceed with 1 μL of the standard solution under the above operating conditions and use a column from which the internal standard and l-menthol are eluted in this order with a resolution between the two peaks being not less than 5. followed by a cool aftertaste. . Mentha Oil contains not less than 30.05 mol/L sulfuric acid VS: a red color develops.455 and 1. Mentha Oil is practically insoluble in water. (5) Alkali carbonates⎯Take the washings obtained in (4). Amount (g) of menthol (C10H20O) Q = amount (g) of l-Menthol RS × T QS Internal standard solution—A solution of n-ethyl caprylate in ethanol (1 in 25). Weigh accurately about 0. previously dried at 105 o C for 1 hour. add 10 g of sea sand (No.0% in the case of the powder and not more than 10. Column: A glass column about 3 mm in inside diameter and about 2 m in length. filter the solution through a glass filter (G4).70 mL of 0. add 3.0 g of lMenthol RS and dissolve in ethanol to make exactly 100 mL. (3) Ethanol-insoluble substances⎯Weigh accurately about 2 g of Medicinal Soap.0 g of Medicinal Soap according to Method 2 and perform the test. if any. Carrier gas: Nitrogen. Specific Optical Rotation o [α ]20 D : Between -17.15%. Prepare the control solution with 2.20 mL of 0. add 3 drops of methyl orange TS and 2 mL of 0.885 and 0. add exactly 10 mL of the internal standard solution and use this solution as the test solution.0.KP VIII 1189 the test solution: a red color develops.467. than the following control solution. add 6 mL of dilute nitric acid and water to make 50 mL. Methylcellulose contains not less than 26. and average three observed values. add 5 mL of water. and warm to rise the temperature at a rate of 2 to 5 o C per minute while stirring: the temperature. powder or granules. Methylcellulose swells. to make 200. Description Methylcellulose is a white to yellowish white. immediately cool in an ice-bath. Perform the test with the test solution at 20±0. Identification (1) Disperse evenly 1.0 g. Method II: Apply to Methylcellulose having a labeled viscosity of not less than 600 mPa·s.0 g of Methylcellulose over the surface of 100 mL of water in a beaker.1 o C as directed in the Method I under the Viscosity Determination: not less than 80% and not more than 120% of the labeled viscosity. wide-mouth bottle.0% of methoxyl group (-OCH3: 31. Use the so obtained solution as the test solution.1 mL of the test solution obtained in (2).. viscous liquid. shake and allow to stand at 25 o C : a red color develops immediately and it does not change to purple within 100 minutes.0 g. (2) Add 1.0. stopper the bottle. take off the sample attached on the walls of the bottle. and dissolve by a continuous stirring in a water-bath not exceeding 5 o C for 20 to 40 minutes. Methylcellulose is practically insoluble in dehydrated ethanol. Part II Packaging and Storage tight containers. rotation frequency.00 g on the dried basis. The kinematic viscosity of Methylcellulose is shown in millipascal second (mPa·s) on the label.0 g of Methylcellulose to 100 mL of hot water. wide-mouth bottle. in a tared. depending on the labeled viscosity. if the solution reveals yellow color by addition . equivalent to 10. Purity Heavy metals—Put 1.0 g of Methylcellulose in a 100-mL Kjeldahl flask. and allow the water to evaporate: a transparent film results. If necessary. then heat until the volume of the solution becomes to 2 to 3 mL. add exactly 50 mL of the viscous fluid obtained in (2). put them in the dispersed solution. and stir: it becomes a suspension.1190 Monographs.0 g. and stir: the resulting liquid is a clear or a slightly cloudy. stopper the bottle. (5) Pipet 50 mL of water.6 mL of ninhydrin TS.000 g on the dried basis. Cool the suspension to 5 o C . and stop the rotation for 2 minutes. using a single cylinder –type rotational viscometer. mix with a stirrer at 350 to 450 revolutions per minute for 10 to 20 minutes to obtain a homogeneous dispersion. and prepare the test solution in the same manner as directed in Method I . Perform the test with the test solution at 20±0. add hot water to make 200. Then boil gently until the solution changes to black. Operating conditions Apparatus: Brookfield type viscometer LV model Rotor No. if necessary. viscous fluid. and centrifuge the solution if necessary to expel any entrapped air bubbles. and conversion factor : Use the conditions as directed in the following table. After cooling. while gently tapping the top of the container. Place an exact portion of Methylcellulose. Not less than 600 and less than 1400 Not less than 1400 and less than 3500 Not less than 3500 and less than 9500 Not less than 9500 and less than 99500 Not less than 99500 Procedure of apparatus: Read value after 2 minutes of rotation. Repeat this procedure until to use totally 18 mL of the mixture of nitric acid and sulfuric acid.03). Preserve in light-resistant. add hot water to make 500.0% and not more than 33. according to the following operating conditions: not less than 75% and not more than 140% of the labeled viscosity. calculated on the dried basis. Add cooled water. and heat until the solution changes to black.0 and 8. heat in a water-bath for exactly 3 minutes. and heat strongly until dense white fumes are evolved. 3 Rotation frequency (/min) 60 Conversion factor 20 3 12 100 4 60 100 4 6 1000 4 3 2000 Labeled viscosity (mPa·s) Rotor No. Viscosity Method I: Apply to Methylcellulose having a labeled viscosity of less than 600 mPa·s. if necessary. boil gently until dense white fumes are evolved. After cooling. add carefully 0. Place an exact portion of Methylcellulose. Repeat this procedure until the solution no longer changes to black. in a tared. when water is added and forms a clear or slightly turbid. Methylcellulose Methylcellulose is a methyl ether of cellulose. and heat gently. is not less than 50 o C . After cooling. (3) Take 0. and allow the beaker to stand: it aggregates on the surface of water. add 9 mL of diluted sulfuric acid (9 in 10). Repeat this procedure two more times. equivalent to 4. shake.1 o C as directed in the Method II (2) under the Viscosity Determination. add a sufficient amount of a mixture of nitric acid and sulfuric acid (5 : 4) to wet the test specimen. add 2 mL of nitric acid. (4) Pour and spread out 2 to 3 mL of the viscous fluid obtained in (2) onto a glass plate. pH Allow the test solution obtained in the Viscosity to stand at 20±2 o C for 5 minutes: the pH of the so obtained solution is between 5. when a white turbidity of the solution starts to increase. Column: A glass column 3–4 mm in inside diameter and 1. Residue on Ignition Not more than 1. so that the reaction bottle can be fitted. After cooling.0 mL of the internal standard solution and 2. After allowing to stand for 5 minutes.5 and not more than 101. To these solutions add 1. Separately. In the case where hydrogen peroxide is added for the preparation of the test solution. put 0. dilute the solution with 2 to 3 mL of water. . and add water to make 40 mL each. iodomethane. and calculate the ratios .0 mL of standard lead solution in a 100-mL Kjeldahl flask. of the peak area of iodomethane to that of the internal standard for the test solution and the standard solution. Flow rate: Adjust the flow rate so that the retention time of the internal standard is about 10 minutes. having holes 20 mm in diameter and 32 mm in depth.50% or there is no evidence of a leak. Nitrogen N2: 28. In the case when the stirrer or shaker is not available. Stir or shake for 60 minutes while heating so that the temperature of the bottle content is 130±2 o C . or equivalent. and heat until the volume of the solution becomes to 2 to 3 mL. pH 3. use the upper layer of the mixture as the test solution. Perform the test with 1 to 2 µL each of the test solution and the standard solution as directed under the Gas Chromatography according to the following operating conditions. weigh accurately. System suitability System performance: When the procedure is run with 1-2 µL of the standard solution under the above operating conditions. Assay (1) Apparatus—Reaction bottle: A 5-mL pressure-tight glass vial. coated with methyl silicone polymer at the ratio of 10– 20 %. add the same amount of hydrogen peroxide. o C. 2. QT and QS . heat for 30 minutes with repeated shaking at 5-minute intervals by hand. isopropyl iodide and the internal standard are eluted in this order.01 Nitrogen contains not less than 99. observe vertically both tubes on a white background: the color obtained from the test solution is not more intense than that from the control solution (not more than 20 ppm). and use so obtained solution as the control solution. 1 mL of Nitrogen dissolves in 65 mL of water and in 8 mL of ethanol at 20 o C and at a pressure of 101. 2. add water to make 25 mL. After cooling.2 mL each of thioacetamide-alkaline glycerin TS.10 g of adipic acid in a reaction bottle. with complete separations among the three peaks. having 20 mm in outside diameter and 50 mm in height. add 60 mg to 100 mg of adipic acid. Packaging and Storage Preserve in well-closed containers. calculated on the dried basis Internal standard solution—A solution of n-octane in o–xylene (3 in 100). Use a heater capable of stirring the content of the reaction bottle by means of magnetic stirrer or by connecting the reaction bottle to a reciprocal shaker of about 100 times per minute.0 mL of the internal standard solution and 2. equipped with a septum of butyl –rubber processed having the surface with fluoroplastics. Carrier gas: Helium for thermal conductivity detector.0 . 125 to 150 µm in diameter. or Helium or Nitrogen for hydrogen flameionization detector.4. Loss on Drying Not more than 5.KP VIII 1191 of 5 mL of water. transfer to the reaction bottle. If the mass loss is less than 0. put 2. (2) Procedure—Weigh accurately about 65 mg of Methylcellulose. Description Nitrogen is colorless gas and is odorless. 105 1 hour). and use the upper layer of the mixture as the standard solution.06 to 0.0 mL of hydroiodic acid.0% of Nitrogen (N2).8–3 m in length. respectively. stopper the bottle immediately.0% (1 g). Content (%) of methoxyl group (-CH3O) Q W = T × S × 21. Operating conditions Detector: A thermal conductivity detector or hydrogen flame-ionization detector. add 10 mL of water. and weigh accurately. and use this solution as the test solution. which can be fixed tightly to vial with aluminum seal. Separately. and weigh accurately.86 QS W WS : Amount (mg) of iodomethane in the standard solution W : Amount (mg) of Methylcellose taken. Add 45 µL of iodomethane for assay through the septum using a micro-syringe. Adjust the pHs of the test solution and the control solution to 3. Allow the bottle to cool. and heat until white fumes are evolved . then proceed in the same manner for preparation of the test solution. 2 mL each of acetate buffer solution. transfer to a Nessler tube. add 1 mL of hydrogen peroxide.3 kPa.5 and water to make 50 mL each. Column temperature: A constant temperature of about 100 o C . packed with siliceous earth for gas chromatography. Heater: A square-shaped aluminum block.0 with strong ammonia solution water. and again weigh accurately. and continue heating for an additional 30 minutes. the neck 20 mm in outside diameter and 13 mm in inside diameter.0 mL of hydroiodic acid. add 18 mL of the mixture of nitric acid and sulfuric acid (5 : 4) and an amount of nitric acid equal to that used for preparation of the test solution.0% (1 g. stopper the bottle immediately. stir thoroughly. Congealing point of the fatty acids⎯Between o 17 C and 26 o C . Description Olive oil is pale yellow oil.0 mL of oxygen into the gas mixer. add Nitrogen to make 100 mL and mix thoroughly. approximately 1 mm in diameter. Specific Gravity 25 : Between 0. Wash the flask with 50 mL of petroleum ether. Olive Oil Olive Oil is the fixed oil obtained by expression from the ripe fruit of Olea europaea Linné (Oleaceae). Control solution⎯Take 50 mL of barium hydroxide TS in a Nessler tube. allow to stand and separate the petroleum ether layer. boil for 2. Proceed with 1. Olive oil is miscible with ether or with petroleum ether.1 g of sodium bicarbonate in 100 mL of freshly boiled and cooled water. Pass 1000 mL of Nitrogen into 50 mL of barium hydroxide TS in a Nessler tube during 15 minutes through a delivery tube with an orifice. Part II 1000 mL of Nitrogen at 0 o C and at a pressure of 101. packed with zeolite for Gas Chromatography (250 μm to 350 μm in particle diameter).251 g. through a directly connected polyvinyl chloride tube. cool. Unsaponifiable Matters Not more than 1. Perform the test with this solution as directed under the Gas Chromatography according to the following operating conditions. Purity (1) Drying oil⎯Mix 2 mL of Olive Oil with 10 mL of diluted nitric acid (1 in 4). Wash the petroleum ether solution repeatedly with 20 mL volumes of water until the washings show no more acidity to methyl orange TS. mix thoroughly and use this mixture as the standard gas mixture. filter. about 3 mm in inside diameter and about 3 m in length.3 kPa weighs about 1. AT of oxygen. wash the anhydrous sodium sulfate twice with 10 mL volumes of petroleum ether. Iodine Value Between 79 and 88. Dissolve the residue in acetone to make exactly 20 mL and use this solution as the test so- . System suitability System performance: Introduce 1. shake.0 g of Olive Oil. The whole or a part of it congeals at between 0 o C and 6 oC . Flow rate: Adjust the flow rate so that the retention time of oxygen is about 3 minutes. dissolve in 60 mL of sulfuric acid-hexanemethanol TS.5%. Amount (%) of Nitrogen (N2) = 100 − AT AS Operating conditions Detector: A thermal-conductivity detector. Column temperature: A constant temperature of about 50 o C .0%. Nitrogen is inert and does not support combustion. not exceeding 40 o C . Then add 5 g of anhydrous sodium sulfate. d 25 Acid Value Not more than 1. (2) Peanut oil⎯Weigh exactly about 1. Introduce 1. Carrier gas: Hydrogen or helium. Purity Carbon dioxide⎯Maintain the containers of Nitrogen at a temperature between 18 o C and 22 o C for more than 6 hours before the test and correct the volume to be at 20 o C and 101.1192 Monographs. and has bland taste. Proceed with 1.0 mL of this mixture according to the above operating conditions.0 mL of oxygen into the gas mixer.0 mL of this mixture in the same manner under Nitrogen and measure the peak area.0. Measure the peak area. Saponification Value Between 186 and 194. combine the filtrates.3 kPa.0 mL of Nitrogen into a gas-measuring tube or syringe for gas chromatography from a metal cylinder with a vaccum valve. Assay Collect the test as directed under the Purity. has faint odor which is not rancid.908 and 0. Use a column giving well-resolved peaks of oxygen and ni- trogen in this order and clearly dividing each peak. transfer to a separatory funnel and add 100 mL of water. shake. introduce 1. Separately. add 1 mL of a solution of 0. Extract the water layer with another 50 mL of petroleum ether and combine the petroleum ether layer with the former petroleum ether solution. Packaging and Storage Preserve in metal cylinders.5 hours on a water-bath under a reflux condenser. Identification The flame of a burning wood splinter is extinguished immediately in an atmosphere of Nitrogen.914. System reproducibility: When the test is repeated 6 times according to the above conditions with the standard gas mixture: the relative standard deviation of peak area of oxygen is not more than 2. keeping the end of the tube at a distance of 2 mm from the bottom of the Nessler tube: any turbidity produced is not more than that produced in the following control solution. distil the petroleum ether on a water-bath passing nitrogen. AS of oxygen. add the washing to the separatory funnel. add 1 g of powdered sodiun nitrite little by little with thorough shaking and allow to stand in a cold place for 4 to 10 hours: the mixture congeals to a white solid. Olive oil is slightly soluble in ethanol. Column: A column. add carrier gas to make exactly 100 mL . filter the washings using the former funnel. Column: A glass column.5 mL of the test solution. and use this solution as the standard solution. Perform the test with exactly 2 μL each of the test solution and the standard solution as directed under the Gas Chromatography according to the following operating conditions.474. 2 mL of dilute acetic acid. Carrier gas: Nitrogen. aromatic odor and slightly bitter taste. Control solution—To 5. Perform the test with these solu- . Pipet exactly 2 mL of this solution. 12. contains not less than 98. and water to make 50 mL(not more than 20 ppm) (4) Related substances—Dissolve 0. Flow rate: Adjust the flow rate so that the retention time of methyl benhenate is about 18 minutes. Orange oil Orange oil is the essential oil obtained by expression from the peel of the edible fruit of Citrus species (Rutaceae). then add 0.1 mL of bromocresol greensodium hydroxide-ethanol TS.0 g of Butylparaben in 25 mL of acetone. (2) Acidity—Dissolve . add acetone to make exactly 20 mL and use this solution as the standard solution. add 2 mL of dilute acetic acid and water to make 50 mL. H T and HS .0 mL of Orange Oil according to Method 2 and perform the test.0 g of Butylparaben in 10 mL of dehydrated ethanol : the solution is clear and not more intensely colored than the following control solution.0 mL of iron (III) chloride colorimetric stock solution and 2. crystalline powder. and use this solution as the test solution.KP VIII 1193 lution. Packaging and Storage tight containers. Refractive Index nD20 : Between 1. Prepare the control solution with 4. Description Butylparaben is colorless crystals or white.0 mL of Standard Lead Solution add 25 mL of acetone. Column temperature: A constant temperature of about 220 o C . (3) Heavy metals—Dissolve 1. Identification Determie the infrared spctra of Butylparaben and Butylparaben RS as directed in the potassium bromide disk method under Infrared Spectrophotometry : both spectra exhibit similar intensities of absorption at the same wavenumbers.0 mL of standard lead solution (not more than 40 ppm). and has characteristic. d 20 Purity Heavy metals⎯Proceed with 1.472 and 1. Description Orange oil is a yellow to yellow-brown liquid. Butylparaben is freely soluble in ethanol or in acetone. Preserve in light-resistant. dissolve 67 mg of methyl behenate in acetone to make exactly 50 mL.0% of Butylparaben (C11H14O3).1 mol/L sodium hydroxide VS : the solution shows a blue color.0 mL of cupper(II) sulfate colorimetric stock solution add water to make 1000 mL. add acetone to make exactly 100 mL. Prepare the control solution as follows : to 2. Packaging and Storage Preserve in tight containers. Operating conditions Detector: A hydrogen flame-ionization detector. Separately. and perform the test using this solution as the test solution. of methyl behenate for the test solution and the standard solution. Melting Point Between 68 o C and 71 o C .0 and not more than 102. add 5 mL of freshly boiled and cooled water and 0. coated with polyethylene glycol 20 M in a ratio of 5%.0 mL of cobalt(II) chloride colorimetric stock solution. and practically insoluble in water.842 and 0. Detection sensitivity: Adjust the detection sensitivity so that the peak height of methyl behenate obtained from 2 μL of the standard solution is 5 mm to 10 mm.1 mL of 0. Measure the peak heights. Pipet 0. Butylparaben O COCH2CH2CH2CH3 OH Butyl Parahydroxybenzoate C11H14O3: 194. about 3 mm in inside diameter and about 2 m in length. Orange oil is miscible with an equal volume of ethanol with turbidity. Specific Optical Rotation o [α ]20 D : Between +85 and +99 o (100 mm). respectively: H T is not higher than HS . Purity (1) Clarity and color of solution—Dissolve 1.10 g of Butylparaben in 10 mL of acetone.23 Butylparaben. Specific Gravity 20 : Between 0.848. packed with silanized siliceous earth for gas chromatography (150 μm to 180 μm in particle diameter). when dried.020 g of Butylparaben in 5 mL of dehydrated ethanol. 0 g of Butylparaben. and air-dry the plate. Each mL of 1mol/L sodium hydroxide VS = 166.1 mol/L sodium hydroxide VS : the solution shows a blue color. add exactly 20 mL of 1 mol/L sodium hydroxide VS. and perform the test using this solution as the test solution. and use this solution as the test solution. add acetone to make exactly 100 mL. Develop the plate with a mixture of methanol.2 mg of C9H10O3 Packaging and Storage Preserve in well-closed containers. Perform the test with these solutions as directed under Thin-layer Chromatography.020 g of Ethylparaben in 5 mL of dehydrated ethanol. Prepare the control solution as follows : to 2.0% of Ethylparaben (C9H10O3). Spot 2 μL each of the test solution and standard solution on a plate of silica gel with fluorescent indicator for thin-layer chromatography. and very slightly soluble in water. Develop the plate with a mixture of methanol.18 Ethylparaben. Purity (1) Clarity and color of solution—Dissolve 1. Residue on Ignition Not more than 0. Ethylparaben O COCH2CH3 the solution is clear and not more intensely colored than the following control solution. Melting Point Between 115 o C and 118 o C .0 g of Ethylparaben in 10 mL of dehydrated ethanol : Assay Weigh accurately about 1.1 mL of 0. and immediately cool in ice. Perform a blank determination. then add 0. and air-dry the plate. 2 mL of dilute acetic acid. Residue on Ignition Not more than 0. water and glacial acetic acid (70 : 30 : 1) to a distance of about 15 cm.10% (1 g). Pipet 0. heat at about 70 o C for 1 hour. OH Ethyl Parahydroxybenzoate C9H10O3: 166. Endpoint Detection Method in Titrimetry). Assay Weigh accurately about 1. contains not less than 98. Titrate the excess sodium hydroxide with 0.1 mL of bromocresol greensodium hydroxide-ethanol TS. and immediately cool in ice. Spot 2 μL each of the test solution and standard solution on a plate of silica gel with fluorescent indicator for thin-layer chromatography. Examine under ultraviolet light(main wavelength : 254 nm) : the spot other than the principal spot is not more intense than the spot obtained with the standard solution.0 mL of Standard Lead Solution add 25 mL of acetone. water and glacial acetic acid (70 : 30 : 1) to a distance of about 15 cm.10 g of Ethylparaben in 10 mL of acetone. and use this solution as the standard solution. and water to make 50 mL(not more than 20 ppm) (4) Related substances—Dissolve 0. Examine under ultraviolet light(main wavelength : 254 nm) : the spot other than the principal spot is not more intense than the spot obtained with the standard solution. when dried. Titrate the excess sodium hydroxide with 0. Each mL of 1 mol/L sodium hydroxide VS = 194. Endpoint Detection Method in Titrimetry). Control solution—To 5. 12.0 mL of iron (III) chloride colorimetric stock solution and 2. (2) Acidity—Dissolve .2 mg of C11H14O3 Packaging and Storage Preserve in well-closed containers. Description Ethylparaben is colorless crystals or white.5 mol/L sulfuric acid VS up to the second equivalent point(potentiometric titration.1194 Monographs.0 mL of cobalt(II) chloride colorimetric stock solution.5 mL of the test solution. heat at about 70 o C for 1 hour. add 2 mL of dilute acetic acid and water to make 50 mL. Part II tions as directed under Thin-layer Chromatography.0 and not more than 102. crystalline powder.5 mol/L sulfuric acid VS up to the second equivalent point(potentiometric titration. add exactly 20 mL of 1 mol/L sodium hydroxide VS. .0 g of Ethylparaben. Identification Determie the infrared spctra of Ethylparaben and Ethylparaben RS as directed in the potassium bromide disk method under Infrared Spectrophotometry : both spectra exhibit similar intensities of absorption at the same wavenumbers.0 mL of cupper(II) sulfate colorimetric stock solution add water to make 1000 mL. Ethylparaben is freely soluble in ethanol or in acetone.10% (1 g). add 5 mL of freshly boiled and cooled water and 0. (3) Heavy metals—Dissolve 1. Perform a blank determination.0 g of Ethylparaben in 25 mL of acetone. 20 Propylparaben. 2 mL of dilute acetic acid. when dried. Purity (1) Clarity and color of solution—Dissolve 1.0% of Propylparaben (C10H12O3). Control solution—To 5.1 mL of 0. and perform the test using this solution as the test solution. Perform a blank determination.0 mL of Standard Lead Solution add 25 mL of acetone.0 mL of cobalt(II) chloride .15 Methylparaben. Spot 2 μL each of the test solution and the standard solution on a plate of silica gel with fluorescent indicator for thin-layer chromatography. Identification Determie the infrared spctra of Methylparaben and Methylparaben RS as directed in the potassium bromide disk method under Infrared Spectrophotometry : both spectra exhibit similar intensities of absorption at the same wavenumbers.0 mL of iron (III) chloride colorimetric stock solution and 2. contains not less than 98. Prepare the control solution as follows : to 2. OH Methyl Parahydroxybenzoate C8H8O3: 152.10 g of Methylparaben in 10 mL of acetone. Description Propylparaben is colorless crystals or white. Pipet 0. o o Melting Point Between 125 C and 128 C .0 g of Methylparaben in 25 mL of acetone.10% (1 g). Perform the test with these solutions as directed under Thin-layer Chromatography. Purity (1) Clarity and color of solution—Dissolve 1.0 and not more than 102. Propylparaben O COCH2CH2CH3 OH Propyl Parahydroxybenzoate C10H12O3: 180. Propylparaben is freely soluble in ethanol or in acetone. and very slightly soluble in water. Methylparaben O COCH3 Residue on Ignition Not more than 0. water and glacial acetic acid (70 : 30 : 1) to a distance of about 15 cm. and immediately cool in ice.0 mL of cobalt(II) chloride colorimetric stock solution.0 mL of cupper(II) sulfate colorimetric stock solution add water to make 1000 mL. crystalline powder. Methylparaben is freely soluble in ethanol or in acetone. Titrate the excess sodium hydroxide with 0. add 2 mL of dilute acetic acid and water to make 50 mL. and slightly soluble in water. Endpoint Detection Method in Titrimetry).1 mg of C8H8O3 Packaging and Storage Preserve in well-closed containers.0% of Methylparaben (C8H8O3). add 5 mL of freshly boiled and cooled water and 0. and use this solution as the test solution.5 mol/L sulfuric acid VS up to the second equivalent point(potentiometric titration. heat at about 70 o C for 1 hour.0 g of Methylparaben in 10 mL of dehydrated ethanol : the solution is clear and not more intensely colored than the following control solution. (3) Heavy metals—Dissolve 1. contains not less than 98. Control solution—To 5. Melting Point Between 96 o C and 99 o C . when dried. add acetone to make exactly 100 mL. then add 0.1 mol/L sodium hydroxide VS : the solution shows a blue color. add exactly 20 mL of 1 mol/L sodium hydroxide VS. 12.1 mL of bromocresol greensodium hydroxide-ethanol TS. crystalline powder. Description Methylparaben is colorless crystals or white.0 g of Methylparaben. Each mL of 1 mol/L sodium hydroxide VS = 152. Identification Determie the infrared spctra of Propylparaben and Propylparaben RS as directed in the potassium bromide disk method under Infrared Spectrophotometry : both spectra exhibit similar intensities of absorption at the same wavenumbers. and water to make 50 mL(not more than 20 ppm) (4) Related substances—Dissolve 0.KP VIII 1195 mixture of methanol. (2) Acidity—Dissolve .0 and not more than 102. and air-dry the plate. and use this solution as the standard solution.020 g of Methylparaben in 5 mL of dehydrated ethanol.5 mL of the test solution. Examine under ultraviolet light(main wavelength : 254 nm) : the spot other than the principal spot is not more intense than the spot obtained with the standard solution.0 g of Propylparaben in 10 mL of dehydrated ethanol : the solution is clear and not more intensely colored than the following control solution. Develop the plate with a Assay Weigh accurately about 1. 1 mL of 0. Paraffin Paraffin is a mixture of solid hydrocarbons obtained from petroleum.92 (proceed as directed in the Specific gravity (2) under the Fats and Fatty Oils).5 g of Paraffin with 0. and use this solution as the standard solution. water and glacial acetic acid (70 : 30 : 1) to a distance of about 15 cm. Description Paraffin is colorless or white.5 mol/L sulfuric acid VS up to the second equivalent point(potentiometric titration.0 mL of iron (III) chloride colorimetric stock solution and 2. (4) Sulfur compounds⎯Take 4. 0.5 g of sulfur with shaking carefully: the odor of hydrogen sulfide is perceptible. Melting Point Between 50 o C and 75 o C (Method 2). then between 450 o C and 550 o C to ash. Endpoint Detection Method in Titrimetry). and air-dry the plate.0 g of Paraffin according to Method 3 and perform the test (not more than 2 ppm). (2) Heavy metals⎯Ignite 2.0 mL of ferric chloride colorimetric stock solution and shake vigorously. Packaging and Storage Preserve in well-closed containers.0 g of Paraffin placed in a Nessler tube at a temperature near the melting point. 2 mL of dilute acetic acid. 12.0 g of Propyl Parahydroxy benzoate. Perform the test with these solutions as directed under Thin-layer Chromatography. Prepare the control solution as follows: to 2. add 2 mL of dilute acetic acid and water to make 50 mL (not more than 10 ppm). Perform a blank determination. add 2 mL of dilute acetic acid and water to make 50 mL and perform the test. immediately shake vigorously and vertically for 3 seconds and warm for 1 minutes in a water-bath at 70 o C . To the residue.0 g of Paraffin with 10 mL of hot water and 1 drop of phenolphthalein TS in a water-bath for 5 minutes and shake vigorously: a red color is not produced.020 g of Propylparaben in 5 mL of dehydrated ethanol. Each mL of 1 mol/L sodium hydroxide VS = 180.20 mL of 0.0 mL of Standard Lead Solution add 25 mL of acetone. further add 2 drops of a clear saturated solution of lead monoxide in a solution of sodium hydroxide (1 in 5) and heat for 10 minutes at 70 o C with occasional shaking: no dark brown color develops in the aqueous layer. Assay Weigh accurately about 1. (3) Arsenic⎯Prepare the test solution with 1. then add 0. add acetone to make exactly 100 mL.10% (1 g). Identification (1) Heat Paraffin strongly in a porcelain crucible and ignore: it burns with a bright flame and the odor of paraffin vapor is perceptible. (5) Readily carbonizable substances⎯Melts 5. Prepare the control solution as follows : to 2. and use this solution as the sample solution.0 g of Paraffin in a crucible. (2) Heat 0. Add 5 mL of sulfuric acid for the test of readily carbonizable substances and warm at 70 o C for 5 minutes in a water-bath. (2) Acidity—Dissolve .5 mL of the sample solution. Pipet 0. Examine under ultraviolet light(main wavelength : 254 nm) : the spot other than the principal spot is not more intense than the spot obtained with the standard solution. Spot 2 μL each of the sample solution and standard solution on a plate of silica gel with fluorescent indicator for thin-layer chromatography. add 2 mL of dilute acetic acid and water to make 50 mL. . add 2 mL of hydrochloric acid and evaporate on a water-bath to dryness.1 mL of bromocresol greensodium hydroxide-ethanol TS. add 2 mL of dehydrated ethanol.5 mL of cupric sulfate colorimetric stock solution and 5 mL of liquid paraffin to 3. and water to make 50 mL(not more than 20 ppm) (4) Related substances—Dissolve 0.0 g of Paraffin. Paraffin is sparingly soluble in ether and practically in- soluble in water. add exactly 20 mL of 1 mol/L sodium hydroxide VS. Repeat this procedure five times: the color of the sulfuric acid layer is not more intense than that of the following control solution.2 mg of C10H12O3 Packaging and Storage Preserve in well-closed containers. Develop the plate with a mixture of methanol. and immediately cool in ice.10 g of Propylparaben in 10 mL of acetone. Titrate the excess sodium hydroxide with 0.5 mL of cobaltous chloride colorimetric stock solution. and perform the test using this solution as the test solution. heat at about 70 o C for 1 hour. Add 0.1 mol/L sodium hydroxide VS : the solution shows a blue color.0 mL of cupper(II) sulfate colorimetric stock solution add water to make 1000 mL. first moderately until chared. (3) Heavy metals—Dissolve 1.02mol/L sodium hydroxide VS to this solution and shake: a red color is produced. add 5 mL of freshly boiled and cooled water and 0. Residue on Ignition Not more than 0. in ethanol or in dehydrated ethanol. Remove the tube from the water-bath. slightly clear. odorless and tasteless. Control solution⎯Add 1.0 g of Propylparaben in 25 mL of acetone.1196 Monographs. crystalline mass.0 mL of standard lead solution. Part II colorimetric stock solution. Cool. Purity (1) Acid or alkali⎯Boil 10. 20 Specific gravity─ d 20 : About 0. and perform the test.5 mL of cobaltous chloride colorimetric stock solution and 0. Liquid Paraffin is freely soluble in ether. Solid paraffin.5 mL of strong hydrogen peroxide water and fire to burn. to a Nessler tube and cool in ice-water for 4 hours: the turbidity produced. remove the tube from the water-bath and immediately shake vigorously and vertically for 5 seconds. Transfer the lower layer to a 10-mL glass-stopered centrifuge tube and centrifuge between 2500 revolutions per minute and 3000 revolutions per minute for about 10 miutes and use the clear solution as the test solution. Boiling point⎯Above 300 o C . Light Liquid Paraffin is freely soluble in ether and practically insoluble in water or in ethanol. Acid or alkali. d 20 Not less than 37mm2/s (Method 1. previously dried at 105 o C for 2 hours.890.5 mL of 0.0 g of Liquid Paraffin. centrifuge between 2500 and 3000 revolutions per minute for about 10 minutes and use the clear solution as a control solution. Control solution⎯Mix 3. Purity (1) Odor.01 mol/L hydrochloric acid. Immediately determine the absorbance of the test solution using the control solution as the blank: not more than 0. 37. Specific Gravity 20 : Between 0. Tocopherol of a suitable from may be added at a concentration not exceeding 0. (8) Readily carbonizable substances⎯Transfer 5 mL of Liquid Paraffin to a Nessler tube and add 5 mL of sulfuric acid for Readily Carbonizable Substances. shake vigorously for 2 minutes with 5.KP VIII 1197 Liquid Paraffin Liquid Paraffin is a mixture of liquid hydrocarbons obtained from petrolatum. and is odorless and tasteless. further add 2 drops of a clear saturated solution of lead monoxide in a solution of sodium hydroxide (1 in 5) and heat for 10 minutes at 70 o C with occasional shaking: no dark brown color develops in the aqueous layer.0 mL of dimethylsufoxide and allow to stand for 15 minutes. Add 10 mL of an ethanol solution of magnesium nitrate (1 in 50). (4) Arsenic⎯Prepare the test solution with 1. if any. Description Light Liquid Paraffin is a clear.10 at the wavelength region between 260 nm and 350 nm. After heating in a water-bath for 2 minutes. Transfer the lower layer to a 10-mL glass-stoppered centrifuge tube. very slightly soluble in dehydrated ethanol and practically insoluble in water or in ethanol.0 mL of dimethylsulfoxide and allow to stand for 2 minutes. 20 : Between 0. Tocopherol of a suitable form may be added at a concentration not exceeding 0.8 o C ). Shake this solution vigorously for 2 minutes with 5.50 mL of cupric sulfate colorimetric stock solution. Repeat this procedure four times: the Liquid Paraffin layer remains unchanged in color and the sulfuric acid layer is not more intense than the following control solution. d 20 Viscosity Less than 37 mm2/s (Method 1.001% as a stabilizer. (3) Heavy metals⎯Proceed as directed in the Purity (2) under Paraffin.860 and 0. Control solution⎯Take 1. add 6 mL of dilute nitric acid and water to make 50 mL. and is odorless and tasteless. 37. (5) Solid paraffin⎯Transfer 50 mL of Liquid Paraffin. add 1 mL of silver nitrate TS and allow to stand for 5 minutes. add 2 mL of dehydrated ethanol. transparent.001% as a stabilizer. transfer to a 100-mL separatory funnel and wash out the cylinder with 25 mL of n-hexane and shake vigorously. Shake this solution with 0. Boiling point⎯Above 300 o C . (6) Sulfur compounds⎯ Take 4. Specific Gravity Viscosity o C ). is not more intense than that of the following control solution.20 mL/L of 0.870. Transfer 25 mL of n-hexane to another 50-mL separatory funnel.8 Purity (1) Odor⎯Transfer a suitable amount of Liquid Paraffin to a small beaker and heat on a water-bath: a foreign odor is not perceptible.0 g of Paraffin. Description Liquid Paraffin is colorless.02 mol/L sodium hydroxide: a red color develops. Polycyclic aromatic hydrocarbons and Readily carbonizable substances⎯Proceed as di- . Identification Proceed as directed in the Identification under Paraffin. according to Method 3. Light Liquid Paraffin Light Liquid Paraffin is a mixture of hydrocarbons obtained from petroleum. oily liquid.830 and 0. (2) Acid or alkali⎯Shake vigorously 10 mL of Liquid Paraffin with 10 mL of hot water and 1 drop of phenolphthalein TS: no red color develops. add 1. nearly free from fluorescence. colorless oily liquid. Packaging and Storage Preserve in tight containers. Identification Proceed as directed in the Identification under Paraffin. (not more than 2 ppm). (7) Polcyclic aromatic hydrocarbons⎯Take 25 mL of Liquid Paraffin by a 25-mL cylinder. nearly free from fluorescence.0 mL of ferric chloride colorimetric stock solution with 1. Sulfur compounds. heat it with 40 mL of dilute hydrochloric acid and 20 mL of water until the oily layer is entirely clear.5%. Iodine Value Between 84 and 103. Identification Saponify 5 g of Peanut Oil by boiling with 2.5 mL of ammonia-ethanol TS 2 to 3 drops of silver nitrate TS and warm the mixture at about 50°C for 5 minutes and protected from light: no brown color develops. When the solution prepared by dissolving 0. Boil the fatty acids with 50 mL of diluted hydrochloric acid (1 in 100). White Petrolatum White Petrolatum is a decolorized and purified mixture of hydrocarbons obtained from petroleum. Evaporate the ethanol.916.71. transfer the mixture to a porcelain dish and dilute with water: no odor of nitrobenzene is perceptible. Description White Petrolatum is a white to pale yellow. (6). Specific gravity⎯ d 2020 : Between 0.1198 Monographs. dissolve the residue in 50 mL of hot water and add dilute hydrochloric acid in excess until the free fatty acids separate as an oily layer. Dissolve the solid fatty acid in 25 mL of diluted ethanol (9 in 10) with the aid of gentle heat and then cool to 15 o C to crystallize the fatty acids. allow to stand for 30 minutes. Place the precipitate in a beaker. not less than 90%. add 2. Saponification Value Between 188 and 196. clear. Acid Value Not more than 0. Packaging and Storage Preserve in tight containers. Filter the supernatant liquid. To the ether solution. Peanut Oil is miscible with ether or petroleum ether.5 mL of ethanol. Peanut Oil is slightly soluble in ethanol. allow the fatty acids to solidify and press them between dry filter papers to exclude moisture. Packaging and Storage Preserve in tight containers. Unsaponifiable Matters Not more than 1.1 g of the fatty acids in 10 mL of ethanol is not darkened by the addition of 2 drops of sodium sulfide TS. Petroleum Benzin Petroleum Benzin is a mixture of low boiling point hydrocarbons from petroleum. is odorless and . Petroleum Benzin shows no fluorescence.5 mL of sodium hydroxide solution (3 in 10) and 12. (2) Sulfur compounds and reducing substances⎯Take 10 mL of Petroleum Benzin. Description Peanut Oil is a pale yellow. unctuous mass. (7) and (8) under Liquid Paraffin (2) Heavy metals and arsenic⎯Proceed as directed in the Purity (2) and (3) under Paraffin Packaging and Storage Preserve in tight containers. Petroleum Benzin is miscible with dehydrated ethanol or ether. add a solution of 1 g of lead acetate in 40 mL of ethanol and allow the mixture to stand for 18 hours. Distilling Range Between 50°C and 80°C. Petroleum Benzin is practically insoluble in water.2. (3) Fatty oil and sulfur compounds⎯Drop and evaporate 10 mL of Petroleum Benzin in small volumes on odorless filter paper spread on a previously warmed glass plate: no spot or no foreign odor is perceptible. (4) Benzene⎯Warm 5 drops of Petroleum Benzin with 2 mL of sulfuric acid and 0. odorless or has a slight odor. (5). in vacuum) for 4 hours: the melting point of the dried crystals is between 73 o C and 76 o C .65 and 0. Purity (1) Acid⎯Shake vigorously 10 mL of Petroleum Benzin with 5 mL of water for 2 minutes and allow to stand: the separated aqueous layer does not change moistened blue litmus paper to red. (6) Readily carbonizable substances⎯Shake vigorously 5 mL of Petroleum Benzin with 5 mL of sulfuric acid for readily carbonizable substances for 5 minutes in a Nessler tube and allow to stand: the sulfuric acid layer is not more intense than Color Matching Fluid A. (5) Residue on evaporation⎯Evaporate 140 mL of Petroleum Benzin on a water-bath to dryness and heat the residue at 105°C to constant weight: not more than 1 mg. Recrystallize them from diluted ethanol (9 in 10) 20 mL and dry in a dessicator (P2O5. Petroleum Benzin is very flammable. Congealing point of the fatty acids⎯Between 22 o C and 33 o C . 25 Specific gravity⎯ d 25 : Between 0.909 and 0. Description Petroleum Benzin is a colorless. volatile liquid. remove the separated fatty acids and dissolve them in 75 mL of ether. and a mild taste. Cool the mixture. clear oil. homogeneous.5 mL of nitric acid for about 10 minutes. Part II rected in the Purity (1). (2). and has a characteristic odor. Store remote from fire and not exceeding 30°C. cool and decant the water layer. Peanut Oil Peanut Oil is the fixed oil obtained from the seeds of Arachis hypogaea Linné (Leguminosae). transfer the precipitate to the filter with the aid of ether and filter by suction. Yellow Petrolatum dissolves in ether. according to Method 3 and perform the test. Melting Point 3). Mix this solution with 20.0 g of White Petrolatum and boil for 10 minutes under a reflux condenser. Cool the mixture.0 g of White Petrolatum according to Method 2 and perform the test. White Petrolatum is practically insoluble in water. (3). (5) Sulfur compound⎯Take 4. (4) Arsenic⎯Prepare the test solution with 1. White Petrolatum becomes a clear liquid when warmed. Residue on Ignition Not more than 0. until the color of the solution changes to pale red. add 50 mL of sodium hydroxide solution (1 in 5) and boil for 30 minutes under a reflux condenser. Control solution⎯Add 3.40 mL of 0.0 g of White Petrolatum.0 g of White Petrolatum. Melting Point 3).05% (2 g). Use following control solution. Heavy metals.0 mL of standard lead solution (not more than 30 ppm).2 mL of cobaltous chloride colorimetric stock solution. Phenol is very soluble in ethanol or in ether and soluble in water.01 mol/L sodium hydroxide VS. Packaging and Storage Preserve in tight containers. unctuous mass.0% and not more than 101. Phenol (10 g) is liquefied by addition of 1 mL of water.8 mL of ferric chloride colorimetric stock solution and add 1. Phenol cauterizes the skin. and has a characteristic odor. Yellow Petrolatum is slightly soluble in ethanol and practically insoluble in water.6 mL of ferric chloride colorimetric stock solution. To the combined aqueous layer. add 200 mL of dilute sulfuric acid: neither oily matter nor precipitate is produced. turning it white. then add 1. in ethanol or in dehydrated ethanol. (5). (3) Heavy metals⎯Proceed with 1. (6) and (7) under White Petroleum.4 mL of water to 1.KP VIII 1199 tasteless. . shake vigorously for 5 minutes and then draw off the aqueous layer. White Petrolatum dissolves in ether making a clear liquid or producing slight insoluble substances. Between 38 o C and 60 o C (Method Purity (1) Color⎯Proceed as directed in the Purity (1) under White Petroleum. Residue on Ignition Not more than 0.0% of Phenol (C6H6O).5 mL of strong hydrogen peroxide water and ale to burn (not more than 2 ppm).1 mol/L sodium hydroxide VS with vigorous shaking: the color of the solution remains red. Phenol OH Carbolic Acid C6H6O: 94. Further add 2 drops of methyl orange TS: no red color is produced. add 1 drop of phenolphthalein TS and boil: no red color is produced. (2) Acid or alkali⎯Take 35. Add 2 to 3 drops of phenolphthalein TS to the mixture and 0. The color changes gradually through red to dark red by light or air. clear liquid with slight fluorescence when warmed. making a clear liquid or producing slight insoluble substances. when observed transversely from side against a white background. Prepare the control solution with 3. add 1 drop of phenolphthalein TS and titrate with 0.11 Phenol contains not less than 98. separate the aqueous layer and filter. To the aqueous layer. Fats and fatty oils or resins⎯Proceed as directed in the Purity (2). Between 38 o C and 60 o C (Method Purity (1) Color⎯Melt White Petrolatum by warming and pour 5 mL into a test tube and keep the content in a liquid condition: the liquid is not more intense than the following control solution. if necessary. Yellow Petrolatum becomes a yellow. Yellow Petrolatum Yellow Petrolatum is a purified mixture of hydrocarbons obtained from petroleum. Sulfur compound. Packaging and Storage Preserve in tight containers. Add 10 mL of an ethanol solution of magnesium nitrate (1 in 50). odorless and tasteless. (4).05% (2 g). (2) Acid or alkali. add 100 mL of hot water. homogeneous. Description Phenol is a colorless to slightly red crystal or crystalline mass. Treat twice the White Petrolatum layer in the same manner using 50 mL volumes of hot water.0 g of White Petrolatum. (7) Fats and fatty oils or rosins⎯Take 10. (6) Organic acids⎯Take 100 mL of dilute ethanol. add 2 mL of dehydrated ethanol and 2 drops of sodium hydroxide solution (1 in 5) saturated with lead monoxide. Arsenic.0 g of White Petrolatum. Organic acids. warm the mixture for 10 minutes at about 70 o C with frequent shaking and allow to cool: no dark color is produced. Control solution⎯Take 3. Description Yellow Petrolatum is a yellow. in petroleum benzine or in turpentine oil. crystalline mass. turning it white. Description Phenol for Disinfection is a colorless to slightly red crystal. Phenol for Disinfection Carbolic Acid for Disinfection Phenol for Disinfection contains not less than 95. Each mL of 0. accurately weighed.05 mol/L bromine VS. Purity (1) Clarity of solution⎯Dissolve 1.0% and not more than 101. (2) Residue on evaporation⎯Weigh accurately about 5 g of Phenol. Assay Dissolve about 1. Description Liquefied Phenol is a colorless or slightly reddish liquid. stopper the flask and shake thoroughly. Titrate the liberated iodine with 0.5686 mg of C6H6O Packaging and Storage tight containers. The color changes gradually to dark red on exposure to light or air. Add 2 drops of methyl orange TS: no red color develops. Liquefied Phenol is miscible with ethanol. Congealing point⎯About 30 o C . Perform a blank determination and make any necessary correction. Assay Weigh accurately about 1 g of Phenol for Disinfection. stopper immediately.0% of phenol (C6H6O: 94.10%. Identification (1) Add 1 drop of ferric chloride TS to 10 mL of a solution of Phenol (1 in 100): a blue-purple color develops. Transfer exactly 25 mL of this solution to an iodine flask. or liquid containing the crystal and has a characteristic odor. (2) Take 5 mL of a solution of Phenol for Disinfection (1 in 10000) and add bromine TS drop-wise: a white precipitate is formed and it dissolves at first upon shaking but becomes permanent as excess of the reagent is added. proceed as directed in the Assay under Phenol. add exactly 30 mL of 0.11). turning it white. allow to stand for 15 minutes. (2) Residue on evaporation⎯Weigh accurately about 5.7 g of Liquefied Phenol.0% of phenol (C6H6O: 94. Liquefied Phenol cauterizes the skin. Identification (1) Take 10 mL of a solution of Phenol for Disinfection (1 in 100) and add 1 drop of ferric chloride TS: a blue-purple color is produced. Specific gravity─ d 2020 : About 1. and has a characteristic odor. stopper the flask immediately and shake well.0 g of Phenol for Disinfection in 15 mL of water: the solution is clear. Add 1 mL of chloroform.1200 Monographs. but becomes permanent as excess of the reagent is added.5 g of Phenol and dissolve in water to make exactly 1000 mL.11). Purity (1) Clarity and color of solution and acidity or alkalinity⎯Dissolve 1. (2) Add bromine TS dropwise to 5 mL of a solution of Phenol (1 in 10. Part II Congealing point⎯About 40 o C .000): a white precipitate is produced.0 g of Phenol for Disinfection. .1 mol/L sodium thiosulfate VS (indicator: 1 mL of starch TS). 10 g of Phenol for Disinfection is liquefied by addition of 1 mL of water. Boiling Point Not more than 182 o C .5685 mg of C6H6O Packaging and Storage tight containers.0 g of Phenol in 15 mL of water: the solution is clear and neutral or only faintly acid. which at first dissolves with shaking. then 5 mL of hydrochloric acid and stopper the flask immediately. and dissolve in water to make exactly 1000 mL. Assay Weigh accurately about 1.05 mol/L bromine VS = 1. Liquefied Phenol contains not less than 88. Preserve in light-resistant. Liquefied Phenol Liquefied Carbolic Acid Liquefied Phenol is Phenol maintained in a liquid condition by the presence of 10% of Water or Purified Water. Each mL of 0. Phenol for Disinfection is very soluble in ethanol or in ether and freely soluble in water. Shake the flask repeatedly for 30 minutes. with ether or with glycerin.065. evaporate on a water-bath and dry the residue at 105 o C for 1 hour: not more than 0.05 mol/L bromine VS and 5 mL of hydrochloric acid. Pipet exactly 25 mL of the solution into an iodine flask. add exactly 30 mL of 0. evaporate on a water-bath and dry the residue at 105 o C for 1 hour: not more than 0. Preserve in light-resistant.05%. A mixture of equal volumes of Liquefied Phenol and glycerin is miscible with water. then add 7 mL of potassium iodide TS. Phenol for Disinfection cauterizes the skin. Purity Proceed as directed in the Purity under Phenol.05 mol/L bromine VS = 1. Identification Proceed as directed in the Identification under Phenol. accurately weighed. Amount (mg) of Ethylene Glycol Each mL of 0.5 m in length. Titrate with 0. if necessary. HTa and HAs.25%. coated with D-sorbitol at the ratio of 12%. about 3 mm in inside diameter and about 1. Perform the test with 2 μL each of the test solution and the standard solution as directed under the Gas Chromatography according to the following operating conditions.0 mL of 0.5 mol/L sodium hydroxide VS until a pale red color remains for not less than 15 seconds.0 g of Polyethylene Glycol 400 in 20 mL of neutralized ethanol and add 2 drops of phenolphthalein TS and 0.5 mol/L sodium hydroxide VS and 5 drops of a solution of phenolphtalein in pyridine (1 in 100). exactly measured. add about 1. respectively and calculate the amount of ethylene glycol and diethylene glycol: the sum of the contents of ethylene glycol and diehtylene glycol is not more than 0. Perform a blank determination and make any necessary correction. Add 7 mL of potassium iodide TS. Purity (1) Acid⎯Dissolve 5. Congealing point⎯Between 4 o C and 8 o C .5685 mg of C6H6O Packaging and Storage tight containers.0 g of Polyethylene Glycol 400 in water to make exactly 10 mL and use this solution as the test solution. Preserve in light-resistant. Determine the peak heights. for the test solution and the standard solution.1 mol/L sodium thiosulfate VS (indicator: 1 mL of starch TS). has no odor or a slight. to the level so that the mixture in the bottle soaks completely in water. Flow rate: Adjust the flow rate so that the retention time of diethylene glycol is about 3 minutes. Detection sensitivity: Adjust the detection sensitivity so that the peak height of diethylene glycol obtained from 2 μL of the standard solution composes about 80% of the full scale.110 and 1. System suitability System performance: When the procedure is run with 2 μL of the standard solution under the above operating conditions and calculate the resolution. pH Dissolve 1.0 g of Polyethylene Glycol 400 in 20 mL of water: the pH of this solution is between 4. with ethanol or with pyridine. add 1 mL of a solution of phosphomolybdic acid (1 in 10): a yellow-green precipitate is formed. HTb and HSb. of diethylene glycol. Pipet exactly 25 mL of this solution into an about 200 mL stoppered pressure bottle. Description Polyethylene Glycol 400 is a clear. Shake the bottle vigorously to dissolve the solid and allow to stand for 16 hours or more. Polyethylene Glycol 400 is soluble in ether. Remove the bottle from the bath and allow to cool in air to room temperature. Perform a blank determination and make any necessary correction: Average molecular mass is between 380 and 420.20 mL of 0. To the filtrate. shake well and titrate the liberated iodine with 0. Column: A column. Carrier gas: Nitrogen or helium.05 mol/L bromine VS = 1. Maintain the temperature of the bath at 98 ± 2 o C for 30 minutes. having a temperature of 98 ± 2 o C . in a 1000 mL light-resistant stoppered bottle.KP VIII 1201 shake for 30 minutes and allow to stand for 15 minutes.0. respectively and the H Tb 1 × H Sb 10 Operating conditions Detector: A hydrogen flame-ionization detector. represented by the formula [HOCH2(CH2OCH2)n CH2OH]. Polyethylene Glycol 400 is miscible with water. Add 50. shake and filter. peak heights. Polyethylene Glycol 400 is slightly hygroscopic. ethylene glycol and diethylene glycol are eluted in this order. colorless and viscous liquid. . packed with siliceous earth for gas chromatography. Specific gravity⎯ d 2020 : Between 1.5 g of Polyethylene Glycol 400. with methanol. of ethylene glycol. characteristic odor. add 1 mL of barium chloride TS. for the test solution and the standard solution. 150 µm to 180 µm in particle diameter. in which the value of n ranges from 7 to 9. Weigh accurately about 50 mg each of ethylene glycol RS and diethylene glycol RS. stopper the bottles wrap it securely with strong cloth and immerse in a water-bath.140. Column temperature: A constant temperature of about 165 o C . stopper immediately. (2) Ethylene glycol and diethylene glycol⎯Dissolve 4. Average molecular mass Add 42 g of phthalic anhydride to 300 mL of freshly distilled pyridine. Identification Dissolve 50 mg of Polyethylene Glycol 400 in 5 mL of dilute hydrochloric acid. dissolve in water to make exactly 100 mL and use this solution as the standard solution. = amount (mg) of ethylene glycol RS × H Ta 1 × H Sa 10 Amount (mg) of Ethylene Glycol = amount (mg) of diethylene glycol RS × Polyethylene Glycol 400 Macrogol 400 Polyethylene Glycol 400 is a polymer of ethylene oxide and water.1 mol/L sodium hydroxide VS: the solution is red.0 and 7. 10% (1 g). very slightly soluble in dehydrated ethanol and practically insoluble in ether. To the filtrate. in which the value of n is 5 or 6 for the lower polymer and from 28 to 36 for the higher.13 to 0. flakes or power. volumetric titration. shake with 25. To the filtrate.0 g of Polyethylene Glycol 1500 in 50 mL of water: the solution is clear and colorless. add a mixture of water and freshly distilled acetonitrile (1 : 1) to make exactly 25 mL and use this solution as the standard solution. distil slowly in vaccum of 0.0 g of Polyethylene Glycol 1500 in 20 mL of neutralized ethanol and add 2 drops of phenolphthalein TS and 0. Polyethylene Glycol 4000 is very soluble in water. is colorless or has a faint.0% (2 g. Identification Dissolve 50 mg of Polyethylene Glycol 4000 in 5 mL of dilute hydrochloric acid. freely soluble in methanol. Perform the test with these solutions as directed under the Ultraviolet-visible Spectrophotometry within 2 to 5 minutes: the absorbance of the solution from the test solution at the wavelength of maximum absorption at about 450 nm is not larger than the absorbance of the solution from the standard solution.5. add 1 mL of a solution of phosphomolybdic acid (1 in 10): a yellow-green precipitate is produced.0 and 7.0. Water Not more than 1. shake and filter.0 g of Polyethylene Glycol 1500 in distilling flask. Polyethylene Glycol 4000 Macrogol 4000 Polyethylene Glycol 4000 is a polymer of ethylene oxide and water. shake vigorously.0 mL each of the test solution and the standard solution and add to each 15. in which the value of n ranges from 59 to 84.1 mol/L sodium hydroxide VS: the solution is red. warm to dissolve. smooth petrolatum-like solid. direct titration). if necessary.0 g of Polyethylene Glycol 4000 in 20 mL of water: the pH of this solution is between 4.27 kPa and take 25 mL of the distillate in a 100-mL container with 1-mL graduation. freely soluble in methanol or in pyridine and practically insoluble in dehydrate ethanol or in ether.10% (1 g). pH Dissolve 1.0 mL of freshly distilled acetonitrile and use this solution as the test solution. (2) Acid⎯Dissolve 5.0 mL of cerium (IV) diammonium nitrate TS. cool in ice-water. shake and filter. if necessary. Take 10. is odorless or has a faint. Part II Averagemolecularmass Amount(g) of sample× 400 = a −b a : Volume (mL) of 0.1202 Monographs. Identification Dissolve 50 mg of Polyethylene Glycol 1500 in 5 mL of dilute hydrochloric acid. Polyethylene Glycol 1500 Macrogol 1500 Polyethylene Glycol 1500 is a mixture containing equal amounts of lower and higher polymers of ethylene oxide and water.0 and 7.5 mol/L sodium hydroxide VS used in the blank determination. characteristic odor. if necessary. warm to room temperature and add water to make exactly 25 mL. Description Polyethylene Glycol 1500 is a white. Separately. Congealing point⎯Between 53 o C and 57 o C . Residue on Ignition Not more than 0. b : Volume (mL) of 0.5 mg of diethylene glycol RS. Congealing point⎯Between 37 o C and 41 o C . add 1 mL of barium chloride TS. sparingly soluble in ethanol. congeal the diphenyl ether and filtrate into a 25-mL volumetric flask. direct titration). Packaging and Storage Preserve in tight containers. to 62.5 mol//L sodium hydroxide VS used in the test. Water Not more than 1. add exactly 20 mL of water.0 g of Polyethylene Glycol 1500 in 20 mL of water: the pH of the solution is between 4. combine the washing with the filtrate. add 1 mL of a solution of phosphomolybdic acid (1 in 10): a yellow-green precipitate is formed. Polyethylene Glycol 1500 is very soluble in water. in pyridine or in diphenyl ether. add 1 mL of barium chloride TS. (3) Ehtylene glycol and diethylene glycol⎯Place 50. Purity (1) Clarity and color of solution⎯A solution . Wash the residue with 5 mL of ice-cold water. characteristic odor. paraffin-like solid. represented by the formula [HOCH2(CH2OCH2)n CH2OH]. Transfer this solution to a stoppered flask. Purity (1) Clarity and color of solution⎯Dissolve 5. represented by the formula [HOCH2(CH2OCH2)nCH2OH]. To the distillate. Packaging and Storage Preserve in tight containers. add 75 mL of diphenyl ether.0% (2 g. pH Dissolve 1. Residue on Ignition Not more than 0. volumetric titration. Description Polyethylene Glycol 4000 is a white.20 mL of 0. in which the value of n ranges from 340 to 570. paraffin-like flake or powder. Average molecular mass under Polyethyleneglycol 400: average molecular mass is between 7300 and 9300. Pipet exactly 25 mL of this solution. Water Not more than 1. shake and filter. in petroleum benzine and in Polyethylene Glycol 400. dissolve with vigorous shaking and allow to stand for 16 hours or more. cool and add 0.0 g of Polyethylene Glycol 4000 in 20 mL of neutralized ethanol by warrning. pipet exactly 300 mL of freshly distilled pyridine into a 1000-mL light-resistant.0% (2 g. cool and add 0. represented by the formula [HOCH2(CH2OCH2)n CH2OH]. shake and filter.0 g of Polyethylene Glycol 6000 in 20 mL of neutralized ethanol by warming. represented by the formula [HOCH2 (CH2OCH2)n CH2OH].5 g of Polyethylene Glycol 6000. wrap it securely with strong cloth and perform the test. 5.5 and 7. is ordorless or has a faint. add 42 g of phthalic anhydride. direct titration). dissolve with vigorous shaking and allow to stand for 16 hours or more.5. direct titration).0 g of Polyethylene Glycol 6000 in 50 mL of water: the solution is clear and colorless. Average Molecular Mass Weigh accurately about 12. add 1 mL of barium chloride TS. Congealing point⎯Between 56 o C and 61 o C . stopper the bottle tightly. Packaging and Storage Preserve in well-closed containers. volumetric titration. Average molecular mass under Polyethyleneglycol 400: average molecular mass is between 2600 and 3800. in which the value of n ranges from 165 to 210. Average Molecular Mass Weigh accurately about 12.5.25% (1 g). transfer to the former stoppered pressure bottle. Residue on Ignition Not more than 0. To the filtrate add 1 mL of a solution of phosphomolybdic acid (1 in 10): a yellow-green precipitate is produced. transfer to an about 200-mL stoppered pressure bottle. Polyethylene Glycol 20000 is freely soluble in water and in pyridine and practically insoluble in methanol. volumetric titration. Description Polyethylene Glycol 6000 is a white. add about 25 mL of pyridine. stoppered bottle. transfer to the former stoppered pressure bottle. stopper the bottle tightly.KP VIII 1203 of 5. freely soluble in pyridine and practically insoluble in ethanol. Separately. paraffin-like solid. Congealing point⎯Between 56 o C and 64 o C . Purity (1) Clarity and color of solution⎯Dissolve Polyethylene Glycol 20000 is a polymer of ethylene oxide and water.1 mol/L sodium hydroxide VS and 1 drop of phenolphthalein TS: the color of the solution is red. (2) Acid⎯Dissolve 5. Identification Dissolve 50 mg of Polyethylene Glycol 20000 in 5 mL of dilute hydrochloric acid.0% (2 g. (2) Acid⎯Dissolve 5.5 g of Polyethylene Glycol 4000.5 and 7. Water Not more than 1. pH Dissolve 1. add 1 mL of barium chloride TS. dissolve by warming and allow to cool. characteristic odor. characteristic odor.2% (1 g). pipet exactly 300 mL of freshly distilled pyridine into a 1000-mL light-resistant. To the filtrate. add 42 g of phthalic anhydride. add 1 mL of a solution of phosphomolybdic acid (1 in 10): a yellow-green precipitate is produced. Separately.20 mL of 0. in anhydrous ether.1 mol/L sodium hydroxide VS and 1 drop of phenolphthalein TS: the color of the solution is red. Description Polyethylene Glycol 20000 is a white. dissolve by warming and allow to cool. Identification Dissolve 50 mg of Polyethylene Glycol 6000 in 5 mL of dilute hydrochloric acid. Pipet exactly 25 mL of this solution. is odorless or has a faint. Polyethylene Glycol 6000 is very soluble in water. . in ethanol. Polyethylene Glycol 6000 Polyethylene Glycol 20000 Macrogol 20000 Macrogol 6000 Polyethylene Glycol 6000 is a polymer of ethylene oxide and water. pH Dissolve 1.20 mL of 0. Residue on Ignition Not more than 0. transfer to an about 200-mL stoppered pressure bottle. wrap it securely with strong cloth and perform the test. if necessary. Packaging and Storage Preserve in well-closed containers. if necessary. in dehydrated ethanol or in ether.0 g of Polyethylene Glycol 4000 in 50 mL of water is clear and colorless.0 g of Polyethylene Glycol 20000 in 20 mL of water: the pH of this solution is between 4. add about 25 mL of pyridine.0 g of Polyethylene Glycol 6000 in 20 mL of water: the pH of this solution is between 4. flake or powder. stoppered bottle. dissolve with vigorous shaking and allow to stand for 16 hours or more.67 g of Polyoxyl 40 Stearate. shake . shake well. (3) Mix 6 mL of Polysorbate 80 with 4 mL of water at an ordinary temperature or the lower tempreature: a jelly-like mass is produced. dissolve by warming and allow to cool. in ethanol or in ether. Average Molecular Mass Weigh accurately about 15. Remove the bottle from the bath and allow to cool in air to room temperature. (3) Arsenic⎯Prepare the test solution with 0. add 5 mL of sodium hydroxide TS. cool and add 0. transfer to the former stoppered pressure bottle.5. Polysorbate 80 is miscible with methanol. (2) Acid⎯Dissolve 5. according to Method 3 and perform the test (not more than 3 ppm). add about 25 mL of pyridine.2% (1 g).0 g of Polyethylene Glycol 20000. (2) Heavy metals⎯Proceed with 2. Congealing Point of the Fatty Acid Not less than 53°C. with warm ethanol.0 g of Polyoxyl 40 Stearate according to Method 2 and perform the test.0 g of Polyoxyl 40 Stearate in 20 mL of water: the solution is clear and colorless. Pipet exactly 25 mL of this solution. (4) Take 10 mL of a solution of Polysorbate 80 (1 in 20). partially esterified with oleic acid. boil for 5 minutes.5 mol/L sodium hydroxide VS and 5 drops of a solution of phenolphthalein in pyridine (1 in 100). Packaging and Storage Preserve in tight containers. having a temperature of 98 ± 2 o C . Polyoxyl 40 Stearate Polyoxyl 40 Stearate is the monostearate of condensation polymers of ethylene oxide represented by the formula [H(OCH2CH2)nOOCC17H35]. Residue on Ignition Not more than 0. Part II Purity (1) Clarity and color of solution⎯Dissolve 5. Acid Value Not more than 1.0 g of Polyethylene Glycol 20000 in 50 mL of water: the solution is clear an colorless. viscous liquid. Polysorbate 80 Polysorbate 80 is a polyoxyethylene ether of anhydrous sorbitol. in which n is approximately 40. Averagemolecularmass Amount(g) of sample× 4000 = a−b a: Volume(mL) of 0.0% (2 g.0 mL of standard lead solution (not more than 10 ppm). stopper the bottle tightly. add 5 mL of chloroform.5 mol/L sodium hydroxide VS until a pale red color remains for not less than 15 seconds. Description Polysorbate 80 is a colorless or orangeyellow. Purity (1) Clarity and color of solution⎯Dissolve 1. direct titration). Polysorbate 80 is freely soluble in water and slightly soluble in ether.0°C. Perform a blank determination and make any necessary correction: average molecular mass is between 15000 and 25000.5 mol/L sodium hydroxide VS used in the blank determination.5 and 7. Packaging and Storage Preserve in well-closed containers.1% (1 g). add 5 mL of ammonium thiocyanate-cobaltous nitrate TS. Identification (1) Take 5 mL of a solution of Polysorbate 80 (1 in 20). Separately. Prepare the control solution with 2. cool and acidify with dilute hydrochloric acid: the solution is opalescent. transfer to an about 200 mL stoppered pressure bottle. wrap it securely with strong cloth and immerse in a water-bath. Congealing Point Between 39. Titrate with 0. add 42 g of phthalic anhydride. Residue on Ignition Not more than 0. to the same depth as the mixture in the bottle. pipet exactly 300 mL of freshly distilled pyridine into a 1000 mL light-resistant stoppered bottle.1204 Monographs.0 g of Polyethylene Glycol 20000 in 20 mL of neutralized ethanol by warming.20 mL of 0. Polyoxyl 40 Stearate is soluble in water. with ethanol. Water Not more than 1. Maintain the temperature of the bath at 98 ± 2 o C for 60 minutes.1 mol/L sodium hydroxide VS and 1 drop of phenolphthalein TS: the color of the solution is red. Add exactly 50 mL of 0. Saponification Value Between 25 and 35. pH⎯The pH of a solution of Polysorbate 80 (1 in 20) is between 5. having a faint.0°C and 44. Description Polyoxyl 40 Stearate is a white to pale yellow. (2) Take 5 mL of a solution of Polysorbate 80 (1 in 20) and add 2 to 3 drops of bromine TS: the color of the test solution is discharged. characteristic odor and a warm.5 mol/L sodium hydroxide VS used in the test. with pyridine and with chloroform. is odorless or has a faint fat-like odor. waxy solid or powder. slightly bitter taste. b : Volume(mL) of 0. volumetric titration. volumetric titration. Potassium Carbonate K2CO3: 138. previously dried and accurately weighed. Prepare the control solution as fol- Potassium Hydroxide KOH: 56.10 mg of K2CO3 Packaging and Storage Preserve in tight containers. Potassium Carbonate is very soluble in water and practically insoluble in ethanol. (3) Sodium⎯Dissolve 1. add 2 mL of dilute acetic acid and 2. (2) Arsenic⎯Prepare the test solution with 1. 25 o C ). in 25 mL of water.11 Potassium Hydroxide contains not less than 85.0% and not more than 101. contains not less than 99.5 mol/L sulfuric acid until the blue color of the solution changes to yellow-green. in small pellets. Loss on Drying Not more than 1. dilute with water to make 50 mL and perform the test. Assay Dissolve about 1. A solution of Potassium Carbonate (1 in 10) is alkaline.5 g of Potassium Carbonate.21 Potassium Carbonate. Potassium Hydroxide is hard and brittle and shows a crystalline fracture. 4 hours).0 g of Potassium Carbonate in 20 mL of water: the solution is clear and colorless. (2) Heavy metals⎯Dissolve 1. Viscosity Between 345 and 445 mm2/s (Method 1.0 g of Potassium Hydroxide in water and add water to make 100 mL. Potassium Hydroxide is freely soluble in water or in ethanol and practically insoluble in ether.0% (1 g. Potassium Hydroxide deliquesces in the presence of moisture. 180 o C . back titration).0 g of Polysorbate 80 according to Method 2 and perform the test. Description Potassium Carbonate is white granule or powder and odorless. Prepare the control solution with 2. Purity (1) Clarity and color of solution⎯Dissolve 1.5 g of Potassium Carbonate. Use chloroform instead of carbon tetrachloride and titrate without using an indicator.0 g of Potassium Carbonate in 2 mL of water and 6 mL of dilute hydrochloric acid and evaporate to dryness on a waterbath.0 mL of standard lead solution to dryness and dilute with water to make 50 mL (not more than 20 ppm).15% (2 g).0 g of Potassium Carbonate in 20 mL of water and perform the test as directed under the Flame Coloration Test (1): no persisting yellow color is produced. Purity (1) Clarity and color of solution⎯Dissolve 1.0 g of Potassium Hydroxide in 20 mL of water: the solution is clear and colorless. boil cautiously. To 25 mL of the solution. Description Potassium Hydroxide occurs as white fused masses. then cool and titrate until a greenish yellow color develops (indicator: 2 drops of bromocresol green TS). until the yellow color of iodine disappears.0% (3 g. Potassium Carbonate is hygroscopic. Prepare the control . Packaging and Storage Preserve in tight containers.095. (2) Chloride⎯Dissolve 2. Specific Gravity 20 : d 20 Between 1.KP VIII 1205 and allow to stand: a blue color develops in the chloroform layer. (4) Arsenic⎯Prepare the test solution with 0. Residue on Ignition Not more than 0.0.0% of K2CO3.0% of potassium hydroxide (KOH). Dissolve the residue in 35 mL of water and 2 mL of dilute acetic acid. Water Not more than 3.0 and not more than 101. Iodine Value Between 19 and 24. (2) A solution of Potassium Hydroxide (1 in 25) responds to the Qualitative Test for potassium salt. in flasks.065 and 1. Perform the test. Purity (1) Heavy metals⎯Proceed with 1. Identification A solution of Potassium Carbonate (1 in 10) responds to the Qualitative Tests for potassium salt and for carbonate. add 8 mL of dilute nitric acid and water to make 50 mL. titrate with 0. Each mL of 0.5 mol/L sulfuric acid = 69. lows: evaporate 6 mL of dilute hydrochloric acid on a water-bath to dryness. Potassium Hydroxide rapidly absorbs carbon dioxide in air. in sticks and in other forms. Acid Value Not more than 2. when dried. Identification (1) A solution of Potassium Hydroxide (1 in 500) is alkaline. Saponification Value Between 45 and 55. according to Method 1 and perform the test (not more than 4 ppm).0 g of Polysorbate 80 according to Method 3 and perform the test (not more than 2 ppm).0 mL of standard lead solution (not more than 20 ppm). 5 mol/L sulfuric acid consumed. Potato Starch.028%). previously dried.5 mol/L sulfuric acid consumed.0 g of Potassium Sulfate in 20 mL of water and perform the test as directed under the Flame Coloration Test (1): no persistent yellow color develops. preserved in a mixture of water and glycerin (1 : 1). (4) Sodium⎯Dissolve 0.21 × B Assay Weigh accurately about 1. Calculate the amount KOH from the amount.26 Potassium Sulfate. Identification (1) Under a microscope. Potato Starch is practically insoluble in water or in dehydrated ethanol.0 mL of hydrochloric acid and add gradually 8 mL of boiling barium chloride TS. then add 2 drops of methyl orange TS and titrate again with 0. Prepare the control solution as follows: evaporate 7 mL of dilute hydrochloric acid on a water-bath to dryness. Amount of potassium carbonate (mg) = 138. (3) Heavy metals⎯Proceed with 2. rarely 2. boil with 200 mL of water and 1.5 g of Potassium Sulfate.21) is not more than 2.40 mL of 0. contains not less than 99. (5) Arsenic⎯Prepare the test solution with 4. Heat the mixture on a water-bath for 1 hour. Prepare the control solution with 2. Prepare the control solution with 0. Description Potassium Sulfate is colorless crystals or a white. Amylum Solani Potato Starch consists of starch granules derived from the tuber of Solanum tuberosum Linné (Solanaceace).01 mol/L hydrochloric acid (not more than 0.7466 Packaging and Storage Preserve in well-closed containers. add 7 mL of dilute hydrochloric acid and evaporate on a water-bath to dryness. Description Potato Starch is a white powder. Each mL of 0. or spherical simple grains 10-35 µm in diameter. (2) Chloride⎯Perform the test with 0.11 mg of KOH Packaging and Storage Preserve in tight containers. Part II solution with 0. add 2 drops of phenolphthalein TS and titrate with 0. Loss on Drying Not more than 1. 110 o C .01 mol/L hydrochloric acid (not more than 0. 4 hours).10 g of Potassium Hydroxide in 10 mL of dilute hydrochloric acid and perform the test as directed under the Flame Coloration Test (1): no persistent yellow color develops.7 mL of 0. often more than 100 µm in diameter.0 g of potassium Sulfate in 20 mL of water: the solution is clear. crystalline powder. (4) Sodium⎯Dissolve 1.1206 Monographs. Record the amount A (mL) of 0. appears as unevenly ovoid or pyriform simple grains usually 30–100 µm. Dry.5 mol/L sulfuric acid until the solution changes to a persistent pale red color.5 g of Potassium Hydroxide and dissolve in 40 mL of freshly boiled and cooled water.to 4-compound grains.39). colorless and neutral.0 g of Potassium Sulfate according to Method 1 and perform the test (not more than 5 ppm).5 g of Potassium Sulfate. (5) Potassium carbonate⎯The amount of potassium carbonate (K2CO3: 138. A (mL) B (mL). Identification A solution of Potassium Sulfate (1 in 20) responds to the Qualitative Tests for potassium salt and for sulfate. collect the precipitate and wash the precipitate with water until the last washing shows no opalescence on the addition of silver nitrate TS.0 mL of standard lead solution (not more than 10 ppm). add water to make 50 mL and perform the test. Assay Weigh accurately about 0. dissolve the residue in 2 mL of dilute acetic acid and 3. 2 mL of dilute acetic acid and 1 drop of ammonia TS.0% of Potassium Sulfate (K2SO4).5 mol/L sulfuric acid = 56.0 g of Potassium Hydroxide in 5 mL of water. has a slightly saline and somewhat bitter taste. Record the amount B (mL) of 0.0% when calculated by the following equation using B (mL) obtained in the Assay.0% and not more than 101. ignite to constant weight between 500 o C and 600 o C by rising the temperature gradually and weigh as barium sulfate (BaSO4: 233.0 mL of standard lead solution and add water to make 50 mL (not more than 30 ppm). Dissolve the residue in 35 mL of water. Amount (mg) of Potassium Sulfate (K2SO4) = amount (mg) of barium sulfate (BaSO4) × 0. (3) Heavy metals⎯Dissolve 1. striation . Purity (1) Clarity and color of solution and acidity or alkality⎯Dissolve 1. spherical simple grains with non -centric or slightly eccentric hilum. Cool the solution to 15°C.0% (1 g.0 g of Potassium Sulfate according to Method 1 and perform the test. Potato Starch Potassium Sulfate K2SO4:174.050%). when dried. Potassium Sulfate is soluble in water and practically insoluble in ethanol.5 mol/L sulfuric acid until the red color of the solution disappears. 0 and 8. (3) Sulfur dioxide—(i) Apparatus Use apparatus shown in the figure. Perform a blank determination and make any necessary correction: the volume of 0. its intersection point on hilum. and use this solution as the control solution. pH Place 5. Transfer 10 mL each of these solutions into test tubes. and titrate with 0.0 g of potassium iodide. 130 90 minutes). Heat in a water-bath for 15 minutes. pour 80 mL of 2 mol/L hydrochloric acid TS into the funnel. close the tap of the funnel. Amount (ppm) of sulfur dioxide Amount (mL) of 0. (2) To 1 g of Potato Starch.5 to 1. add 0. open the tap to introduce the hydrochloric acid into the flask. and place 10 mL of hydrogen peroxide-sodium hydroxide TS in the test-tube.0. and use the filtrate as the test solution. and allow to cool: a subtle white-turbid. pasty liquid is formed. Add 1 mL of starch TS and titrate the solution with 0.6% (1 g). After 15 minutes. add water to make 20 mL each. Packaging and Storage Preserve in well-closed containers. and mix. add 50.1 mol/L sodium hydroxide VS until the color changes from yellow to violet-blue lasting for at least 20 seconds. Pass cooling water through the condenser.203 Loss on Drying Not more than 20. boil for 1 minute. remove the funnel without interrupting the stream of carbon dioxide. mix. in order to avoid losing sulfur dioxide. mix by shaking and allow to stand for . add 25. and introduce through the opening into the flask about 25 g of Potato Starch.05 mL of diluted iodine TS (1 in 10): an orange-red to deep blue color develops. mix by shaking for 5 minutes and centrifuge. allow to stand for 5 minutes and compare the color of these solutions against a white background: the color of the test solution is not darker than that of the control solution (not more than 10 ppm). calculated as hydrogen peroxide). Residue on Ignition Not more than 0.0 mL of standard iron solution. To 2.002 mol/L sodium thiosulfate VS until the color of the solution disappears. Make the each solution alkaline to litmus paper with strong ammonia water. add 1 mL of glacial acetic acid and 0.KP VIII 1207 distinct in all grains. Funnel C. add 2 mL each of a solution of citric acid (2 in 10) and 0.0% (1 g. 25 to 30 minutes in a dark place. Test tube (2) Oxidizing substances—To 4. mix gently for 1 minute to form a suspension. and the color disappears by heating. and heat the mixture for 1 hour. Perform a blank determination and make any necessary correction. add 15 mL of 2 mol/L hydrochloric acid TS.0 g of Potato Starch in a non -metal vessel. Purity (1) Iron—To 1. and close the tap while several mL of the hydrochloric acid remains. and connect the funnel. add 50 mL of water.0 mL of freshly boiled and cooled water. filter. (ii) Procedure Introduce 150 mL of water into the boiling flask. Boiling Flask B.0 mL of water. A. Place the flask in a water-bath.1 mL of bromophenol blue TS.5 g of Potato Starch. o C. Add 0.0 mL of the supernatant liquid. is observed when grains are put between two nicol prisms fixed at right angle to each other. add water to make 20 mL.0 g of Potato Starch. and cool. and pass carbon dioxide through the whole system at a rate of 100 ± 5 mL per minute. and mix. Condenser D.1 mL each of mercaptoacetic acid. (3) To 1 mL of the pasty liquid obtained in (2). a black cross.1 mol/L sodium hydroxide VS consumed = Amount (g) of Potato Starch taken × 1000 × 3. Transfer 10 mL each of the test solution and the control solution in test tubes. Apply tap grease to the outside of the connection part of the funnel. Calculate the amount of sulfur dioxide by applying the following formula: it is not more than 50 ppm. Close the tap of the funnel. with the aid of 100 mL of water.002 mol/L sodium thiosulfate VS consumed is not more than 1.4 mL (not more than 20 ppm. To 30. Transfer the contents of the testtube with the aid of a little water to a wide-necked conical flask. and allow to stand for 15 minutes: the pH of this solution is between 5. accurately weighed. 05 mL of aldehyde dehydrogenase solution to each of the cells. as directed in the potassium bromide.2 . allow to cool to room temperature and use this solution as the test solution. Operating conditions Detector: An ultraviolet absorption photometer (detection wavelength: 254 nm). Determine the absorbances. Determine the absorbances. Content (ppm) of aldehydes ( A − AT1 ) − ( AB2 − AB1 ) 1000 = T2 × W ( AS2 − AS1 ) − ( AB2 − AB1 ) W : Weighed amount (g) of povidone.5 mL of 0. dissolve 50 mg of 1-vinyl-2pyrrolidone in methanol to make exactly 100 mL. calculated on the anhydrous basis.0 and 0.0 mL of this solution and add methanol to make exactly 100 mL.10 g of freshly distilled acetaldehyde in water previously cooled to 4 o C to make exactly 100 mL. previously dried at 105 o C for 6 hours. (2) Heavy metals⎯Proceed with 2.0 for Povidone having the nominal K-value of 30 or less and between 4.0 mL of this solution. AT and AS of 1-vinyl-2pyrrolidone for the test solution and the standard solution. dissolve 0. Allow to stand at 4 o C for about 20 hours. pH 9. disk method under the Infrared Spectrophotometry: both spectra exhibit similar intensities of absorption at the same wavenumbers.vinyl .05 mol/L pyrophosphate buffer solution. respectively: the content of 1-vinyl-2pyrrolidone is not more than 10 ppm. Povidone contains not less than 11.0 mL of standard lead solution (not more than 10 ppm). Povidone is hygroscopic. Stopper. Separately.5% and not more than 12.0 for Povidone having the nominal K-value exceeding 30. the standard solution and water at 340 nm.0 g of Povidone and dissolve in 0. to make exactly 100 mL. calculated on the anhydrous basis.0. The nominal K-value is shown on the label. respectively.25 g of Povidone. add diluted methanol (1 in 5) to make exactly 100 mL and use this solution as the standard solution. (3) Aldehydes⎯Weigh accurately about 1. transfer to separate cells. AS2 and AB2 of aldehyde of these solutions in the same manner as above: the content of aldehydes is not more than 500 ppm expressed as acetaldehyde.1208 Monographs. AS2 and AB1 of the subsequent solution of the test solution. Separately. slightly soluble in acetone and practically insoluble in ether. to make exactly 100 mL and use this solution as the standard solution. (4) 1-Vinyl-2-pyrrolidone⎯Weigh accurately about 0. Purity (1) Clarity and color of solution ⎯Dissolve 1. calculated on the anhydrous basis.5 cm in length and about 4 . or pale red. Povidone is freely soluble in water. mix and stopper tightly.0 g of Povidone in 20 mL of water: the solution is clear and colorless to pale yellow. AT1 .0 g of Povidone according to Method 2 and perform the test.2 mL of β-nicotinamide adenine dinucleotide TS to each of these cells. pH Dissolve 1.0. is odorless or has a faint. pipet 1. the standard solution and water (for blank test). Part II Povidone CHCH2 N O n Polyvidone Polyvinylpyrrolidone (C6H9NO)n Povidone is a chain polymer of 1-vinyl-2-pyrrolidone. Identification Determine the infrared spectra of Povidone and Povidone RS. AT2 . pH 9.0 g of Povidone in 20 mL of water: the pH of this solution is between 3. Povidone has a nominal K-value of not less than 25 and not more than 90. mix and stopper tightly.05 mol/L pyrophosphate buffer solution. add 0. Perform the test with 50 μL each of the test solution and the standard solution as directed under the Liquid Chromatography according to the following operating conditions and determine the peak areas. heat at 60 o C for 60 minutes. dissolve in diluted methanol (1 in 5) to make exactly 10 mL and use this solution as the test solution.0 and 5.8% of nitrogen (N: 14.01). Description Povidone is a white to slightly yellowish fine powder. in methanol or in ethanol.pyrrolidon e A 2 . Pipet 5.3 mol/L pyrophosphate buffer solution. Measure 0.0 mL of this solution.0 and 7. Pipet 1.5 mL each of the test solution. Allow to stand for 5 minutes at 22 ± 2 o C . add 2. Add 0.5 = T × AS W W : Weighed amount (g) of povidone. pH 9. Allow stand for 2 to 3 minutes at 22 ± 2 o C and perform the test with these solution as directed under the Ultraviolet-visible Spectrophotometry using water as the control solution. Prepare the control solution with 2. characteristic odor. Column: Stainless steel columns. Content (ppm) of 1 . about 4 mm in inside diameter and about 2. Spot 10 μL each of the test solution and the standard solution on a plate coated with dimethylsilanzed silica gel with fluorescent indicator for thin-layer chromatography. To 25 mL of the test solution.5 log η rel − 1 + 0. stopper tightly.5 g. Perform the test with the test solution and the standard solution as directed under the Thin-layer Chromatography. Separately.3 and the fluorescence of the spot from the test solution corresponding to the spot from the standard solution is not more intense than that of the spot from the standard solution (not more than 1 ppm). Develop the plate with diluted methanol (2 in 3) to a distance of about 15 cm and air-dry the plate. Allow to stand for 30 minutes and perform the test with this solution as directed under the Ultraviolet-visible Spectrophotometry. Perform the test with the test solution and water at 25 o C as directed in Method 1 under the Viscosity Determination and calculate the K-value by the following formula: the K-value of Povidone is not less than 90.KP VIII 1209 mm in inside diameter and about 25 cm in length. 1 g of cupric sulfate and 1 g of titanium dioxide and wash down any adhering sample from the neck of the flask with a small amount of water. Allow to cool. 3 drops of bromocresol green-methyl red TS and sufficient water to immerse the lower end of the condenser tube. volumetric titration. Washing of the guard column: After each test with the test solution. (6) Hydrazine⎯Transfer 2.003c 2 c : Mass (g) of Povidone in 100 mL of the solution. allow to stand for 60 minutes and use this solution as the test solution. Heat the flask on an asbestos wire gauze over a free flame until the solution has a clear. Add 500 μL of a solution of salicyladehyde in methanol (1 in 20). immediately close the clamp attached to the rubber tube. yellow-green color and the inside wall of the flask is free from a carbonaceous material and then heat for further 45 minutes. System suitability System performance: Dissolve 10 mg of 1-vinyl2-pyrrolidone and 0. Column temperature: A constant temperature of about 40 o C . Examine under ultraviolet light (main wavelength: 365 nm): the Rf value of the fluorescent spot from the standard solution is about 0. Water Not more than 5. Residue on Ignition Not more than 0. η rel : Kinematic viscosity of the test solution relative to that of water.0% (0.5 g of vinyl acetate in 100 mL of methanol.0. Add 5 g of a powdered mixture of 33 g of potassium sulfate. dissolve in water to make exactly 100 mL and use this solution as the test solution.0 g calculated on the anhydrous basis. respectively.0% and not more than 108. Use a column giving elution of 1-vinyl-2-pyrrolidone and vinyl acetate in this order with the resolution between their peaks being not less than 2. Assay Weigh accurately about 0. K= 300c log η rel + (c + 1.00 g calculated on the anhydrous basis and dissolve in water to make exactly 100 mL. using a solution prepared by adding 2 mL of 13% sulfuric acid to 25 mL of the test solution at 405 nm is not more than 0. Add 7 mL of sulfuric acid allowing to flow down the inside wall of the flask.0% of the nominal Kvalue. add cautiously 20 mL of water.35 (not more than 400 ppm. centrifuge and use the upper layer of the mixture as the test solution. Add 30 mL of a solution of sodium hydroxide (2 in 5) through the funnel. cool the solution and connect the flask to the distillation apparatus previously washed by passing steam through it.1% (1 g) K-Value Weigh accurately an amount of Povidone. the relative standard deviation of obtained peak areas of 1-vinyl-2-pyrrolidone is not more than 2. System reproducibility: When the test is repeated 6 times with the standard solution under the above operating conditions. To 1 mL of this solution. shake vigorously for 2 minutes. After cooling. Mobile phase: A mixture of water and methanol (4 : 1). equivalent to 1. dissolve 90 mg of salicylaldazine in toluene to make exactly 100 mL. wash away the polymeric material of Povidone from the guard column by passing the mobile phase through the column backwards for about 30 minutes at the same flow rate as applied in the test. add 2 mL of titanium trichloride-sulfuric acid TS and mix.0%.0 mL of toluene.003c 0. Proceed with 50 μL of this solution according to the above operating conditions and calculate the resolution. add diluted methanol (1 in 5) to make 100 mL. Detection sensitivity: Adjust the detection sensitivity so that the peak height of 1-vinyl-2-pyrrolidone obtained from 50 μL of the standard solution is between 10 mm and 15 mm. Pipet exactly 1 mL of this solution. stir and warm at 60 o C for 15 minutes in a water-bath. rinse cautiously the funnel with 10 mL of water. equivalent to 4. add toluene to make exactly 100 mL and use this solution as the standard solution. expressed as hydrogen peroxide).5 g of Povidone to a 50mL centrifuge tube.15c + 0.1 g of Povidone and place in a Kjeldahl flask. (5) Peroxides⎯Weigh exactly an amount of Povidone.5c log η rel ) 2 1. packed with octylsilanized silica gel for liquid chromatography (5 μm in particle diameter) and use them as a guard column and a separation column. calculated on the anhydrous basis. add 25 mL of water and stir to dissolve. direct titration).15 + 0. Flow rate: Adjust the flow rate so that the retention time of 1-vinyl-2-pyrrolidone is about 10 minutes. add 30 mL of a solution of boric acid (1 in 25). To the absorption flask. then start the distillation with . add 2. Purity (1) Acid⎯Mix 10. Specific Gravity 20 : d 20 Between 1. add 1 mL of pyridine and heat under a reflux condenser on a water-bath for 1 hour.2 mL of sulfuric acid and heat strongly with care to constant weight: the residue is not more than 0. Part II steam to get 80 mL to 100 mL of the distillate. direct titration). previously dried at 80 o C for 2 hours.025 mol/L sulfuric acid until the color of the solution changes from green through pale grayish blue to pale grayish red-purple.0 g of Propylene Glycol with 0. previously dried at 80 o C for 2 hours. moisten the residue with 0.002%).025 mol/L sulfuric acid = 0. volumetric titration.0 g of Propylene Glycol.0 g of Pyroxylin.0 g of Propylene Glycol according to Method 1 and perform the test. Distilling Range less than 95 vol% Between 184 o C and 189 o C . not Packaging and Storage Preserve in tight containers. with methanol. Cool. with ethanol and with pyridine. Purity (1) Clarity of solution⎯Dissolve 1. Propylene Glycol is hygroscopic. shake with 20 mg of activated charcoal and filter. Pyroxylin Pyroxylin is a nitric acid ester of cellulose. in 25 mL of a mixture of ether and ethanol (3 : 1): the solution is clear. (6) Glycerin⎯Heat 1. Pyroxylin is usually moistened with isopropanol or some appropriate solvent. Residue on Ignition Weigh accurately about 20 g of Propylene Glycol in a weighed crucible and heat to boiling.7 g of triphenylchloromethane.5 g of potassium bisulfate: a characteristic odor is evolved.5 mg.1210 Monographs.09 Description Propylene Glycol is a clear.005 mol/L sulfuric acid (not more than 0. (2) Acid⎯Shake 1. Water Not more than 0. Perform a blank determination and make any necessary correction.007%) (3) Sulfate⎯Perform the test with 10. colorless.5 mL of standard lead solution (not more than 5 ppm).0 g of Propylene Glycol. After cooling. Each mL of 0.5 g of potassium bisulfate and evaporate to dryness: no odor of acrolein is perceptible. Prepare the control solution with 0. (4) Residue on ignition⎯Weigh accurately about 2 g of Pyroxylin. (3) Water-soluble substances⎯Evaporate 10 mL of the filtrate obtained in (2) on a water-bath to dryness and dry at 105 o C for 1 hour: the residue is not more than 1. previously dried at 80 o C for 2 hours and moisten with 10 mL of a solution of castor oil in acetone (1 in 20) to gelatinize the test sample. Identification (1) Mix 2 to 3 drops of Propylene Glycol with 0. Remove the absorption flask from the lower end of the condenser tube.040. Pyroxylin is decomposed with the evolution of nitrous acid vapors.0 g of Propylene Glycol according to Method 1 and perform the test (not more than 2 ppm).1 mol/L sodium hydroxide VS: the solution has a red color. is odorless and has a slightly bitter taste. Stop heating and immediately ignite to burn. dissolve the mixture in 20 mL of acetone by warming. Identification Ignite Pyroxylin: it burns very rapidly with a luminous flame. Propylene Glycol OH CH3CCH2OH and enantiomer H C3H8O2: 76.0 g of Pyroxylin.5% (2 g. with 20 mL of water for 10 minutes: the filtrate is neutral.035 and 1. viscous liquid.40 mL of 0. rinsing the end part with a small quantity of water and titrate the distillate with 0. Collect the separated crystals and dry in a desiccator (silica gel) for 4 hours: the crystals melt between 174 o C and 178 o C . (4) Heavy metals⎯ Prepare the test solution with 5. Prepare the control solution with 0. (2) Chloride⎯Perform the test with 2. Propylene Glycol is freely soluble in ether. (2) Heat gently 1 mL of Propylene Glycol with 0.30 mL of 0. (5) Arsenic⎯Prepare the test solution with 1. Upon heating or exposure to light. Propylene Glycol is miscible with water.005%. Pyroxylin is freely soluble in acetone and very slightly soluble in ether.0 mL of Propylene Glycol with 50 mL of freshly boiled and cooled water and add 5 drops of phenolphthalein TS and 0. Concentrate the filtrate to about 10 mL and cool.40 mL of 0. Prepare the control solution with 2. Ignite .7003 mg of N Packaging and Storage Preserve in tight containers.01 mol/L hydrochloric acid (not more than 0. Description Pyroxylin is a white cotton-like substance or flake-like substance. Saponification Value Between 169 and 195. These simple grains often gather in ellipsoidal. add water to make 1 mL. and use this solution as the control solution. slightly viscous oil. neutral and . For Sterile Water for Injection. Rape Seed Oil Rape Seed Oil is the fixed oil obtained from the seed of Brassica campestris Linné subsp. boil. in size. Sterile Water for Injection is used mainly as solvent for injections to be reconstituted or suspended before use. Rape Seed Oil is miscible with ether. Rice Starch is practically insoluble in water or in ethanol.13 mL of 0.25 EU per mL. tight containers packed loosely.KP VIII 1211 the contents to carbonize the test sample. When Sterile Water for Injection is prepared by the distillation and packed in containers may be labeled as Distilled Water for Injection as a commonly used name. Bacterial Endotoxins Less than 0. (6) Ammonium⎯Perform the test as directed under the Ammonium Limit Test. (2) Chloride⎯For Sterile Water for Injection in containers holding a volume not more than 10 mL. (6) Ammonium and (9) Residue on evaporation. Under a microscope. For Sterile Water for Injection in containers holding a volume exceeding 10 mL. Plastic containers for aqueous infusions may be used. with chloroform or with petroleum benzine. add 3 drops of nitric acid and 0. odorless and tasteless.01 mol/L sodium hydroxide VS and allow to stand for 30 seconds: a red color develops. Description Rape Seed Oil is clear. add proceed in the same manner as the test solution (not more than 0. remote from fire and preferably in a cold place.00005%).0 mL of dilute nitric acid.5%.2. compound grains.13 mL of 0. (2) Chloride. Unsaponifiable Matters Not more than 1. Mix the test solution and the control solution separately with 0. Packaging and Storage Preserve in tight containers.0 mg for that exceeding 10 mL. add purified water for ammonium limit test to make 30 mL. pale yellow. ignite at about 500 o C for 2 hours and allow to cool in a dessicator (silica gel): the residue is not more than 0. 3 μm to 10 μm. mostly 4 μm to 6 μm. allow to stand for 5 minutes under the protection from sunlight and compare the turbidity of the solutions on a black background: the turbidity of the test solution is not thicker than that of the control solution (not more than 0. napus Hooker fil. Identification (1) To 1 g of Rice Starch add 50 mL of water. to 0.20 mL of 0. is odorless or has slight odor and mild taste. using 30 mL of Sterile Water for Injection as the test solution. Description Rice Starch is a white mass or powder. Rape Seed Oil is slightly soluble in ethanol. Hilum and striation are not observable. Rice Starch appears as polyhedral.906 and 0. Rice Starch Rice Starch consists of the starch granules obtained from the seeds of Oryza sativa Linné (Gramineae). Packaging and Storage Preserve in light-resistant.5 mL of silver nitrate TS to 50 mL of Sterile Water for Injection: the solution remains unchanged.0 mg for Distilled Water for Injection in a volume not more than 10 mL and not more than 3. Acid Value Not more than 0. Shake gently 20 mL of Sterile Water for Injection with 0.0 mL of dilute nitric acid to 15 mL of Sterile Water for Injection and use this solution as the test solution.05 mL of bromothymol blue TS and 0.30 mL each of silver nitrate TS.30%. 25 Specific gravity— d 25 : Between 0.6 mL of standard ammonium solution for Sterile Water for Injection in containers holding a volume exceeding 10 mL. Sterile Water for Injection Sterile Water for Injection is prepared by the sterilization of Water for Injection preserved in containers.001 mol/L hydrochloric acid. simple grains.05 mL of phenol red TS and 0. and allow to cool: a turbid. Separately. (1) Acid or alkali⎯Take gently 20 mL of Sterile Water for Injection with 0. Purity Proceed as directed in the Purity test under Purified Water. 50 μm to 100 μm in diameter. et Anderson var. perform the test according to the following Methods (1).920. Iodine Value Between 95 and 127. (2). (9) Residue on evaporation⎯Evaporate 100 mL of Sterile Water for Injection and dry the residue at 105 o C for 1 hour: the residue is not more than 4. (6) and (9) for (1) Acid or Alkali. add 2. then add 2.01 mol/L hydrochloric acid and allow to stand for 30 seconds: a yellow color develops.2 mg/L for Sterile Water for Injection in a volume not more than 10 mL and not more than 0.1 mg/mL for that Sterility Test It meets the requirement. exceeding 10 mL). Prepare the control solution as follows: to 0. nippo-oleifera Makino (Cruciferae). Packaging and Storage Preserve in Hermetic containers. 7 mL of dilute hydrochloric acid.0 g of Saccharin Sodium Hydrate in 40 mL of water. Rosin is freely soluble in ethanol. dissolve 0. Ash Not more than 0.1 mol/L sodium hydroxide VS to the solution: the color changes to red. and has intensely sweet taste.0% and not more than 101. from which essential oils have been removed. Identification (1) Determine the infrared spectra of Saccharin Sodium Hydrate and Saccharin Sodium Hydrate RS as directed in the potassium bromide disk method under the Infrared Spectrophotometry: Both spectra exhibit similar intensities of absorption at the same wavenumbers.0%. of the peak height of orthotoluene sulfonamide to that of the internal standard for the test solution and the standard . dehydrate with 5 g of anhydrous sodium sulfate and evaporate the ethyl acetate. contains not less than 98.0 mL of the standard lead solution.0 g of Saccharin Sodium Hydrate in 10 mL of water and add 1 drop of phenolphthalein TS: the solution is colorless.10 g of orthotoluene sulfonamide in ethyl acetate to make exactly 100 mL. dissolve the residue in 5. Saccharin Sodium Hydrate effloresces slowly and loses about half the amount of water of crystallization in air. Loss on Drying Not more than 15.0 mL of the internal standard solution and use this solution as the standard solution. (2) Acid or alkali⎯Dissolve 1. Perform the test with 1 µL each of the test solution and the standard solution as directed under the Gas Chromatography according to the following operating conditions and calculate the ratios. It may contain a minute quantity. Rosin has a slight odor. QT and QS. Description Rosin is a pale yellow to pale brown. Saccharin Sodium Hydrate O NNa 2 H2O SO2 C7H4NNaO3S·2H2O: 241. Ash Not more than 1.1212 Monographs. Allow the solution to stand for 1 hour after the beginning of crystallization and then filter through dry filter paper.1%.0% (6 hours).17). dilute with water to make 50 mL and rub the inner wall of the vessel with a glass rod until crystallization begins. Purity (1) Clarity and color of solution⎯Dissolve 1. crystalline powder. brittle mass and its surface is often covered with a yellow powder. even in 10000 dilutions.20 Saccharin Sodium Hydrate. wash with 30 mL of a solution of sodium chloride (1 in 4). A solution of Rosin in ethanol is acidic. Rosin melts easily and burns with a yellow-brown flame. if any. Combine all the ethyl acetate extracts. (6) Orthotoluene sulfonamide⎯Dissolve 10 g of Saccharin Sodium Hydrate in 50 mL of water and extract three times with 30 mL volumes of ethyl acetate. (2) To a portion of Rice Starch add iodine TS: a dark blue-purple color is produced.0 g of Saccharin Sodium Hydrate. (5) Benzoate and salicylate⎯Dissolve 0. Purity Foreign matter⎯Under a microscope. Separately. (3) Heavy metals⎯Dissolve 2.0 mL of this solution. Add 2 mL of dilute acetic acid and water to make 50 mL and perform the test.5 mL of water or in 50 mL of ethanol: the solution is clear and colorless. Rice starch does not contain starch grains of any other origin. Dissolve the residue in 5. of fragments of the tissue of the original plant. Part II pasty liquid is formed. Add 1 drop of 0. in glacial acetic acid or in ether. Prepare the control solution as follows: to 2. add 5 drops of acetic acid and 3 drops of ferric chloride TS: no turbidity is produced and no red-purple to purple color develops. according to Method 1 and perform the test (not more than 2 ppm). Rosin Rosin is the resin obtained from the exudation of plants of Pinus species (Pinaceae).5 g of Saccharin Sodium Hydrate in 10 mL of water. Discard the first 10 mL of the filtrate and take 25 mL of the subsequent filtrate. when dried. Pipet 1. add 0. sparingly soluble in ethanol and practically insoluble in ether.0% of saccharin sodium (C7H4NNaO3S: 205. glassily transparent. add 2 mL of dilute acetic acid and water to make 50 mL and use this solution as the control solution (not more than 20 ppm).0 mL of the internal standard solution and use this solution as the test solution. Saccharin Sodium Hydrate is freely soluble in water. Description Saccharin Sodium Hydrate is colorless crystal or a white.0 g of Saccharin Sodium Hydrate in 1. evaporate on a water-bath to dryness. Acid Value Between 150 and 177. (4) Arsenic⎯Prepare the test solution with 1. The fractured surface is shell-like and lustrous. (4) A solution of Saccharin Sodium Hydrate (1 in 10) responds to the Qualitative Tests for sodium salt. heat slightly if necessary. coated with diethyleneglycol polyester for gas chromatography succinate at the ratio of 3%. and make any necessary correction. Description White Shellac is a yellowish white to pale yellow. White Shellac White Shellac is a resin-like substance obtained from a bleached secretion of Laccifer lacca Kerr (Coccidae). add 50 mL of neutralized ethanol as a solvent and dissolve by warming. Sesame Oil is miscible with ether.2. 120 °C. Internal standard solution⎯A solution of caffeine in ethyl acetate (1 in 500).0%.1 mol/L perchloric acid VS = 20. 4 hours).5 g of White Shellac. Unsaponifiable Matters Not more than 2. add 40 mL of water and cool. System suitability System performance: When the procedure is run with 1 μL of the standard solution according to the above operating conditions. Allow the solution to stand between 48°C and 50°C for 10 minutes: the solution is not more intense than Color Matching Fluid A. Flow rate: Adjust the flow rate so that the retention time of caffeine is about 6 minutes. characteristic odor.914 and 0. Description Sesame Oil is clear. Sesame Oil congeals between 0 o C and -5 o C . and titrate with 0. Packaging and Storage Preserve in tight containers.921.0. Add 12 mL of dilute nitric ac- . Specific Gravity 25 : Between 0. Water Not more than 15. packed with siliceous earth for gas chromatography (180 μm to 250 μm in diameter). with chloroform. Injection port temperature: A constant temperature of about 250 °C.40 g of White Shellac in 5 mL of ethanol while warming. Congealing point of the fatty acids⎯between o 20 C and 25 o C . odorless or has a faint. Acid Value Between 65 and 90. Weigh accurately about 0. Assay Weigh accurately about 0.20 g of Saccharin Sodium Hydrate.1 mol/L perchloric acid VS (potentiometric titration. respectively: QT is not more than QS. direct titration).0% (0.52 mg of C7H4NNaO3S Packaging and Storage Preserve in well-closed containers.0% (1 g. volumetric titration. brittle granule and is odorless or has faint.1 g of sucrose and 10 mL of hydrochloric acid and shake for 30 seconds: the acid layer becomes pale red and changes to red on standing. Column temperature: A constant temperature of about 200 °C.5 g of Saccharin Sodium Hydrate. White Shellac dissolves in sodium hydroxide TS. (7) Readily carbonizable substances⎯Perform the test with 0.KP VIII 1213 solution.1 g. Carrier gas: Nitrogen. d 25 Acid Value Not more than 0. add 0. the internal standard and orthotoluene sulfonamide are eluted in this order with a resolution between their peaks being not less than 2. Column: A column. White Shellac is sparingly soluble in ethanol. Identification Take 1 mL of Sesame Oil. System repeatability: When the test is repeated 6 times with 1 μL of the standard solution according to the above operating conditions. After cooling. Purity (1) Chloride⎯Shake and dissolve 0. Sesame Oil Oleum Sesami Sesame Oil is the fixed oil obtained from seeds of Sesamum indicum Linné (Pedaliaceae). Saponification Value Between 187 and 194. perform the test. Operating conditions Detector: A hydrogen flame-ionization detector. very slightly soluble in petroleum ether and practically insoluble in water. about 3 mm in inside diameter and about 1 m in length. Endpoint Detection Method in Titrimetry). Each mL of 0.0%. with petroleum ether or with carbon disulfide. pale yellow oil. hard. Sesame Oil is slightly soluble in ethanol. the relative standard deviation of the ratio of the peak height of orthotoluene sulfonamide to that of the internal standard is not more than 2. Perform a blank determination. characteristic odor and has bland taste. Iodine Value Between 103 and 118. Loss on Drying Not more than 15. dissolve in 50 mL of glacial acetic acid. brittle scutella. Loss on Drying Not more than 6. transfer to a beaker and dry at 65°C until the water is almost evaporated. titrate with 0. characteristic odor. (2) Sulfate⎯Shake and dissolve 0. (4) Rosin⎯Dissolve 2. (6) Rosin⎯Proceed as directed in the Purity (4) under Purified Shellac. Packaging and Storage Preserve in well-closed containers. Prepare the control solution as follows: to 0. 1 mL of dilute hydrochloric acid and water to make 50 mL (not more than 0.0% (1 g. Loss on Drying Not more than 2. Ash Not more than 1. (4) Arsenic⎯Proceed as directed in the Purity (2) under Purified Shellac.1 mol/L potassium hydroxide VS (potentiometric titration). Dissolve the wax remaining in the beaker with a suitable quantity of chloroform by warming.0 g of Purified Shellac in 150 mL of a solution of sodium carbonate (9 in 200) with shaking on a water-bath and continue the heating for 2 hours. then for 15 hours in a desiccator (calcium chloride for drying). Purified Shellac Purified Shellac is a resin-like substance obtained from a purified secretion of Laccifer lacca Kerr (Coccidae). Packaging and Storage containers. add gradually 50 mL of petroleum ether while shaking and filter. previously dried at 105°C for 2 hours. (3) Ethanol-insoluble substances⎯Dissolve about 5 g of Purified Shellac.140%). Prepare the control solution with 2.01 mol/L hydrochloric acid VS. hard. Use a cylindrical weighing bottle for taring the extraction thimble.0%. Store in cold place. Prepare the control solution as follows: to 0. add 2. Pour the solution into the thimble and extract with chloroform for 2 hours. (7) Wax⎯Proceed as directed in the Purity (5) under Purified Shellac. proceed as directed in the Ash under the Crude Drugs Test). (5) Ethanol-insoluble substances⎯Proceed as directed in the Purity (3) under Purified Shellac. then add 1. in 50 mL of ethanol on a water-bath while shaking. Immediately cover both depressions with a watch glass and allow to stand: the solution of the residue exhibits no purple or blue color within 1 minute. Perform the test using 50 mL of the filtrate as the test solution. lustrous. Weigh accurately about 1 g of medium powder of Purified Shellac and dry at 40°C for 4 hours. Perform the test using 50 mL of the filtrate as the test solution. Description Purified Shellac is a pale yellow-brown to brown. (5) Wax⎯Dissolve 10. Purified Shellac is freely soluble in ethanol or in dehydrated ethanol and practically insoluble in water or in ether.1214 Monographs. Wash the solution twice with 50 mL volumes of water.0 g of Purified Shellac in 10 mL of dehydrated ethanol with thorough shaking. then for 15 hours in a desiccator (calcium chloride for drying).005 mol/L sulfuric acid. add 40 mL of neutralized ethanol and dissolve by warming. add 2. (2) Arsenic⎯Prepare the test solution with 0. if necessary.0%. Dissolve the residue in 2 mL of a mixture of carbon tetrachloride and phenol (2 : 1). Ash Not more than 1. Weigh accurately about 1 g of medium powder of White Shellac and dry at 40°C for 4 hours.45 mL of 0. and has no odor or has a faint. Purified Shellac dissolves in sodium hydroxide TS. (3) Heavy metals⎯Proceed as directed in the Purity (1) under Purified Shellac.0 mL of standard lead solution (not more than 10 ppm).40 g of Purified Shellac according to Method 3 and perform the test. Evaporate the chloroform solution to dryness and dry the residue at 105°C for 3 hours: the residue is not more than 20 mg. Add 2 mL of dilute hydrochloric acid and water to make 100 mL and filter. collect the floating wax by filtration.0 g of Purified Shellac according to Method 2 and perform the test. wash the wax and the filter paper with water. Purity (1) Heavy metals⎯Proceed with 2.0%. 6 mL of dilute nitric acid and water to make 50 mL (not more than 0. Pour the ethanol solution into a tared extraction thimble. Preserve in well-closed . add 40 mL of water and cool. Part II id and water to make 100 mL and filter.40 g of White Shellac in 5 mL of ethanol by warming. Weigh accurately about 1 g of Purified Shellac. proceed as directed in the Ash under the Crude Drugs Test).5 mL of strong hydrogen peroxide water and fire to burn (not more than 5 ppm). filter the upper layer and evaporate the filtrate on a water-bath to dryness.5 mL of ethanol. After cooling. transfer the solution to a depression of a spot plate and fill the neighboring depression with a mixture of carbon tetrachloride and bromine (4 : 1).0% (1 g. Add 10 mL of an ethanol solution of magnesium nitrate (1 in 50). Transfer the wax together with the filter paper to an extraction thimble in a Soxhlet extractor. Acid Value Between 60 and 80. accurately weighed. After cooling.80 mL of 0.5 mL of ethanol. in a Soxhlet extractor and extract with ethanol for 3 hours: the residue is not more than 2.110%). 01 mol/L hydrochloric acid VS (not more than 0. contains not less than 99. add 5 mL of dilute sulfuric acid. Each mL of 0. calculated on the anhydrous basis. dry air. When cooled to 10 °C.35 mL of 0.5% and not more than 101. Sodium Carbonate Hydrate is freely soluble in water and practically insoluble in ethanol or in ether. previously dried. (5) Heavy metals⎯Proceed with 2.0% of sodium acetate (C2H3NaO2: 82.1 mol/L perchloric acid until the color of the solution changes from yellow to green (indicator: 1 mL of αnaphtholbenzeine TS).0 g of Sodium Acetate Hydrate in 100 mL of water. Prepare the control solution with 0.0 mL of 0. (7) Arsenic⎯Prepare the test solution with 1.03).KP VIII 1215 Sodium Acetate Hydrate CH 3 COONa 3 H 2O C2H3NaO2·3H2O: 136.2 g of Sodium Acetate Hydrate. Identification A solution of Sodium Carbonate Hydrate (1 in 20) responds to the Qualitative Tests for sodium salt and for carbonate.0 g of Sodium Carbonate Hydrate in 5 mL of water: the solution is clear and colorless (2) Chloride⎯Dissolve 0. A solution of Sodium Carbonate Hydrate (1 in 10) is alkaline.011%).0 mL of standard lead solution (not more than 10 ppm). the red color disappears. Prepare the control solution with 2.14 Sodium Carbonate Hydrate contains not less than 99. boil. dissolve in 50 mL of glacial acetic acid and titrate with 0.0 g of Sodium Acetate Hydrate. Sodium Acetate Hydrate is very soluble in water. Prepare the control solution with 1.1 g of methylthymol blue-potassium nitrate indicator): the amount of 0. when dried. add 6 g of ammonium chloride. add 0.0 g of Sodium Acetate Hydrate according to Method 1 and perform the test. (4) Sulfate⎯Perform the test with 1.0 g of Sodium Acetate Hydrate in 20 mL of water: the solution is clear and colorless. according to Method 1 and perform the test (not more than 2 ppm). odorless or has a slight. Sodium Carbonate Hydrate Na2CO3·10H2O: 286. Loss on Drying Not less than 39.203 mg of C2H3NaO2 Identification A solution of Sodium Acetate Hydrate (1 in 10) responds to the Qualitative Tests for acetate and sodium salt.071%).0% and not more than 103.005 mol/L sulfuric acid VS (not more than 0.01 mol/L disodium ethylenediamine tetraacetate VS consumed is not more than 0. (3) Chloride⎯Perform the test with 1. Description Sodium Carbonate Hydrate is colorless or white crystal.0 g of Sodium Acetate Hydrate in 20 mL of freshly boiled and cooled water and add 3 drops of phenolphthalein TS: a red color develops. freely soluble in glacial acetic acid. (3) Heavy metals⎯Dissolve 2. Assay Weigh accurately about 0. saline and slight bitter taste. Prepare the control solution with 0.5% (1 g. Sodium Carbonate Hydrate is efflorescent in air. Sodium Acetate Hydrate is efflorescent in warm. Perform a blank determination and make any necessary correction.002 mol/L potassium permanganate VS and further boil for 5 minutes: the red color of the solution does not disappear. (8) Potassium permanganate-reducing substance⎯Dissolve 1. Packaging and Storage Preserve in tight containers. 20 mL of strong ammonia water and 0. add 7 mL of dilute nitric acid.50 mL of 0.0 g of Sodium Carbonate Hydrate in 10 mL of water.5 mL.01 mol/L disodium ethylenediamine tetraacetate VS until the blue color changes to grayish blue (indicator: 0. dilute with water to make 50 mL and perform the test. Description Sodium Acetate Hydrate is a colorless crystal or white.25 mL of a solution of sodium bisulfite (1 in 10) and titrate with 0. (2) Acid or alkali⎯Dissolve 1.0 mL of 0. crystalline powder.01 mol/L hydrochloric acid VS is added after cooling to 10 °C. acetous odor and has cool. Purity (1) Clarity and color of solution⎯Dissolve 1.0 g of Sodium Acetate Hydrate.017%). soluble in ethanol and practically insoluble in ether.0 g of Sodium Acetate Hydrate in 25 mL of water. add 8 mL of dilute .1 mol/L perchloric acid = 8. first at 80 °C for 2 hours and then at 130 °C for 2 hours).30 mL of 0.08 Sodium Acetate Hydrate.5 g of Sodium Carobonate Hydrate in 10 mL of water. Purity (1) Clarity and color of solution⎯Dissolve 2.0% of Sodium Carbonate Hydrate (Na2CO3·10H2O). Sodium Carbonate Hydrate liquefies in its water of crystallization at 34 o C and becomes anhydrous at above 100 o C .01 mol/L hydrochloric acid (not more than 0. (6) Calcium and magnesium⎯Dissolve 4.0% and not more than 40.0 g of Sodium Acetate Hydrate. or 1. Loss on Drying Not less than 61. A solution of Dried Sodium Carbonate (1 in 10) is alkaline.65 g of Sodium Carbonate Hydrate according to Method 1 and perform the test (not more than 3.2 g of Dried Sodium Carbonte. Dried Sodium Carbonate is hygroscopic. Prepare the control solution as follows: evaporate 8 mL of dilute hydrochloric acid on a water-bath to dryness.0% of Sodium Carbonate (Na2CO3). and titrate with 0.1 ppm). Assay Dissolve about 3. dilute with water to make 50 mL and perform the test. cool and further titrate until a greenish yellow color appears (indicator: 2 drops of bromocresol green TS). which foams on agitation. add 0. (2) A solution of Sodium Lauryl Sulfate (1 in 10) responds to the Qualitative Tests (1) for sodium salt.5 mL of dilute hydrochloric acid on a water-bath to dryness. add 2 mL of dilute with water to make 50 mL (not more than 20 ppm). forming a clear or an opalescent solution. Sodium Lauryl Sulfate Dried Sodium Carbonate Na2CO3: 105. 4 hours). Each mL of 0.0 mL of 0. (4) Arsenic⎯Prepare the test solution with 0.07 mg of Na2CO3·10H2O drochloric acid and evaporate on a water-bath to dryness.60 mL of 0. Prepare the control solution as follows: evaporate 7.0 g of Dried Sodium Carbonate in 10 mL of water: the solution is clear and colorless. Boil carefully. (3) Heavy metals⎯Dissolve 1. add 4 mL of brominecyclohexane TS with vigorous shaking. Dissolve the residue in 35 mL of water and 2 mL of dilute acetic acid. add 2 drops of phenol red TS and 0. add 12 mL of dilute nitric acid.1216 Monographs. 105 o C .38).5 mol/L sulfuric acid until the color of the solution changes from blue to yellow-green. Each mL of 0.0 and not more than 101. weighed accurately. (3) Take a solution of Sodium Lauryl Sulfate (1 in 10).0% (2 g. 2 drops). Packaging and Storage Preserve in tight containers. titrate until to a greenish yellow color develops (Indicator: bromcresol green TS.0 mL of standard lead solution and dilute with water to make 50 mL (not more than 10 ppm). Assay Dissolve about 1. (4) Arsenic⎯Prepare the test solution with 0. contains not less than 99. add 2 mL of dilute acetic acid and 2. and has a slightly characteristic odor.5 g of Dried Sodium Carbonate in 10 mL of water. Prepare the control solution with 1. (2) Sodium chloride⎯Dissolve about 5 g of Sodium .0 and not more than 63. Loss on Drying Not more than 2.0% (1 g. 1 g of Sodium Lauryl Sulfate dissolves in 10 mL of water.0 g of Sodium Carbonate Hydrate.2 g of the residue obtained in Total alcohol content.65 g of Dried Sodium Carbonate according to Method 1 and perform the test (not more than 3.5 mol/L sulfuric acid = 143.5 mol/L sulfuric acid until the color of solution changes from blue to yellow-green. Sodium Lauryl Sulfate is sparingly soluble in methanol and in ethanol and practically insoluble in ether. dilute with water to make 50 mL and perform the test.0 g of Dried Sodium Carbonate in 10 mL of water.99 mg of Na2CO3.0 g of Sodium Lauryl Sulfate in 100 mL of water. cool. Description Dried Sodium Carbonate is a white crystal or crystalline powder.99 Dried Sodium Carbonate. Part II hydrochloric acid and evaporate to dryness on a waterbath. Then boil cautiously. 105 o C .3 g of Nbromosuccinimide and heat in a water-bath at 80 o C for 5 minutes: a red color develops. in 25 mL of water.5 mol/L sulfuric acid = 52. (2) Chloride⎯Dissolve 0. add dilute hydrochloric acid to make acid.5 mL of dilute hy- Sodium Lauryl Sulfate is a mixture of sodium alkyl sulfate consisting chiefly of sodium lauryl sulfate (C12H25NaO4S: 289.1 ppm).071%). 4 hours). Description Sodium Lauryl Sulfate is a white to pale yellow crystal or powder. when dried.1 mol/L hydrochloric acid VS: the solution remains yellow. add 7. boil gently and cool: the solution responds to the Qualitative Tests for sulfate. Identification A solution of Dried Sodium Carbonate (1 in 20) responds to the Qualitative Tests for sodium salt and for carbonate. Packaging and Storage Preserve in tight containers. Purity (1) Clarity and color of solution ⎯Dissolve 1. weighed accurately. in 25 mL of water and titrate with 0. Dried Sodium Carbonate is freely soluble in water and practically insoluble in ethanol or in ether. Identification (1) Take 0.01 mol/L hydrochloric acid (not more than 0. Dissolve the residue in 35 mL of water and 2 mL of dilute acetic acid. Purity (1) Alkali⎯Dissolve 1. dilute with water to make 50 mL and perform the test. 04) obtained in the next (3) is not more than 8. Sodium Bisulfite is freely soluble in water and practically insoluble in ethanol and in ether.1 mol/L silver nitrate VS (indicator: 2 drops of fluorescein sodium TS). accurately weighed. add 5 mL of hydrochloric acid and evaporate on a water-bath to dryness. Combined the petroleum benzin extracts and wash with three 50 mL volume of water. in 150 mL of water and 50 mL of hydrochloric acid and boil under a reflux condenser for 4 hours.0 g of Sodium Bisulfite in 15 mL of water. Dry the residue at 105 o C for 30 minutes: the residue is not less than 59. Prepare the control solution as follows: evaporate 5 mL of hydrochloric acid on a water-bath to dryness and add 2 mL of dilute acetic acid and 2. Add 1 mL of hydrochloric acid and titrate the excess iodine with 0. Identification A solution of Sodium Bisulfite (1 in 20) responds to the Qualitative Tests for sodium salt and for bisulfite.5 g of Sodium Bisulfite in 10 mL of water. Cool.0 g of Sodium Bisulfite in 10 mL of water: the solution is clear and colorless.06). Prepare the control solution with 2.0 mL of standard iron solution (not more than 20 ppm). add 100 mL of ethanol and heat at a temperature just below the boiling point for 2 hours.6086 (4) Unsulfated alcohols⎯Dissolve about 10 g of Sodium Lauryl Sulfate. shake and allow to stand for 5 minutes: no turbidity is produced.1 mol/L sodium chloride TS and titrate with 0. Dry the precipitate. Purity (1) Clarity and color of solution⎯Dissolve 1.0 mL of 0.0% (0. heat to boiling. if necessary. add 2 mL of dilute acetic acid and water to make 50 mL and perform the test. stopper.5 g. (3) Heavy metals⎯Dissolve 1.KP VIII 1217 Lauryl Sulfate. Dissolve the precipitate by washing with 150 mL of water.05 mol/L iodine VS = 3. (5) Arsenic⎯Dissolve 0.44) and sodium sulfate (Na2SO4: 142. in 50 mL of water.1 mol/L sodium thiosulfate VS (indicator: 1 mL of starch TS).39). in 10 mL of water. (3) Sodium sulfate⎯Dissolve about 1 g of Sodium Lauryl Sulfate. . Evaporate the petroleum benzin on a water-bath and dry the residue at 105 o C for 30 minutes.1 mol/L silver nitrate VS = 5.0% and not more than 67. add slowly 5 mL of dilute hydrochloric acid. add 5.0 g of Sodium Bisulfite in 10 mL of water. If an emulsion forms.0 g of Sodium Lauryl Sulfate. sodium chloride may be added to promote separation of the two layers.0 mL of 0.05 mol/L iodine VS.0%.4% of sulfur dioxide (SO2: 64. Sodium Bisulfite is slowly affected by air or by light. Add 10 mL of hydrochloric acid. Packaging and Storage Preserve in well-closed containers Each mL of 0. add water to make 5 mL and perform the test (not more than 4 ppm). Sodium Bisulfite contains not less than 64. Collect the precipitate and wash with water until the last washing shows no opalescence with silver nitrate TS. accurately weighed. To the residue. Perform a blank determination and make any necessary correction.2032 mg of SO2 Amount (mg) of sodium sulfate (Na2SO4) = amount (mg) of barium sulfate (BaSO4) × 0. Add 1 mL of sulfuric acid. (2) Thiosulfate⎯Dissolve 1.0 mL of standard lead solution and dilute with water to make 50 mL (not more than 20 ppm). Water Not more than 5. Each mL of 0. direct titration). Perform a blank determination and make any necessary correction.0 g of Sodium Bisulfite according to Method 1 and perform the test according to Method A.15 g of Sodium Bisulfite and transfer immediately to an iodine flask containing 50. and has the odor of sulfur dioxide. volumetric titaration. shake and allow to stand for 5 minutes in a dark place. Total alcohol content Dissolve about 5. add 25 mL of barium chloride TS and allow to stand overnight. heat on a sand-bath until white fumes are evolved. in 100 mL of water. ignite to a constant weight between 500 o C and 600 o C by raising the temperature gradually and weigh as barium sulfate (BaSO4: 233. collecting the washings in a beaker. neutralize the solution with dilute nitric acid. Extract the solution with three 50 mL volume of petroleum benzin. A solution of Sodium Bisulfite (1 in 20) is acid. Assay Weigh accurately about 0.0%. (4) Iron⎯Prepare the test solution with 1. accurately weighed. Description Sodium Bisulfite is white granule or powder.844 mg of NaCl The combined content of sodium chloride (NaCl: 58.0% of the mass of the Sodium Lauryl Sulfate taken. extract twice with 75 mL volumes of ether and evaporate the combined ether extracts on a water-bath. Sodium Bisulfite Sodium Hydrogen Sulfite Sodium Bisulfite is a mixture of sodium bisulfite and sodium pyrosulfite. The mass of the dried residue is not more than 4. Filter through a glass filter (G4) while hot and wash with 100 mL of boiling ethanol. accurately weighed. add 100 mL of ethanol and transfer to a separatory funnel. 0 mL of 0. Add water to make 5 mL. (2) A solution of Sodium Hydroxide (1 in 25) responds to the Qualitative Tests for sodium salt. shake and proceed as directed above.04 Dried Sodium Sulfite contains not less than 97. Sodium Hydroxide rapidly absorbs carbon dioxide in air. Dried Sodium Sulfite is freely soluble in water and practically insoluble in ethanol or in ether. To 25 mL of the solution. add water to make 50 mL and perform the test. (5) Sodium carbonate⎯The amount of sodium carbonate (Na2CO3: 105.99) is not more than 2.0 mL of a solution of sodium tetraphenylboron (1 in 30). add 11 mL of dilute hydrochloric acid and evaporate on a water-bath to dryness.0% of sodium sulfite (Na2SO3). Sodium Hydroxide NaOH: 40.0 g of Sodium Hydroxide in 5 mL of water. tight containers. shake immediately and allow to stand for 10 minutes: the solution has no more turbidity than the following control solution. Description Sodium Hydroxide occurs as white fused masses. take this solution as the test solution and perform the test (not more than 4 ppm). add 10 mL of dilute nitric acid and water to make 50 mL and perform the test. Store in preferably well-filled and not exceeding 30 °C. Add 1 mL of hydrochloric acid and titrate the excess iodine with 0. sticks and other forms. Control solution⎯Dissolve 9.0 g of Sodium Hydroxide in 20 mL of water: the solution is clear and colorless.01 mol/L hydrochloric acid (not more than 0. add gradually 5 mL of hydrochloric acid. (3) Heavy metals⎯Dissolve 1. (2) Heavy metals⎯Dissolve 1.0 g of Dried Sodium Sulfite in 15 mL of water. (3) Arsenic⎯Dissolve 0. Packaging and Storage Preserve in tight containers.0 mL of this solution. Purity (1) Clarity and color of solution⎯Dissolve 1. Add 3 mL of boiling water and 1 mL of hydrochloric acid to the residue and again evaporate to dryness on a water-bath.0% of sodium hydroxide (NaOH).0% and not more than 101. add water to make 50 mL (not more than 30 ppm). flakes.1218 Monographs. Add 1. Dissolve the residue in 2 mL of dilute acetic acid and water to make 50 mL and perform the test. Prepare the control solution as follows: evaporate 3 mL of hydrochloric acid to dryness and add 2 mL of dilute acetic acid. (4) Potassium⎯Dissolve 0.1 mol/L sodium thiosulfate VS (indicator: 1 mL of starch TS). Prepare the control solution with 0. Sodium Hydroxide is freely soluble in water or in ethanol and practically insoluble in ether. pH⎯The pH of a solution of Dried Sodium Sulfite (1 in 10) is about 10. Part II Packaging and Storage Preserve in light-resistant.302 mg of Na2SO3.0 mL of dilute acetic acid to 4.0 mL of this solution and shake. add 2 mL of dilute acetic acid and 1 drop of ammonia TS. Sodium Hydroxide deliquesces in moist air. Add 1.0%. Dried Sodium Sulfite Na2SO3: 126. when calculated by the following equation using B .7 mL of 0. add 2 mL of hydrochloric acid gradually and evaporate the mixture on a water-bath to dryness. Add 5.0 mL of dilute acetic acid to 4.5 mg of potassium chloride in water and dilute with water to make 1000 mL. add 1 mL of sulfuric acid and evaporate on a sand-bath until white fumes are evolved.05 mol/L iodine VS = 6. Dried Sodium Sulfite gradually changes in moist air.5 g of Dried Sodium Sulfite in 5 mL of water. Perform a blank determination and make any necessary correction. shake and allow to stand for 5 minutes: no turbidity is produced. (2) Chloride⎯Dissolve 2. small pellets. Prepare the control solution as follows: evaporate 11 mL of dilute hydrochloric acid on a water-bath to dryness. Identification An aqueous solution of Dried Sodium Sulfite (1 in 20) responds to the Qualitative Tests for sodium salt and sulfite. dissolve the residue in 2 mL of dilute acetic acid and 3. Sodium Hydroxide is hard and brittle and shows a crystalline fracture.05 mol/L iodine VS.0 mL of standard lead solution and water to make 50 mL (not more than 20 ppm). 2. stopper.0% and not more than 101.050%). Dissolve the residue in 35 mL of water. Each mL of 0. Identification (1) A solution of Sodium Hydroxide (1 in 500) is alkaline. Description Dried Sodium Sulfite is white crystal or powder and odorless. Purity (1) Thiosulfate⎯Dissolve 1.10 g of Sodium Hydroxide in water and dilute with water to make 40 mL. Assay Weigh accurately about 0.0 g of Dried Sodium Sulfite in 5 mL of water.00 Sodium Hydroxide contains not less than 95. transfer immediately to an iodine flask containing 50.0 g of Sodium Hydroxide in water and add water to make 100 mL.2 g of Dried Sodium Sulfite.0 mL of standard lead solution. shake and allow to stand for 5 minutes in a dark place. Purity (1) Acid⎯Take 2. neutralize gradually with purified hydrochloric acid and add 5 mL of diluted sulfuric acid (1 in 2). shake with 5 mL of petroleum ether. add 50 mL of neutralized ethanol and heat on a waterbath nearly to boiling with stirring once or twice.5 mol/L sulfuric acid consumed.0 g of Sorbitan Sesquioleate according to Method 2 and perform the test. Specific Gravity Sorbitan Sesquioleate Sorbitan Sesquioleate is a mixture of monoester and diester of sorbitol anhydride. A (mL). add 10 mL of stannous chloride-sulfuric acid TS.0 g of Sorbitan Sesquioleate. Soybean Oil is miscible with ether or with carbon tetrachloride.5 mol/L sulfuric acid until the red color of the solution disappears. Saponification Value Between 150 and 168. Soybean Oil congeals between -10 o C and -17 o C . Description Soybean Oil is clear.99 × B (6) Mercury⎯Dissolve 2. Cool. Shake 2 mL of the lower layer with 2 mL of freshly prepared catechol solution (1 in 10). has faint.960 and 1.0% (1 g.KP VIII 1219 (mL) which is obtained in the Assay. partially esterified with oleic acid. Then add 2 drops of methyl orange TS to the solution and further titrate with 0.5 g of Sodium Hydroxide and dissolve in 40 mL of freshly boiled and cooled water. Perform the tests according to the Atomic Absorption Spectrophotometry (Cold vapor type) with the test solution.0 mL of standard mercury solution add 1 mL of a solution of potassium permanganate (3 in 50). A (mL) -B (mL). direct titration. add 2 drops of phenolphthalein TS and titrate with 0. Read the absorbance AT of the test solution when the indication of the recorder rises rapidly and becomes constant at the wavelength of 253. On the other hand. Identification (1) Take 0. characteristic odor and slightly bitter taste. add 4. Water Not more than 3. add a solution of hydroxylamine hydrochloride (1 in 5) until the precipitate of manganese dioxide disappears. Packaging and Storage Preserve in tight containers. add 2 mL of diluted nitric acid (1 in 2) and then add 0. viscous oily liquid. Record the amount.1 mol/L sodium hydroxide VS and 5 drops of phenolphthalein TS: a red color develops. connect the bottle immediately to the atomic absorption spectrophotometer and circulate air. of 0. (2) Heavy metals⎯Proceed with 1. when cooled. of 0. (3) Arsenic⎯Prepare the test solution with 1. To the residue. Cool. soluble in ethanol and very slightly soluble in methanol. Congealing point of the fatty acids⎯Between . crystals are formed. odorless or has slight odor and bland taste. Sesquioleate is dispersed as fine oily drops in water. stir for 30 minutes). Cool the solution to 15 °C.5 g of Sorbitan Sesquioleate. B (mL). then with 5 mL of sulfuric acid: a red to red-brown color develops.5 mol/L sulfuric acid = 40.0 g of Sorbitan Sesquioleate according to Method 2 and perform the test (not more than 2 ppm). Calculate the amount of NaOH from the difference. Record the amount.0 g of Sodium Hydroxide in 1 mL of a solution of potassium permanganate (3 in 50) and 30 mL of water. Place the test solution in the test bottle of an atomic absorption spectrophotometer. to 2. 25 : d 25 Soybean Oil Oleum Sojae Soybean Oil is the fixed oil obtained from the seeds of Glycine max Merrill (Leguminosae).020. slightly Between 0. Assay Weigh accurately about 1. AS of the solution obtained by the same procedure as used for the test solution: AT is smaller AS. Sorbitan Sesquioleate is freely soluble in ether.5 g of potassium nitrite between 30 °C and 35 °C with stirring: the solution develops an opalescence and.5 mol/L sulfuric acid until the solution shows a persistent pale red color. volumetric titration.0 mL of standard lead solution (not more than 20 ppm). Residue on Ignition Not more than 1. Prepare the control solution with 2. (2) Heat the upper layer obtained in (1) on a waterbath and evaporate petroleum ether. To this solution. add water to make exactly 100 mL and use this solution as the test solution.00 mg of NaOH Packaging and Storage Preserve in tight containers.7 nm.3 mL of 0. Description Sorbitan Sesquioleate is pale yellow to pale yellow-brown.5 mol/L sulfuric acid consumed. Each mL of 0. add 5 mL of ethanol and 5 mL of dilute sulfuric acid and heat on a water-bath for 30 minutes.0% (1 g). Amount (mg) of sodium carbonate = 105. 30 mL of water and a volume of purified hydrochloric acid equal to that used in the preparation of the test solution and read the absorbance. Soybean Oil is slightly soluble in ethanol and practically insoluble in water. pale yellow oil. allow to stand and separate the upper layer and the lower layer. Ester Value Not more than 3.0.0. shake with 5 mL of boiling water for 2 minutes. it melts and swells and decomposes. Iodine Value Not more than 2. Packaging and Storage containers. Packaging and Storage Preserve in tight containers. Preserve in well-closed Preserve in well-closed Sucrose CH2OH H H CH2OH O H O H OH H H OH H HO O CH2OH HO OH H C12H22O11: 342. Stearic Acid is freely soluble in ether. Melting Point Between 56 °C and 62 °C (Method 2). Acid Value Between 194 and 210. unctuous or crystalline mass or powder and has a faint. (2) Heavy metals⎯Proceed with 1. Stearyl Alcohol Saponification Value Between 188 and 195.70 mL of 0. Sucrose is very soluble in water. Iodine Value Between 126 and 140.0%. (2) Alkali⎯Take the solution obtained in (1) and add 2 drops of phenolphthalein TS: no red color develops. Purity (1) Mineral acid⎯Melt 5 g of Stearic Acid by warming. Part II 22 o C and 27 o C . Residue on Ignition Not more than 0. Identification (1) When 1 g of Sucrose is ignited.2. Specific Gravity 25 : Between 0.0 g of Stearic Acid with 0. (3) Fat and paraffin⎯Boil 1. to bulky charcoal. very slightly soluble in ethanol and practically insoluble in ether.1% (1 g). filter after cooling and add 1 drop of methyl orange TS to the filtrate: no red color develops. Stearyl Alcohol is a mixture of solid alcohols and consists chiefly of stearyl alcohol (C18H38O). Unsaponifiable Matter Not more than 1. is odorless and has a sweet taste. Melting point—Between 56 °C and 72 °C (Method 2). Acid Value Not more than 1.0 g of Stearic Acid according to Method 2 and perform the test.922. is clear or not more turbid than the following control solution.0.05% (2 g).0. or lustrous colorless or white crystal.916 and 0.0 g of Stearyl Alcohol in 25 mL of dehydrated ethanol by warming: the solution is clear.01 mol/L hydrochloric acid. Packaging and Storage containers. Stearyl Alcohol is freely soluble in ethanol. A solution of Sucrose (1 in 10) is neutral.1 g of Sucrose. fatty odor. emitting an odor of caramel. characteristic odor and is tasteless. Control solution⎯Take 0.0 mL of standard lead solution (not more than 20 ppm). add 6 mL of dilute nitric acid and water to make 30 mL and add 1 mL of silver nitrate TS. Prepare the control solution with 2. d 25 Acid Value Not more than 0. Description Stearyl Alcohol is a white. Description Stearic Acid is a white. Iodine Value Not more than 4.5 g of anhydrous sodium carbonate and 30 mL of water: the solution. while hot. Residue on Ignition Not more than 0. soluble in ethanol and practically insoluble in water. add 2 mL of dilute sulfuric .1220 Monographs.30 Description Sucrose is a white crystalline powder. Stearic Acid Stearic Acid is a solid fatty acid obtained from fats and consists chiefly of stearic acid (C18H36O2) and palmitic acid (C16H32O2). in dehydrated ethanol or in ether and practically insoluble in water. Purity (1) Clarity of solution⎯Dissolve 3. Hydroxyl Value Between 200 and 220. unctuous matter and has a faint. (2) Take 0. To 20 mL of test solution. if necessary and use this solution as the test solution. then to 5 mL of this solution add 0.0 g of Sucrose according to Method 1 and perform the test.0 g of Sucrose according to Method 1 and perform the test (not more than 2 ppm). heat at 130 o C for 10 minutes: the principal spot from the test solution is the same with the principal spot from the standard solution (1) in the Rf . Specific Optical Rotation and +67. fructose and white soft sugar. add methanol (3 in 5) to make 20 mL and use this solution as the standard solutions (1) and (2). the label states the purpose. 50 mL of water.01 mol/L hydrochloric acid VS (not more than 0.50 mL of 0.5 mL of standard lead solution (not more than 5 ppm).0 g of Purified Sucrose in recently boiled and cooled water to make 100 mL and use this solution as the test solution. boil and add 4 mL of 2 mol/L sodium hydroxide TS: orange precipitates are immediately produced. add diluted methanol (3 in 5) to make 20 mL each and use these solutions as the test solution and the standard solution (1). (4) Calcium⎯Take 10 mL of the test solution obtained in (2) and add 1 mL of ammonium oxalate TS: this solution shows immediately no change. (2) Dissolve 50.15 mL of freshly prepared cupric sulfate TS and 2 mL of freshly prepared 2 mol/L sodium hydroxide TS: the solution is clear and blue and not changes on boiling. Perform the. add water to make 100 mL.005 mol/L sulfuric acid VS (not more than 0. Prepare the control solution with 0. (5) Heavy metals⎯Proceed with 5.005%). Purified Sucrose is very soluble in water and slightly soluble in ethanol.30 mL of 0. Identification (1) Take 10 mg each of Purified Sucrose and white soft sugar. stopper and allow to stand for 2 days: no precipitate is produced. 13 g. add 4 mL of sodium hydroxide TS and 3 mL of Fehling’s TS and heat to boiling: red to dark red precipitate is produced. Residue on Ignition Not more than 0. Then to this solution. Perform the test. Spot 2 μL each of the test solution and the standard solutions (1) and (2) on a plate of silica gel for thin-layer chromatography and dry the plate completely.KP VIII 1221 acid.0 g of sucrose and add water to make 100 mL. take 50 mL of this solution in a Nessler tube and view transversely the Nessler tube against a white background: the solution is colorless or slightly yellow and has blue color.30% (15 g. place 100 mL of alkaline cupric sulfate TS in a 300 mL beaker. 2 hours).3 . For Purified Sucrose used for preparation of the large volume infusions. Separately. CH2OH H H CH2OH O H O H OH H H OH H HO O CH2OH HO OH H C12H22O11: 342. Prepare the control solution with 2. Wash the residue on the filter with water until the last washing is neutral. (6) Arsenic⎯Prepare the test solution with 1. add at once 50 mL of freshly boiled and cooled water. Spray evenly a solution of 0. color and size and four spots from the standard solution (2) are apparently distinguishable. cover the beaker with a watch glass and boil.006%). then wash with 10 mL of ethanol. To 1 mL of the test solution.0 (after drying. Prepare the control solution with 0. Separately. (3) Sulfate⎯Take 40 mL of the test solution obtained in (2). Immediately add 50 mL of the test solution. boil.0 g of Sucrose in water to make 100 mL and filter. Develop the plate with a mixture of 1.120 g.10% (2 g). (7) Invert sugar⎯Dissolve 5. Specific Optical Rotation o [α ]20 D : Between +66. 100 Purity (1) Clarity and color of solution⎯Dissolve 100 g of Sucrose in 100 mL of water. add 4 mL of dilute hydrochloric acid. or lustrous colorless or white crystal. add 6 mL of dilute nitric acid and water to make 50 mL. respectively. Fill the solution in the Nessler tube.30 Purified Sucrose contains no additives. to 10 mg each of glucose. Description Purified Sucrose is a white crystalline powder. (2) Chloride⎯Take 10.5 g of thymol in 100 mL off mixture of ethanol and sulfuric acid (19 : 1). lactose.2-dichloroethane. And immediately repeat the development with replaced developing mixture and dry the plate in the same way. o Purified Sucrose o [α ]20 D : Between +65. glacial acetic acid. Loss on Drying Not more than 1. 105 o C . methanol and water (10 : 5 : 3 : 2) to a distance of about 15 cm and dry the plate with a hot air. add 10 mL of ether and dry at 105 o C for 30 minutes: the residual precipitate is not more than 0. boil the mixture exactly for 5 minutes. dip in a water-bath of a temperature below 10 o C for 5 minutes and collect the precipitate in a tared glass filter (G4). add 1 mL of dilute hydrochloric acid and water to make 50 mL. Perform the test with the test solution and the solutions as directed under the Thin-layer Chromatography. Packaging and Storage Preserve in well-closed containers.0 mm). 01 cm−1 to 1 cm−1 .0 g.0 mL of nitric acid to make exactly 100 mL and make any necessary correction (not more than 0. Use a cell giving the cell constant of 0.0746 g and 0. in newly distillated water having less conductivity than 2 μS· cm−1 to get three kinds of the standard solution containing 0.0 mL each of the test solution and the standard solution. seal up the vessel and heat at 150 o C for 5 hours. (2) Acid or alkali⎯Take 10 mL of the test solution obtained in the Identification (2).3 mL of phenolphthalein TS: the solution is colorless and develops a red color on addition of 0. Temperature for atomization: 2100 o C . To 5. the absorbance of the test solution is not larger than that of the standard solution (not more than 15 ppm as SO2). (3) Procedure⎯Use the suitable potassium chloride conductivity calibration standard solution to the measurement. After exactly 2 minutes.5 mL of nitric acid to dissolve. Perform the test with more than 3 parts of the test solution as directed in the standard addition method under the Atomic Absorption Spectrophotometry (electrothermal type) according to the following operating conditions. respectively. result of the left is invalid. add 0. take the tube out of the bath and examine the solution immediately: the blue color does not disappear completely (0. then pipet 5. The cell constant.0 g) 0.0 mL of water in the same manner as above. Temperature for drying: 110 o C . add water to make exactly 100 mL.3 mL of 0. The conductivities of these solutions at 20 o C are shown in the following table. Pipet 3. Lamp: A hollow cathode lamp. kept up the cell with the calibration standard solution and determine the conductivity of the calibration standard solution kept at 20 ± 0. 100 mm).0 mL of decolorized fuchsin TS and 2.4 mL of ferric chloride colorimetric stock solution and 0. about 150 mm in length and about 16 mm in diameter.0 mL of methylene blue TS.0 g of Sucrose in 40 mL of water. mix and place in a water-bath. add 1.0149 g of potassium chloride in 1000.0 mL of this solution. G x0 (μS).0 o (26.0746 0. The standard solution is prepared by adding water to a suitable volume of standard lead solution exactly and perform a blank determination with a solution prepared by adding water to 10. 0.7455 g.0 mL of formalin TS and allow to stand for 30 minutes.0 mL of this solution.0 mL of diluted hydrochloric acid (7 in 250). Separately. 2. add 0.6 mL of cobaltous chloride colorimetric stock solution add 7. is calculated by the following equation. Part II and +67. 100 mL. Conductivity (1) Potassium chloride conductivity calibration standard solution⎯Dissolve powdered potassium chloride. pipet 10. (3) Sulfite⎯Dissolve 5. previously dried at 500 o C to 600 o C for 4 hours. add water to make exactly 5 mL and use this solution as the test solution.0 26. After washing the well with water.0 mg of Purified Sucrose in a polytetrafuruoroethylene decomposition-vessel. The conductivity cell contains of two parallel platinum electrodes coated with platinum black and both electrodes are generally protected by a glass tube which allows good exchange between the solution and the electrodes. After cooling. Purity (1) Clarity and color of solution⎯The test solution obtained in the Identification (2) is clear and is not more intense than the following control solution. Determine the absorbance at 583 nm of the test solution and the standard solution as directed under the Ultraviolet-visible Spectrophotometry using the control solution obtained by proceeding with 10.1222 Monographs.0 mL of diluted hydrochloric acid (7 in 250).1 o C . water. add 5 mL of water. 1. Control solution⎯Take 2. (5) Invert sugar⎯Transfer 5 mL of the test solution obtained in the Identification (2) to a test-tube. Wavelength: 283. (4) Lead⎯Take 50. add 2. J .3 nm.7455 0. It is usually equipped with a temperature compensation device. add 4.0 mL of 3 mol/L hydrochloric acid. Repeat the determination and measure the conductivity of the calibration standard solution. J = xKCl G x0 . dissolve 76 mg of sodium metabisulfate in water to make exactly 50 mL. Immediately.0 mL of this solution. The apparatus is supplied with alternative current to avoid the effects of electrode polarization. Ignore any blue color at the air and solution interface.0 g.0 mL of 1 mol/L sodium hydroxide TS and 1. after a stable reading of ± 3% is obtained. rinse 2 to 3 times with the calibration standard solution.0 mL of dilute sodium hydroxide TS and water to make exactly 100 mL and use this solution as the standard solution. Temperature for incineration: 600 o C .0 Resistivity (Ω·cm) 752 7519 37594 (2) Apparatus⎯Use an appropriate conductivity meter. add 95.0149 Conductivity (μS· cm−1 ) 1330 133. When the standard solution does not show a red color.5 ppm). Standard solution (g/1000.01 mol/ 1 sodium hydroxide VS.04%). The conductivity is determined to measure the electrical resistance of the column of liquid between the electrodes of the immersed measuring device (conductivity cell).0 mL of dilute sodium hydroxide TS and water to make exactly 50 mL and use this solution as the test solution. boil and filter. until the filtrate becomes clear: the filtrate is neutral. Loss on Drying Not more than 5. (4) Arsenic⎯Take 0.05 mL of iodine TS: the solution remains yellow. Combine the filtrate and the washing. Bacterial Endotoxins Less than 0. until the filtrate becomes clear. add 10 mL of hydrochloric acid and evaporate the mixture on a water-bath to dryness. Centrifuge. if necessary. add 50 mL of water. Purity (1) Acid-soluble substances⎯Weigh accurately about 1. fill up with the test solution and determine the conductivity of the test solution. Add 10 mL of a solution of methylene blue (1 in 1000) to the residue and wash with water: the precipitate is blue. add 8 mL of water. GT (μS). x T (μS · cm−1 ) = JGT x 0 (μS · cm−1 ) = JG0 Determine the corrected conductivity. kept at 20 ± 0. x C . heat with 20 mL of dilute hydrochloric acid at 50 o C for 15 minutes with stirring. add 20 mL of water. To 25 mL of this filtrate. weigh and boil for 30minutes. evaporate to dryness and ignite to a constant weight at 800 ± 25 o C : the residue is not more than 2. (2) Dissolve 2 g of ammonium chloride and 5 mL of ammonia TS in the filtrate obtained in (1). 3 hours). Evaporate 20 mL of the filtrate to dryness and dry the residue at 105 o C for 1 hours: the residue is not more than 4. Cool. fine.25 EU per mg of Purified Sucrose when Purified Sucrose is used to prepare large volume aqueous infusions.2 g of Talc with 0. Dissolve 31. Talc is practically insoluble in water. by the following expressions. rinse the cell with the test solution 2 to 3 times.0 g of Talc. between 450 o C and 550 o C . while stirring. Identification (1) Mix 0. xT (μS · cm−1 ) and x 0 (μS · cm−1 ). 0.35 x 0 Loss on Drying Not more than 0. Cool.5 g of Talc.0%. Talc Talc is a native. if necessary. Tartaric Acid HOOC H OH C C OH H COOH . if necessary and add dibasic sodium phosphate TS: a white.1% (2 g. in ethanol or in ether. Talc is unctuous and adheres readily to the skin. add 1 mL of dilute sulfuric acid.0 g of Talc. Packaging and Storage Preserve in well-closed containers. After washing well the cell with water. is odorless and tasteless. crystalline powder. add 5 mL of dilute sulfuric acid and heat gently to boiling with shaking. (2) Acid or alkali and water-soluble substances⎯Take 10. then with 10 mL of water. filter and wash the residue with 5 mL of dilute sulfuric acid. Cool and transfer the fused mixture to a beaker with the aid of 50 mL of hot water. sometimes containing a small volume of aluminum silicate.0% (1 g. add water to make exactly 50 mL and filter. Cool.0 mg (3) Water-soluble iron⎯Make 10 mL of the filtrate obtained in (2) weakly acidic with hydrochloric acid and add drop-wise potassium ferrocyanide TS: the liquid does not acquire a blue color. 3 hours). Determine the conductivity of the water used for preparation of the test solution. x KCl : Conductivity constant of the potassium chloride conductivity calibration standard solution (μS · cm−1 ) (20 o C ). Centrifuge. add water to restore the original mass and filter. of the test solution by the following equation: not more than 35 μS · cm−1 x C (μS · cm−1 ) = x T − 0.KP VIII 1223 J : Cell constant ( cm−1 ). filter.9 g of anhydrous sodium carbonate and 1. crystalline precipitate is produced.1 o C . to 2 mL of the test solution obtained in the Identification (2).3 g of Purified Sucrose in newly distillated water to make exactly 100 mL and use this solution as the test solution. supplying water lost by evaporation. hydrous magnesium silicate. Cool immediately. Add hydrochloric acid until it ceases to cause effervescence. G x0 : Conductivity measured (μS). G0 (μS). 105 o C . Packaging and Storage Preserve in well-closed containers. in the same manner as above and calculate the conductivity. Dextrins For Sucrose used to prepare large volume aqueous infusions. Description Talc is white to grayish white. evaporate to 5 mL on a water-bath and perform the test (not more than 4 ppm).05 mL of dilute hydrochloric acid and 0.3 g of anhydrous potassium carbonate and heat the mixture in a platinum or nickel crucible until fusion is complete. add 10. Separately.5% and not more than 101. Titanium Oxide TiO2: 79.3 nm. Shake 1 g of Titanium Oxide with 10 mL of water: the mixture is neutral.1224 Monographs. Residue on Ignition Not more than 0.04 mg of C4H6O6 Packaging and Storage Preserve in well-closed containers.09 Tartaric Acid. with potassium hydroxide.0 mL of standard lead solution (not more than 10 ppm). Determine the absorbances of the test solution and the standard solution as directed under the Atomic Absorption Spectrophotometry according to the following operating conditions: the absorbance of the test solution is smaller than that of the standard solution (not more than 60 ppm). Wavelength: 283. Each mL of 1 mol/L sodium hydroxide VS = 75. Standard stain—Proceed in the same manner without Titanium Oxide. place 6. To this solution.0 g of potassium bisulfate. dissolve in 40 mL of water and titrate with 1 mol/L sodium hydroxide VS (indicator: 2 drops of phenolphthalein TS). add 30 mL of a solution of ammonium citrate (9 in 20) and 50 mL of water. (2) Oxalate⎯Dissolve 1.0 mL of standard lead solution in a platinum crucible. Loss on Drying Not more than 0.50 mL of 0. then raise the temperature gradually and heat strongly with occasional shaking until the contents fuse to yield a clear liquid. silica gel.005 mol/L sulfuric acid (not more than 0. Cool. dissolve by heating on a water-bath. freely soluble in ethanol and slightly soluble in ether. in nitric acid or in dilute sulfuric acid. heat gently with caution at the beginning. Lamp: Lead hollow cathode lamp. add 2 to 3 drops of hydrogen peroxide TS: a yellow-red color develops. Purity (1) Sulfate⎯Perform the test with 0. Titanium Oxide dissolves in hot sulfuric acid or in hydrofluoric acid and does not dissolve in hydrochloric acid. A solution of Tartaric Acid (1 in 10) is dextrorotatory. Prepare the control solution with 0.5 g of Tartaric Acid. (4) Calcium⎯Neutralize a solution of 1. add 20.5 mL of ammonia TS. shake for 10 minutes and use this n-butyl acetate solution as the test solution. Description Titanium Oxide is a white powder. (2) Arsenic⎯Perform the test with 20 mL of the test stock solution obtained in (1) as the test solution: the stain is not more intense than the following standard stain. cool. transfer 20 mL of the obtained solution to a generator bottle. Part II C4H6O6: 150. 3 hours). Tartaric Acid is very soluble in water. is odorless and has strong acid taste.0 g of Tartaric Acid in 10 mL of water and add 2 mL of calcium chloride TS: no turbidity is produced.7 and not more than 101.5 g of Titanium Oxide with 5 mL of sulfuric acid until white fumes are evolved. Assay Weigh accurately about 1.0% of Tartaric Acid (C4H6O6). When fused by heating with potassium bisulfate. previously dried.0 mL of a solution of dithizone in n-butyl acetate (1 in 500). cool.0 g of Titanium Oxide in a platinum crucible. Identification (1) Ignite Tartaric Acid gradually: it decomposes and an odor of burning sugar is perceptible.0 g of Tartaric Acid according to Method 1 and perform the test (not more than 1 ppm). in dehydrated ethanol or in ether. contains not less than 99. add 2.0 mL of standard arsenic solution and proceed in the same manner as the test with the test solution (not more than 10 ppm). Take 25 mL of the solution to a separatory funnel. contains not less than 98. Prepare the control solution with 2. (5) Arsenic⎯Prepare the test solution with 2. crystalline powder. (3) Heavy metals⎯Proceed with 2.5 g of Tartaric Acid. when dried. odorless and tasteless. Identification Heat 0.5% (3 g. . neutralize with ammonia TS and add 2.87 Titanium Oxide. or with potassium carbonate. Titanium Oxide is practically insoluble in water. Gas: Combustible gas—Acetylene gas or hydrogen gas Supporting gas—Air. add cautiously water to make 100 mL and filter. it changes to soluble salts.05% (1 g).0 g of Tartaric Acid according to Method 4 and perform the test. add 10 mL of a solution of ammonium sulfate (2 in 5) and 5 drops of thymol blue TS. proceed as directed in the test solution and use this solution as the standard solution. Purity (1) Lead⎯Place 1. Description Tartaric Acid is colorless crystal or white. To 5 mL of the filtrate. when dried. add water to make 100 mL and use this solution as the test stock solution.048%).0% of titanium oxide (TiO2). (2) A solution of Tartaric Acid (1 in 10) changes blue litmus paper to red and responds to the Qualitative Tests for tartrate.0 g of Tartaric Acid in 10 mL of water with ammonia TS and add 1 mL of ammonium oxalate TS: no turbidity is produced. Assay Dissolve about 2 g of Trolamine. . wash the crucible with a mixture of 75 mL of water and 2. 105 °C.19 of C6H15NO3 Packaging and Storage tight containers. Description Triethanolamine is colorless or pale yellow viscose liquid with a slight odor of ammonia. shake thoroughly and filter through double filter paper. After sedimentation of a yellow precipitate.3 mL of cobaltous chloride TS : a carmine-red color is developed. Identification (1) Take 1 mL of Trolamine.128 d 20 Water Not more than 0.0 g of Titanium Oxide with 50 mL of water and allow to stand overnight.120 and 1. Packaging and Storage Preserve in well-closed containers.486. with ethanol or with chloroform. Trolamine contains not less than 99.19). volumetric titration. add 2 to 3 drops of bromothymol blue TS. transfer to a crucible and add 3 g of potassium pyrosulfate. add 5 mL of sodium hydroxide TS. add again cupferron TS until a white precipitate is produced. Heat strongly between 900 °C and 950 °C to constant weight. transfer the contents of the crucible to a 250 mL beaker. evaporate 100 mL of the clear filtrate on a water-bath and heat strongly at 650 °C to constant weight: the mass of the residue is not more than 5.5% (1. When the precipitate is filtered and washed. Dry the precipitate together with the filter paper at 70 °C. Wash the precipitate on the filter paper with ten 25 mL volumes of a solution of ammonium tartrate (1 in 100). Continue heating for 30 minutes at a higher temperature to make the fused mixture a deep yellow-red.0% and not more than 107. containing 2. nD20 : Between 1.0 mg. Cool. previously dried. if necessary and allow titanium oxide to settle.5 mL of ammonium sulfide TS.19 Triethanolamine Trolamine is a mixture of alkanolamines consisting largely of triethanolamine containing some diethanolamine and monoethanolamine. Assay Weigh accurately about 0. (2) Take 1 mL of Trolamine. neutralize with ammonia TS and acidify with 1 mL to 2 mL of diluted sulfuric acid (1 in 2). Cool and dilute with water to make 400 mL. Residue on Ignition Not more than 0. direct titration. Cover and heat gently at first. Combine the filtrate and the washings. add further 2 mL of ammonium chloride TS.2 g of Titanium Oxide. Loss on Drying Not more than 0.KP VIII 1225 (3) Water-soluble substances⎯Shake thoroughly 4.5 mL of sulfuric acid into the beaker and heat on a water-bath until the solution becomes almost clear. add 40 mL of diluted sulfuric acid (1 in 2) and boil to expel hydrogen sulfide. evaporate by heating to 2 mL: the color of the solution does not change. transfer to a tared crucible and heat very gently at first and raise the temperature gradually after smoke stops evolving. add 0. add 30 mL of ammonia TS. accurately weighed. in 75 mL of water. cool and weigh as titanium oxide (TiO2).1 mL of cupric sulfate TS: a deep blue color is developed. Discard the first 10 mL of the filtrate. add 0.4% of alkanolamines. Add gradually 40 mL of cupferron TS to the solution with stirring and allow to stand. 20 : Between 1. Preserve in light-resistant. calculated on the basis as triethanolamine (C6H15NO3: 149.05% (2 g). Pass hydrogen sulfide sufficiently through the solution. gradually raise the temperature and then heat the fused contents for 30 minutes. Dissolve 2 g of l-tartaric acid in the solution. Trolamine CH2CH2OH N CH2CH2OH CH2CH2OH C6H15NO3: 149. To this solution.0 g. Refractive Index Specific Gravity (method 1). Each mL of 1 mol/L hydrochloric acid = 149. prevent ferrous sulfide from oxidation by filling the solution on the filter paper. almost clear liquid. Triethanolamine is miscible with water.5% (1 g. again saturate the solution with hydrogen sulfide. using a mixture of 5. 3 hours). wash twenty times with diluted hydrochloric acid (1 in 10) and remove water by stronger suction at the last washing. (3) Heat 1 mL of Trolamine gently in a test tube: the vapors turn moistened red litmus paper blue. titrate with 1 mol/L of hydrochloric acid (indicator: methylet TS 2 drops).481 and 1. Filter by slight suction using quantitative filter paper.0 mL of glacial acetic acid and 20 mL of methanol instead of methanol for Karl Fisher method). allow to stand for 10 minutes and filter. Shake thoroughly with 2 mL of ammonium chloride TS. Add water to make 200 mL. warm between 60 o C and 65 o C for 10 minutes and add sulfuric acid to raise the lower level of the oily layer to the graduated volume of the neck: not more than 0. Residue on Ignition Not more than 0.465 and 1. bitter taste.2 g of Urea. dissolve in water and add water to make exactly 200 mL. Identification (1) Heat about 0.1% (1 g). Shake 5 mL of Turpentine Oil with 5 mL of a solution of potassium hydroxide (1 in 6): the aqueous layer does not show a yellow-brown to dark brown color. then cool. and has characteristic odor and pungent.5 g of Urea in a test tube: it liquefies and ammonia is evolved.007%). freely soluble in boiling ethanol. colorless to pale yellow liquid.40 mL of 0. Continue the heating until the liquid becomes turbid.875. (2) Sulfate⎯ Perform the test with 2.30028 mg of CH4N2O Preserve in light-resistant.005 mol/L sulfuric acid VS = 0.860 and 0.0% and not more than 101.05 mol/L sulfuric acid VS (not more than 0. Prepare the control solution with 0. Urea is very soluble in water. pH Between 5. Turpentine Oil (1 mL) is miscible with 5 mL of ethanol and this solution is neutral. Description Turpentine Oil is clear.01 mol/L hydrochloric acid VS (not more than 0.0 mL of standard lead solution (not more than 20 ppm) (4) Ethanol-insoluble matter⎯Dissolve 5.0 g of Urea. Assay Transfer about 0. filter the solution through a glass filter.0 mg. H2O: 18.1 mL of oil separates.40 mL of 0.6. (3) Mineral oil⎯Place 5 mL of Turpentine Oil in a cassia flask. Prepare the control solution with 2. (3) Heavy metals⎯Proceed with 1. Packaging and Storage Preserve in well-closed containers.02 Water generally means tap water or well water. add drop-wise 25 mL of fuming sulfuric acid while shaking. Melting Point Between 132. Pipet exactly 5 mL of this solution into a Kjeldahl flask and proceed as directed under Nitrogen Determination. Dissolve the fused mass in a mixture of 10 mL of water and 2 mL of sodium hydroxide TS (1 in 10) and add 1 drop of cupric sulfate TS: the solution acquires a reddish violet color. accurately weighed.0% of urea (CH4N2O).06 Urea contains not less than 99. clear liquid. Purity (1) Color and turbidity⎯View downward 50 mL of Water placed in a Nessler tube against white and black backgrounds: it is clear and colorless.010%).1226 Monographs. Distilling Range less than 90% Between 150 o C and 170 o C . Prepare the control solution with 0. Part II Turpentine Oil Oleum Terebinthinae Turpentine Oil is the essential oil distilled with steam from the wood or balsam of Pinus species (Pinaceae). Purity (1) Chloride⎯Perform the test with 2. A solution of Urea (1 in 100) is neutral. is odorless and has a fresh salty taste. Description Urea is a colorless or white crystal or crystalline powder. Refractive Index Specific Gravity nD20 : Between 1.478. .5 o C . d 20 Purity (1) Foreign matter⎯Turpentine Oil has no offensive odor. soluble in ethanol and slightly soluble in ether.1 g of Urea in 1 mL of water and add 1mL of nitric acid: a white crystalline precipitate of urea nitrate is formed. 20 : Between 0.8 and 8. (2) Dissolve 0. Each mL of 0. Urea H 2NCONH Water 2 CH4N2O: 60.5 o C and 134. Description It is a colorless.0 g of Urea according to Method 1 and perform the test.0 g of Urea in 50 mL of warm ethanol and if any insoluble residue remains. cool to a temperature not exceeding 15 o C . not Packaging and Storage tight containers. (2) Hydrochloric acid-coloring substances⎯Shake 5 mL of Turpentine Oil with 5 mL of hydrochloric acid and allow to stand for 5 minutes: the hydrochloric acid layer is pale yellow and not brown.0 g of Urea. wash the residue with 20 mL of warm ethanol and dry at 105 o C for 1 hour: the residue is not more than 2. allow to stand for 10 minutes with occasional shaking. add 1 mL of sodium salicylatesodium hydroxide TS. Separately. (9) Iron⎯Prepare the test solution with 50 mL of Water according to Method 1. Separately.15 mL of standard ammonium solution. (10) Zinc⎯Shake 50 mL of Water with 0. Separately. add 5 mL of pyridinepyrazolone TS. Gas: Combustible gas—Acetylene or hydrogen. Allow to stand.KP VIII 1227 (2) Odor and taste⎯Place 100 mL of Water in a 300-mL glass-stoppered Erlenmeyer flask. Control solution⎯Pipet 1. Prepare the control solution with 1. add water to make exactly 50 mL.5 mL of nitric acid. and add water to make exactly 1000 mL. dilute with purified water for Ammonium limit Test to make 30 mL. Then view the Nessler tube downward or transversely: the color of the solution is not darker than the following control solution.0 mL of standard lead solution (not more than 1 mg/L). (7) Cyanide⎯Place 20 mL of Water in a Nessler tube. Prepare the control solution with 0.01 mg/L). (11) Cadmium⎯Shake 50 mL of Water with 0. add 0. Then add 10 mL of a solution of ammonium sulfate (2 in 5) and 5 mL of a solution of sodium diethyldithiocarbamate trihydrate (1 in 20). allow to stand for several minutes. add 10 mL of water. Place 20 mL of this solution in a Nessler tube. and proceed in the same manner as for the test solution (not more than 0.5 mL of nitric acid. and use this solution as the standard solution.0 mL of Water in a 50 mL beaker.5 mL of nitric acid. and evaporate to dryness on a water bath.0 mL of standard cyanide solution.35453× a × 50 (4) Nitrogen from nitrates⎯Place 2. and allow to stand for 1 hour.5 mL of nitric acid. Wavelength: 228.0 mL of standard zinc solution with water to make exactly 50 mL. and allow to stand for 10 minutes: it dose not exhibit a light-red color. and proceed in the same manner as for the test solution (not more than 0. add 0. Calculate the concentration of chlorine ion in Water from the amount a (mL) of 0. add 10 mL of 4-methyl-2-pentanone. and use this solution as the test solution.5 mL of silver chromate-saturated potassium chromate TS).9 nm. To this solution add 10 mL of a solution of diammonium hydrogen citrate (1 in 4) and 2 drops of bromothymol blue TS. and transfer to a Nessler tube. mix gently. allow to stand for 1 hour. and use this solution as the standard solution. mix well. add 5 mL of phosphate buffer solution (pH 6. and shake vigorously. stopper immediately. dilute 2. (3) Chlorine ion⎯ Pipet 50 mL of Water. and perform the test according to Method B.8) and 1. dissolve with shaking. take 0. (5) Nitrogen from nitrites⎯Place 50 mL of Water in a Nessler tube. and check the odor and taste. and check the odor and taste again as soon as the flask is opened: it has no foreign odor (except a slight chlorine odor) and no foreign taste (except a slight chlorine taste). Gas: Combustible gas—Acetylene or hydrogen. Perform the test with the test solution and the standard solution as directed under the Atomic Absorption Spectrophotometry according to the following operating conditions: the absorbance of the test solution is not more than that of the standard solution (not more than 1 mg/L). (8) Heavy metals⎯Proceed with 30 mL of Water according to Method 1 and perform the test. Perform the test with the test solution and the standard solution as directed under the Atomic Absorption Spectrophotometry according to the following operating conditions: the absorbance of the test solution is not more than that of the standard solution (not more than 0.5 mL of nitric acid.01 mol/L silver nitrate VS consumed by using the following equation: it is not more than 200 mg/L. add 0.01 mg/L).0 mL of standard copper solution with water to make exactly 50 mL. After cooling. add 2 mL of sulfuric acid. and add ammonia TS until the color of the solution changes from yellow to green. separate the 4-methyl-2-pentanone layer and use this solution as the test solution. Prepare the control solution with 3. allow to stand for 2 to 3 minutes.0 mL of diluted sodium toluensulfonchloramide TS (1 in 5).50 mL of standard cadmium solution. Perform the test with the test so- . and use this solution as the standard solution. warm between 40 °C and 50 °C. add 0. and proceed in the same manner as for the test solution (not more than 10 mg/L). (12) Copper⎯Shake 50 mL of Water with 0.05 mg/L).5 mL of standard iron solution (not more than 0. and use this solution as the test solution.8 nm.3 g of griess-romijin’s nitrous acid TS. Wavelength: 213. 1 mL of a solution of sodium chloride (1 in 500) and 1 mL of a solution of ammonium amidosulfate (1 in 1000). Supporting gas—Air. Control solution⎯Pipet 2. proceed in the same manner as for the test solution.3 mg/L). and titrate with 0. allow to stand for 1 hour. Supporting gas—Air. After cooling. add slowly 10 mL of a solution of sodium hydroxide (2 in 5) and water to make 25 mL. Lamp: A zinc hollow cathode lamp. shake vigorously at ordinary temperature.5 mL of nitric acid. 10 mL of a solution of diammonium hydrogen citrate (1 in 4) and 2 drops of bromothymol blue TS. dilute 5. (6) Ammonium⎯Perform the test using 30 mL of Water as directed under the Ammonium limit Test. mix. The concentration (mg/L)of chlorineion 1000 = 0.0 mL of standard nitric acid solution.01 mol/L silver nitrate VS against a white background until a pale red-brown color no longer disappears in the aqueous layer (indicator: 0. Then stopper the flask loosely. and allow to stand between 20°C and 30°C for 50 minutes: the color of the solution is not more intense than the following control solution. Lamp: A cadmium hollow cathode lamp. combine each filtrate with the previously filtered chloroform extract.002 mol/L potassium permanganate VS.5 mL of nitric acid. 10 mL of a solution of diammonium hydrogen citrate (1 in 4) and 2 drops of bromothymol blue TS. (ii) Coliform bacilli⎯Preliminary test: Transplant 5 tubes containing 10 mL each of Water or 50 mL of Water into a fermentation tube.50 mL of standard lead solution with water to make exactly 50 mL. Wavelength: 283. shake for 30 seconds. and add 1 mol/L sodium hydroxide VS until the color of the solution changes to red. add exactly 1 mL of 0. Supporting gas—Air. Repeat the same operation twice or more with 5 mL of chloroform for the remaining aqueous layer. Calculate the amount of potassium permanganate consumed from the total amount. add 5 mL of sulfuric acid TS and 10. add 25 ml of methylene blue-sulfuric acid-sodium dihydrogenphosphate TS and 10 mL of chloroform.0 mL of Water. allow to stand for 1 hour. Add about 15 mL of liquefied nutrient agar kept at 45 °C. Add 10. containing twice or three . Supporting gas—Air. and use this solution as the standard solution.7. Part II lution and the standard solution as directed under Atomic Absorption Spectrophotometry according to the following operating conditions: the absorbance of the test solution is not more than that of the standard solution (not more than 1 mg/L).01 mol/L disodium dihydrogen diethylenediamine tetraacetate VS by using the following equation: it is not more than 300 mg/L.5 mL of nitric acid. Total hardness(as CaCO3 ) (mg/L)= (a − 1) × 1000 100 (15) Residue on evaporation⎯Evaporate to dryness 100 mL of Water on a water bath.31607 100 (17) Anionic surfactant⎯Take 200. proceed in the same manner as for (11) cadmium. and boil for 5 minutes. dry the residue at 105 °C for 2 hours. and titrate with 0. Then add 0. proceed in the same manner as for the test solution.0 mL of 0. and mix well while the culture medium is fluid. shake vigorously for 30 seconds. and proceed in the same manner as for the test solution (not more than 0. a (mL). Procedures: (i) General bacteria⎯Take 80 mL of Water into a sample bottle which has been autoclaved with 20 to 50 mg of powdered sodium thiosulfate pentahydrate in it. of 0. and use this solution as the test solution. and titrate immediately with 0. and allow to stand to separate the chloroform layer from the aqueous layer. and add chloroform to make exactly 50 mL. Lamp: A copper hollow cathode lamp. Add 50 mL of sulfuric acid-sodium dihyrogenphospate TS to the combined chloroform extract in the separatory funnel.01 mol/L magnesium chloride VS and 2 mL of ammonia-ammonium chloride buffer solution. (13) Lead⎯Shake 50 mL of Water with 0. add water to make exactly 200 mL. After cooling. and repeat the same operation twice with 10 mL of chloroform for the remaining aqueous layer.005 mol/L sodium hydroxide VS by using the following equation: it is not more than 10 mg/L. (14) Total hardness⎯Take 100.0 mL of standard sodium dodecylbenzene sulfonate solution. The amount(mg/L)of potassiumpermanganate consumed 1000 = (a − 10) × × 0. Wavelength: 324. add 0. pH 10. (16) Potassium permanganate⎯Take 100. View the solution downward or transversely: the color of the solution is not darker than the following control solution. and cool in a desiccator (silica gel): the residue is not more than 50 mg (not more than 500 mg/L). allow to stand to separate the chloroform layer from the aqueous layer. add 2 to 3 drops of phenolphthalein TS. place the dish upside down in an incubator between 35 °C and 37 °C for 22 to 26 hours. asporogenic aerobic or anaerobic bacilli capable of decomposing lactose and producing acids and gases) per 50 mL.0 mL of Water.sodium chloride indicator).1228 Monographs. Water contains not more than 100 general bacteria (viable bacteria capable of producing colonies on a nutrient agar medium) per mL. and transfer 1 mL of it to a petri dish.002 mol/L potassium permanganate VS consumed before and after the addition of 0. and add the chloroform extract to the separatory funnel into which the first chloroform extract was transferred.0 mL of Water. Perform the test with the test solution and the standard solution as directed under Atomic Absorption Spectrophotometry according to the following operating conditions: the absorbance of the test solution is not more than that of the standard solution (not more than 0.7 nm.5 mol/L sulfuric acid until the red color of the solution disappears.5 mg/L). a (mL). (18) General bacteria and coliform bacilli⎯When examined by the following procedures. Separately. and filter the chloroform layer through absorbent cotton. of 0. dilute 0. Lamp: A lead hollow cathode lamp. filter the chloroform extract through the same absorbent cotton. To this solution add 10 mL of a solution of diammonium hydrogen citrate (1 in 4) and 2 drops of bromothymol blue TS.3 nm.0 mL of 0. Gas: Combustible gas—Acetylene or hydrogen.002 mol/L potassium permanganate VS until a light red color persists for 30 seconds. Calculate the total hardnees of Water from the amount. Transfer the chloroform layer into another separatory funnel. Gas: Combustible gas—Acetylene or hydrogen.01 mol/L disodium dihydrogen ethylenediamine tetraacetate VS (indicator: about 40 mg of eriochrome black T. and count the colonies. Control solution– Pipet 10.1 mg/L).005 mol/L sodium hydroxide VS to decolorize the solution. and none of coliform bacilli (Gram-negative. allow to stand for 10 minutes with occasional shaking. add 1 mL of sodium salicylate-sodium hydroxide TS. add purified water for ammonium limit test to make 30 mL and proceed in the same manner as the test solution (not more than 0. using 30 mL of Purified Water as the test solution. (7) Heavy metals　Take 40 mL of Purified Water and add 2 mL of dilute acetic acid and 1 drop of sodium sulfide TS: no change occurs. Any Gram-negative. and incubate between 35 °C and 37 °C for 24 hours so as to isolate individual colonies.15 mL of standard ammonium solution.02 mol/L potassium permanganate VS and boil again for 10 minutes: the red color does not disappear. (9) Residue on evaporation　Evaporate 100 mL of Purified Water on a water-bath to dryness and dry the residue at 105 o C for 1 hour: the amount of the residue is not more than 1. or by the reverse osmosis-ultrafiltration (a reverse osmosis membrane. inoculate immediately the culture medium in a BGLB fermentation tube with 1 loopful of the material.10 mL of 0. colorless liquid. Water for Injection Water for Injection is water either prepared by distillation of Water or Purified Water.KP VIII 1229 times concentrated lactose broth. Confirmation test: If a gas is produced in the preliminary test.0 mL of Purified Water to a 50 mL beaker.02 ide (2 in 5) slowly and add water to make 25 mL: no yellow color develops. When Water for Injection is prepared by the reverse . It may be stored for a certain period. add 10 mL of dilute sulfuric acid. When prepare Purified Water. Packaging and Storage Preserve in tight containers. dissolve in 2 mL of sulfuric acid.5 mL of barium chloride TS: no change occurs. ultra-filtration). (5) Nitrogen from nitrite　Transfer 10 mL of Purified Water to a Nessler tube and add 1 mL of a solution of sulfanilamide in dilute hydrochloric acid (1 in 100) and 1 mL of N-(1-naphthyl)-N'-diethylethylenediamine oxalate TS: no pale red color develops. Sterile Purified Water Sterile Purified Water is sterilized Purified Water. Plastic containers for aqueous injections may be used. add 0. (8) Potassium permanganate-reducing substances　Take 100 mL of Purified Water. distillation or combination of these methods. colorless liquid.05 mL of bromothymol blue TS: no blue color develops. Cool.05 mg/L). (4) Nitrogen from nitrate　Transfer 2. If gas is evolved in the lactose broth fermentation tube within 48 hours. Identification test: If a gas is evolved in the confirmation test.1 mL of methyl red TS for acid or alkali test: a yellow to orange color develops. Inoculate lactose broth in a fermentation tube and a nutrient agar slant with the microorganisms from a typical colony or from not less than 2 subtypical colonies formed. Packaging and Storage Preserve in hermetic containers. streak immediately EMB plate medium or Endo’s plate medium with 1 loopful of the above cultured broth. Use immediately after purification. Cool. ion. is odorless and tasteless. an ultrafiltration membrane or a combined purification system of these membranes) of Purified Water. (2) Chloride　Take 50 mL of Purified Water and add 3 drops of nitric acid and 0. To 20 mL of Purified Water. Purified Water is the water purified by hyper-filtration (reverse osmosis. asporogenic bacillus indicates the presence of coliform bacilli. be careful to prevent microbial contamination. if it is in suitable containers preventing microbial growth. add 0. add 10 mL of water and transfer to a Nessler tube. and incubate between 35 °C and 37 °C for 45 to 51 hours: no gas production indicates the absence of coliform bacilli. 1 mL of a solution of sodium chloride (1 in 500) and 1 mL of a solution of ammonium sulfamate (1 in 1000) and evaporate on a water-bath to dryness. is odorless and tasteless. (6) Ammonium　Perform the test as directed under the Ammonium Limit Test.exchange. (3) Sulfate　Take 50 mL of Purified Water and add 0. Purified Water H2O: 18.5 mL of silver nitrate TS: no change occurs. and to be used for the preparation of injection. Purity Proceed as directed in the Purity under Purified Water.0 mg. and incubate between 35 °C and 37 °C. apply Gram staining to the colonies grown on the nutrient agar slant. boil. and incubate between 35 °C and 37 °C for 45 to 51 hours: no gas production indicates the absence of coliform bacilli. Prepare the control solution as follows: to 0. Description Sterile Purified Water is clear. add 10 mL of a solution of sodium hydrox- Sterility Test Take 500 mL of Sterile Purified Water and perform the test by the Membrane filtration method: it meets the requirements of the Sterility Test. Description Purified Water is a clear. Purity (1) Acid or alkali　Take 20 mL of Purified Water and add 0. A. Description Wheat Starch is a white mass or powder. preserved in a mixture of water and glycerin (1:1). from lateral view. small sized grains 2-10 µm in diameter. or quite rarely median sized simple grains.4 mL (not more than 20 ppm. Wheat Starch is practically insoluble in water or in dehydrated ethanol Identification (1) Under a microscope. spherical or polygonal. it may be stored for a certain period of time. Wheat Starch Wheat Starch consists of the starch granules obtained from the seeds of Triticum aestivum Linné (Gramineae). To 2. in determination of total organic carbon in a solution of sodium dodecylbenzenesulfonate (3.0 g of Wheat Starch.0. add 50. add 1 mL of glacial acetic acid and 0. allow to stand for 5 minutes and compare the color of these solutions against a white background: the color of the test solution is not darker than that of the control solution (not more than 10 ppm). and use the filtrate as the test solution. Bacterial Endotoxins Less than 0. To 30. Water for Injection preserved for the preparation of injections must be used immediately after preparation. its intersection point on hilum. and mix. disc like or quite rarely reniform. add 2 mL each of a solution of citric acid (1 in 5) and 0. mix. (3) To 1 mL of the pasty liquid obtained in (2).0 mL of the supernatant liquid. mix by shaking and allow to stand for 25 to 30 minutes in a dark place. Test tube .50 mg/L of total organic carbon.0 g of potassium iodide. often cleft on marginal portion visible. Transfer 10 mL each of these solutions into test tubes. However.5 to 1. add 50 mL of water. For the calibration of the apparatus. a black cross. from upper view. add water to make 20 mL. Condenser D. appears as large and small sized simple grains. instead of (8) Potassium permanganate-reducing substances. filter. narrowly ellipsoid or fusiform. Add 1 mL of starch TS and titrate the solution with 0.0 g of Wheat Starch in a non-metal vessel.05 mL of diluted iodine TS (1 in 10): a deep blue color develops.0 mL of standard iron solution. pH Place 5. (8) Total organic carbon　Perform the test with Water for Injection prepared by the reverse osmosisultrafiltration for the preparation of injections. usually.22 mg/L).1230 Monographs. Make the each solution clearly alkaline to litmus paper with strong ammonia water. Wheat Starch. hilum recognized as a long and slender cleft along with long axis. Funnel C. add water to make 20 mL each.5 g of Wheat Starch. centric hilum and striation indistinct or hardly distinct. For Water for Injection prepared by the reverse osmosis-ultrafiltration for the preparation of injections. add 15 mL of 2 mol/L hydrochloric acid TS. use potassium biphthalate (standard reagent).050 mg/L of total organic carbon and. if the purifying system of water is established for avoiding microbial contamination and its growth in preserved period. and allow to stand for 15 minutes: the pH of this solution is between 4. protected from microbial contamination. Use an apparatus which is efficient enough to detect not more than 0.0 mL of freshly boiled and cooled water. Part II osmosis-ultrafiltration. not less than 1. pasty liquid is formed.5 and 7. Purity (1) Iron—To 1. mix gently for 1 minute. (2) To 1 g of Wheat Starch. boil for 1 minute. and mix.1 mL each of mercaptoacetic acid. add 0. using an apparatus for detection of total organic carbon: it contains not more than 0.002 mol/L sodium thiosulfate VS until the color of the solution disappears.002 mol/L sodium thiosulfate VS consumed is not more than 1. and allow to cool: a subtle white-turbid. (2) Oxidizing substances—To 4. (3) Sulfur dioxide—(i) Apparatus Use apparatus shown in the figure. is observed when grains are put between two nicol prisms mixed at right angle to each other. and the color disappears by heating. Transfer 10 mL each of the test solution and the control solution in test tubes. calculated as hydrogen peroxide). Purity Proceed as directed in the Purity test under Purified Water. Boiling Flask B.25 EU/mL Packaging and Storage Preserve in suitable containers. and use this solution as the control solution.0 mL of water. take precaution against microbial contamination of the purifying system to get comfortable quality being equivalent to that of water prepared by distribution. mix by shaking for 5 minutes and centrifuge. add 25. large sized grains about 10-60 µm in diameter. perform the test for (8) Total organic carbon described below.70 mg/L. Perform a blank determination and make any necessary correction: the volume of 0. Place the flask in a water-bath. and cool. remove the funnel without interrupting the stream of carbon dioxide. Amount (ppm) of sulfur dioxide Amount (mL) of 0. and pass carbon dioxide through the whole system at a rate of 100 ± 5 mL per minute. Packaging and Storage Preserve in well-closed containers. and introduce through the opening into the flask 25 g of Wheat Starch.1 mol/L sodium hydroxide VS consumed = Amount (g) of Wheat Starch taken × 1000 × 3. Add 0. Calculate the amount of sulfur dioxide by applying the following formula: it is not more than 50 ppm.1 mL of bromophenol blue TS. with the aid of 100 mL of water. Pass cooling water through the condenser. and connect the funnel. 130 o C . Perform a blank determination and make any necessary correction. pour 80 mL of 2 mol/L hydrochloric acid TS into the funnel. Apply tap grease to the outside of the connection part of the funnel. close the tap of the funnel. accurately weighed.KP VIII 1231 (ii) Procedure Introduce 150 mL of water into the boiling flask. Close the tap of the funnel. and titrate with 0. Residue on Ignition Not more than 0. Transfer the contents of the test-tube with the aid of a little water to a wide–necked conical flask. and heat the mixture for 1 hour.6% (1 g).0% (1 g. in order to avoid losing sulfur dioxide.203 Loss on Drying Not more than 15. . 90 minutes). Heat in a water-bath for 15 minutes. and close the tap while several mL of the hydrochloric acid remains.1 mol/L sodium hydroxide VS until the color changes from yellow to violet-blue lasting for at least 20 seconds. After 15 minutes. open the tap to introduce the hydrochloric acid into the flask. and place 10 mL of hydrogen peroxide-sodium hydroxide TS in the test-tube. Water-soluble substances. striate and slightly thickened at the edges. separate the fibers into two groups.10 g of Purified Absorbent Cotton. both spaces of 20 mm between the wires. (5).4 mm in diameter in the form of a cylinder 50 mm in diameter and 80 mm in depth. deprived of fatty matter and bleached. (6) Absorbency⎯Leave the submerged basket at the bottom of the water in (5) as it is for 3 minutes. while adding water to maintain the original volume.0 g of Absorbent Cotton in 0. 10 in the same horizontal position. Purity Obtain certain amount of Absorbent Cotton from different 10 parts of the same package and combine them to get the required amount.0 mm in length. (8) Neps and adhering impurities⎯Spread evenly about 1 g of Absorbent Cotton between two 10 cmsquare. (6). Lift the basket gently from the water.5 mol/L iodine TS for 1 minute and wash well with water: no colored filament is found. Purified Absorbent Cotton Purified Absorbent Cotton is the hair of the seed of Gossypium herbaceum Linné. keeping its side horizontal and allow to drain for 1 minute on the wire gauze of a sieve No. striate and slightly thickened at the edges. which is 200 mm deep: the time required for complete submersion is not more than 8 seconds. (7) and (8) under Absorbent Cotton. Other filaments. about 0. weigh both groups and determine the content of the short fibers: not more than 10%. Part II 5) Quasi Drugs Absorbent Cotton Absorbent Cotton is the hair of the seed of Gossypium herbaceum Linné. Dyes. (3) Dyes⎯Digest 10 g of Absorbent Cotton with 100 mL of ethanol. (4). Place 5 g of Absorbent Cotton in the basket. (2). Under a microscope.1232 Monographs. (3). (5) Submersion rate⎯Prepare a test basket. Filter the combined extracts and washings. flattened and twisted band. (2) Short fibers⎯Take 0. fine filament-like hair. transfer the cotton to the funnel and press out the water absorbed therein with a glass rod.0 mg.0 mm in length. deprived of fatty matter and bleached.0 g in mass.0 mm in length (short fibers) and the other consisting of fibers exceeding 6. Content (%) of the short fibers = W2 × 100 W1 +W2 W1 : Mass of the group of fibers exceeding 6.5 mm in diameter is not more than 5. Fluorescent whitening agents. 3. hold the basket on its side. free from adhering impurities. Wash the cotton with two 150 mL volumes of hot water and pressing the cotton after each washing. is odorless and tasteless.25% (5 g. (7) Other filaments⎯Dip 1. Evaporate the filtrate to concentrate. 12 mm above the surface of water between 24 o C and 26 o C and drop the basket gently into the water.0 g. or that of other species of the same genus (Malvaceae). Then place in a beaker and weigh: the mass of water absorbed is not less than 100. transfer to a weighing bottle and dry at 105 o C to constant weight: the amount of the residue is not more than 14. is odorless and tasteless. Purified Absorbent Cotton dissolves in ammonia copper TS and does not dissolve in ordinary solvents. Under a microscope. one consisting of fibers not exceeding 6. Description Purified Absorbent Cotton is white. Observe downward: a yellow color develops. add 500 mL of water and boil gently for 30 minutes. made of copper wire. Neps and adhering impurities⎯Proceed as directed in the Purity (1). Absorbent Cotton dissolves in ammonia copper TS and does not dissolve in ordinary solvents. Perform a blank determination and make any necessary correction. fine filament-like hair. (1) Acid or alkali⎯Add 100 mL of freshly boiled and cooled water to 10 g of Absorbent Cotton. (2) Water-soluble substances⎯To 5 g of Absorbent Cotton. Ash Not more than 0. colorless. transparent plates and examine neps and adhering impurities (fragments of rinds and seeds): the total number of the fragments more than 2. Description Absorbent Cotton is white. Purity (1) Acid or alkali. Pour the extract through a funnel into another vessel. soft. soft. press out and transfer 50 mL of the extracts to a Nessler tube. or that of other species of the same genus (Malvaceae). Absorbency. Purified Absorbent Cotton is hollow. flattened and twisted bans. Add 1 drop of methyl orange TS to 25 mL of the extracts: no red color develops. but neither a blue nor a green color develops. Packaging and Storage Preserve in well-closed containers. (4) Fluorescent whitening agents⎯Irradiate Absorbent Cotton with ultraviolet light in a dark place: no fluorescence is perceptible on the surface. Absorbent Cotton is hollow. proceed as directed in the Ash under Crude Drugs Test). . carefully selected. digest and add 3 drops of phenolphthalein TS to make 25 mL of the extracts: no red color develops. striate and slightly thickened at the edges. Packaging and Storage Preserve in tight containers impervious to any microbe.5 g of Sterile Purified Absorbent Cotton (whole amount if not more than 0. filamentary hair.25% (5 g. press out and transfer 50 mL of the extracts to a Nessler tube.5 g) as directed in the Sterility test under Sterile Absorbent Gauze. Pour the extract through a funnel into a 1000mL flask. (6) Submersion rate⎯Prepare a test basket. Under a microscope. . but neither a blue nor a green color develops. Wash the beaker with a small amount of water. Description Sterile Purified Absorbent Cotton is white. Absorbent Gauze Sterile Absorbent Cotton Description Sterile Absorbent Cotton is white soft. is odorless and tasteless. pressing after each washing. filter and add water to make 1000 mL.4 mm in diame- Sterile Absorbent Cotton is sterilized Absorbent Cotton. length and width. Ash Not more than 0. combine the washings with the residue in the weighing bottle and dry at 105 °C to constant weight: the residue is not more than 20. press out the water absorbed therein with a glass rod and wash Absorbent Gauze with two 250 mL volumes of boiling water. The amount of Absorbent Gauze is expressed in terms of its type. transfer the Absorbent Gauze to the funnel. Purity (1) Acid or alkali⎯Take 200 mL of the extract obtained in (2) and add 5 drops of phenolphthalein TS: no red color develops. (3) Dextrin or starch⎯Take 200 mL of the extract obtained in (2). soft. Packaging and Storage Preserve in tight containers impervious to any microbe. Sterility Test Proceed with about 0. Under a microscope.KP VIII 1233 W2 : Mass of the group of fibers not exceeding 6.0 mg. The Absorbent Gauze folded twice or more for special purposes may be expressed in terms of its folded type. Absorbent Gauze consists of non-fatty and wellbleached cotton cloth of plain weave using pure cotton threads obtained from hairs of the seed of Gossypium hirsutum Linné or other species of the same genus (Malvaceae).5 g) as directed in the Sterility test under Sterile Absorbent Gauze. is odorless and tasteless. flattened and twisted band. Sterility Test Proceed with about 0. proceed as directed in the Ash under Crude Drugs Test). (4) Dyes⎯Digest 10 g of Absorbent Gauze with 80 mL of ethanol. flattened and twisted band. Perform a blank determination and make any necessary correction. Purity Proceed as directed in the Purity under Absorbent Cotton. Take 200 mL of the test solution and add 2 drops of methyl orange TS: no red color develops. fine. length and width. Sterile Absorbent Cotton dissolves in ammonia copper TS and does not dissolve in ordinary solvents. Description Absorbent Gauze is a white cotton cloth. evaporate to concentrate and place the residue in a weighing bottle. Ash Not more than 0. Purity Proceed as directed in the Purity under Purified Absorbent Cotton. Absorbent Gauze is odorless and tasteless. proceed as directed in the Ash under the Crude Drugs Test). Sterile Purified Absorbent Cotton is hollow. Ash Not more than 0.0 mm in length. while adding water to maintain the original volume. 3. about 0. Sterile Absorbent Cotton is hollow. made of copper wire. fine. Combine the extract and the washing.5 g of Sterile Absorbent Cotton (whole amount if not more than 0. Observe downward: a yellow color develops. Sterile Purified Absorbent Cotton Sterile Purified Absorbent Cotton is sterilized Purified Absorbent Cotton. proceed as directed in the Ash under the Crude Drugs Test). (5) Fluorescent whitening agents⎯Irradiate Absorbent Gauze with ultraviolet light in a dark place: no fluorescence is perceptible on the surface. Transfer 400 mL of the filtrate to a beaker. add 2 drops of iodine TS: no red-purple to blue color develops. striate and slightly thickened at the edges. (2) Water-soluble substances⎯Place 20 g of Absorbent Gauze in 500 mL of water and boil gently for 15 minutes. Packaging and Storage Preserve in well-closed containers. filamentary hair.25% (5 g. Sterile Purified Absorbent Cotton dissolves in ammonia copper TS and does not dissolve in ordinary solvents.25% (5 g.0 g in mass. measure the length and the width of the net. no large amount . When it has no closely woven parts. Except the closely woven parts. Ash Not more than 0. In the case of the test for the growth of fungi. Part II ter in the form of a cylinder 50 mm in diameter and 80 mm in depth. smooth out the unnatural creases or tensions and measure the full width at more than 3 different locations. When it has closely woven parts at both edges in the length or width directions. resulting in an adhesive mass.25% (5 g. measure the width of folded state.25% (5 g.0 g of Absorbent Gauze in 0. stated size in width and express the mass in terms of g per square meter. Purity Proceed as directed in the Purity under Absorbent Gauze. Test number used in the Sterility Test is indicated in the following table.45 cm2 frame and average the results of more than 3 counts. which is 200 mm deep: the time required for complete submersion is not more than 8 seconds. When unrolled. When it has no closely woven parts. put into a test tube of 25 mm × 200 mm containing 60 mL each of fluid thioglycollate medium using an appropriate utensil and perform the test as directed under the Sterility Test. (1) Number of threads⎯Prepare a frame of 2. Adhesive Plaster Method of Preparation Adhesive Plaster consists of a mixture of carefully selected rubber.5 mol/L iodine TS for 1 minute and wash well with water: no colored filament is found. (5) Fold⎯Count the folding number of Absorbent Gauze folded twice and more for special purpose.54 cm × 2. Fold Absorbent Gauze into about a 10 cm2. Packaging and Storage Preserve in well-closed containers. Place 5 g of Absorbent Gauze in the basket. Sterile Absorbent Gauze Sterile Absorbent Gauze is the sterilized Absorbent Gauze. 1 m in length. Sterility Take Sterile Absorbent Gauze from package aseptically under an aseptic circumstances. When it has no closely woven parts in the length and width directions. (2) Mass⎯Weigh a piece of Absorbent Gauze. Description The surface of Adhesive Plaster is milky white and adheres well to the skin. 12 mm above the surface of water between 24 °C and 26 °C and drop the basket gently into the water. allow to stand at ordinary temperature for 4 hours in a desiccator. measure only the net. (7) Other filaments⎯Dip 1. Number of The number of the same products products sterilized simultaneously used for test 4 Less than 100 Not less than 100 and less than 500 10 20 Not less than 500 Packaging and Storage Preserve in tight containers impervious to any microbe. Purity Adhesive mass⎯The back of the fabric is free from adhesive mass. take about 1. a 200-mL Erlenmeyer flask can also be used. This adhesive mass is spreaded evenly on a fabric. proceed as directed in the Ash under Crude Drugs Test). resins. Count the integral number of the threads in 6. (3) Length⎯Place Absorbent Gauze on a flat plate. Texture Proceed as directed in the Texture under Absorbent Gauze Ash Not more than 0.1234 Monographs. measure the full length. zinc oxide and other substances. measure full length and full width. When it has closely woven parts at both edges in the direction of the length. hold the basket on its side. For Absorbent Gauze being used as folded twice or more for special purpose. measure only the net. (4) Width⎯Place Absorbent Gauze on a plate. For Absorbent Gauze being used as folded twice or more for special purposes. Description Sterile Absorbent Gauze is a white cotton cloth and is odorless and tasteless. measure the full width. the medium supports the substantial growth of the incubated microorganisms. When performing an efficient test of the medium under a condition without Sterile Absorbent Gauze.54 cm and set the thread of to the edge of the frame. both spaces of 20 mm between the wires.0 g of it (whole content in the case of less than 1 g) evenly from 5 different parts around the center volume. measure the length of folded state. previously saturated with the vapor above a saturated solution of sodium nitrate and weigh. proceed as directed in the Ash under the Crude Drugs Test). When it has closely woven parts at both edges in the direction of the width. Texture The texture requirements of Absorbent Gauze are as followings. Take the average of these measurements. eliminate the unnatural creases or tensions and measure the full length at the center line. mix with occasional shaking for 1 hour. Description The Bandage is in various length and width and threads per 2. pass a rubber roller.6 mm less than the declared width. allow to stand and use the supernatant solution as the Calcium Hydroxide Solution. fold back the free edge of the strip attached to the test plate at an angle of 180° and peel about 25 mm from the edge of the test plate. Using a pendulum-type testing machine. Cresol is sparingly soluble in water. calculate with the necessary correction. to a test plate made of phenol resin about 25 mm in width. the quantity of Bentonite Magma may be increased to not more than 400 mL. Microbial Limit When perform the test. Bandage is cut by the Cresol is a mixture of isomeric cresols. uniform paste is formed. Cresol dissolves in sodium hydroxide TS. 12 mm in standard width. no large amount of the adhesive mass remains on the skin. Packaging and Storage Preserve in tight containers. To 3 g of Calcium Hydroxide. Texture Adhesive Plaster is usually rectangular: the length is not less than 98% of the labeled length.KP VIII 1235 of the adhesive mass moves to the back of the next fabric. Tensile strength Cut strip parallel with the warp. add 1000 mL of cold purified water.14 Description Cresol is a clear. Preserve in light-resistant. 125 mm in length and 5 mm in thickness. Finally add enough Calcium Hydroxide Solution to make 1000 mL and shake well. Pull at the rate of 300 mm per minute and measure the maximum breaking load: the average of 10 measurements is not less than 7. twice over Adhesive Plaster at a rate of 300 mm per minute. At once. Gradually incorporate the remainder of the diluted Magma. 12 mm in standard width. nip firmly the free edge with the upper clamp and the test plate with the lower clamp. Packaging and Storage well-closed containers.45 cm2 are followed by the texture. length and width declared on the label. triturating until a smooth. Purity Proceed as directed in the Purity under Absorbent Gauze. calculate with the necessary correction. Cresol becomes dark brown by light or on aging. about 250 mm in length and apply quickly one end of the strip 12 mm in width and 125 mm in length. previously saturated with the vapor over a saturated sodium nitrite solution. When the width is narrower than the standard width. allow to stand at ordinary temperature for 4 hours in a desiccator. The length and width of Bandage are stated on the package. Mix the Calamine and Zinc Oxide intimately with Glycerin and about 100 mL of the diluted Bentonite Magma. Peel off successively at a rate of 300 mm per minute and measure the load in 4 trials at intervals of about 20 mm: the average is not less than 150 g. Calamine Lotion Method of Preparation Calamine 80 g Zinc Oxide 80 g Glycerin 20 mL Bentonite Magma 250 mL Calcium Hydroxide Solution a sufficient quantity ⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯ To make 1000 mL Dilute the Bentonite Magma with an equal volume of Calcium Hydroxide Solution. colorless or yellow to yellow-brown liquid. When the width is narrower than the standard width. . about 200 mm in length. When removed from the skin. Texture Its length is not less than 98% of that declared on the label and its average width measured 5 points in an appropriate interval is not more than 1. 2 or 3 Absorbent Gauze. Using a pendulum-type testing machine. Cresol is miscible with ethanol or with ether. Adhesive strength Cut a strip parallel with the warp. set the target distance to 150 mm and nip firmly with a clamp whose width is between 25 mm and 50 mm. has a phenol-like odor. A saturated solution of Cresol is neutral to bromocresol purple TS. previously kept in a thermostat at 37 °C for 30 minutes. number of threads under Absorbent Gauze. 850 g in mass. C7H8O: 108. Cresol Bandage Gauze Bandage Bandage is made of Type 1. Packaging and Storage Preserve in well-closed containers (each cut). Measure the width at 5 suitable separate locations of the plaster: the average of the 5 measurements is not less than 94% of the labeled width.54 cm2 and threads per 6. Leave in a thermostat at 37 °C for 30 minutes. pseudomonas and staphylococcus are not observed. If a more viscous consistency in the Lotion is desired.5 kg. Cresol is a highly refractive liquid. add 2 to 3 drops of phenolphthalein TS and 0. After complete saponification. heat on a water-bath by thorough stirring and continue the saponification. Purity (1) Hydrocarbons⎯Dissolve 1. has the odor of cresol. add 5 mL of water and shake: the solution is clear.50 mL of Saponated Cresol Solution with 10 mL of neutralized ethanol.60 vol% of cresol.10 mL of 1 mol/L hydrochloric acid VS: no red color is observed. Identification Take 0. not Packaging and Storage tight containers. flocculent precipitate is produced.005 mol/L sulfuric acid and 1. Purity (1) Alkali⎯Mix 0. has the odor of cresol. in required quantity for saponification. add a saturated solution of sodium chloride and allow to stand for more than 3 hours with occasional shaking. exactly measured. using the distillate in the Purity (3). Cresol Solution Cresol Solution contains not less than 1. Saponated Cresol Solution Saponated Cresol Solution contains not less than 42 vol% and not more than 52 vol% of cresol.0 mL of Saponated Cresol Solution. until the distillate measures 90 mL. in a sufficient quantity of Water or Purified Water. The volume (mL) subtracted 3 (mL) from the oil layer measured represents the amount (mL) of Cresol. add 30 mL of water. Distil into a Cassia Method of Preparation Cresol 500 mL Vegetable oil 300 mL Potassium Hydroxide a suitable quantity Water or Purified Water a sufficient quantity ⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯ To make 1000 mL Dissolve Potassium Hydroxide. Allow to stand for 1 to 2 minutes with gentle shaking to combine the separated oil drops with the oil layer.0 mL of 0.0 mL of Cresol in 60 mL of water: the solution shows no more turbidty than that produced in the following control solution. Identification Proceed as directed in the Identification under Cresol. add 40 g of sodium chloride and 3 mL of dilute sulfuric acid. add a sufficient quantity of Ethanol. A corresponding amount of Sodium Hydroxide may be used in place of Potassium Hydroxide. Preserve in light-resistant. After cooling to 15 o C . Shake often the Cassia flask in warm water to dissolve the sodium chloride and allow to stand for 15 minutes. add this solution to vegetable oil.0 mL of barium chloride TS and after thorough shaking.25 vol% and not more than 1. viscous liquid. (2) Sulfur compounds⎯Transfer 20 mL of Cresol in a 100-mL Erlenmeyer flask. Distilling Range less than 90%. but neither brown nor dark tint.041. Saponated Cresol Solution is alkaline. mix with shaking. Between 196 o C and 206 o C . . (i) Take 5 mL of the test solution and add 1 to 2 drops of ferric chloride TS: a blue-purple color develops. filter and perform the following tests using the filtrate as the test solution. (ii) Take 5 mL of the test solution and add 1 to 2 drops of bromine TS: a pale yellow.1236 Monographs. yellow solution.032 and 1. Description Cresol Solution is a clear or slightly turbid. Saponated Cresol Solution is miscible with water. allow to stand for 5 minute. (2) Unsaponifiable matter⎯Take 1.5 mL of the oily layer obtained in the Assay. Description Saponated Cresol Solution is yellowbrown to red-brown. stir thoroughly until the mixture becomes clear and add sufficient Water or Purified water to make 1000 mL. Packaging and Storage Preserve in tight containers. if necessary. place a piece of moistened lead acetate paper on the mouth of the flask and warm for 5 minutes on a water-bath: the lead acetate paper may develop yellow. Specific Gravity 20 d 20 : Between 1. Draw off the water from the condenser and continue the distillation until water vapor begins to come out of the tip of the condenser. Assay Transfer exactly 200 mL of Cresol Solution to a 500-mL distilling flask. and connect distilling apparatus with the distilling flask. Method of Preparation Saponated Cresol Solution 30 mL Water or Purified Water a sufficient quantity ⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯ To make 1000 mL Prepare by mixing the above ingredients. add Cresol. add 6. previously warmed. Part II Identification Take 5 mL of a saturated solution of Cresol and add 1 to 2 drops of dilute ferric chloride TS: a blue-purple color develops. flask which contains 30 g of powdered sodium chloride and 3 mL of kerosene. with ethanol or with glycerin. Control solution⎯Take 54 mL of water. 0 mL of diluted hydrochloric acid (1 in 2).0 mL of this solution. (4) The colored solution obtained in the Assay (3) has a red-purple to purple color. (2) The colored solution obtained in the Assay (2) has a red color. Assay Transfer exactly 5 mL of Saponated Cresol Solution. connect the distilling apparatus with the distilling flask and distil into a Cassia flask which contains 30 g of powdered sodium chloride and exactly 3 mL of kerosene. Pipet 10.0 mL of Dental Iodine Glycerin and add diluted ethanol (3 in 10) to make exactly 50 mL. previously dried at 105 o C for 4 hours and dissolve in diluted ethanol (3 in 10) to make exactly 50 mL.0% and not more than 11. 40 g of sodium chloride and 3 mL of dilute sulfuric acid. The volume (mL) subtracted 3 (mL) from the oil layer measured represents the amount (mL) of cresol. add water to make exactly 200 mL and use this solution as the test solution. Preserve in light-resistant.90). Dental Iodine Glycerin has odor of iodine. Assay (1) Iodine—Pipet 5. pipet 7 mL each of the water layers and to each add 1. Separate the chloroformhexane layer and filter through absorbent cotton. Allow to stand for 1 to 2 minutes with gentle shaking and combine the separated oil drops with the oil layer. Add 200 mL of water. holding the pipet vertically for 15 minutes to draw off the solution into the flask. Draw off the water from the condenser and continue the distillation until water vapor begins to come out of the tip of the condenser. Determine the absorbances. Pipet 5. Filter through absorbent cotton.1% of zinc sulfate (ZnSO4·7H2O: 287. add 1 mL of a solution of cupric chloride in ethanol (1 in 10) and shake: a blue color is observed (glycerin).0 mL of this solution. Packaging and Storage tight containers. Filter and distil exactly 50 mL of the filtrate: the distillate is not less than 43 mL at between 196 o C and 206 o C . Pipet 5. Determine the absorbances. Description Dental Iodine Glycerin is a dark redbrown liquid. Draw off the water from the condenser and continue the distillation until water vapor begins to come out of the tip of the condenser. to a 500-mL distilling flask. Method of Preparation Iodine 10 g Potassium Iodide 8g Zinc Sulfate Hydrate 1g Glycerin 35 mL Purified Water a sufficient quantity ⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯ To make 100 mL Dissolve and mix the above ingredients. of the filtrates obtained from the test solution and the standard solution. at 512 nm as directed under the Ultraviolet-visible Spectrophotometry. not less than 7. Amount (mg) of iodine (I) = amount (mg) of Iodine RS × AT AS (2) Potassium iodide—Separate the water layers of the test solution and the standard solution obtained in (1). weigh accurately about 0.4 g of Potassium Iodide RS.5 g of Iodine RS and about 0. Then add 2 mL of sodium hydroxide TS. shake immediately and separate the chloroform-hexane layer [use the water layer in (2)]. Determine the absorption spectrum of this solution as directed under the Ultraviolet-visible Spectrophotometry: it exhibits maxima between 510 nm and 514 nm (iodine). 1 mL of sodium nitrite TS and 10 mL of a mixture of chloroform and hexane (2 : 1) and shake immediately. Dissolve 20 g of sodium chloride per 100 mL of the distillate.KP VIII 1237 (3) Cresol fraction⎯Transfer 180 mL of Saponated Cresol Solution to a 2000-mL distilling flask. respectively. AT and . AT and AS . add water to make exactly 200 mL and use this solution as the standard solution. to each add exactly 20 mL of a mixture of chloroform and hexane (2 : 1). allow to stand for 4 hours. add a saturated solution of sodium chloride and allow to stand for more than 3 hours with occasional shaking. Identification (1) The colored solution obtained in the Assay (1) has a red color.9% and not more than 1. add 10 mL of ethanol and mix.2% and not more than 8. Determine the absorption spectrum of this solution as directed under the Ultraviolet-visible Spectrophotometry: it exhibits maxima between 510 nm and 514 nm (potassium iodide). (3) Take 1 mL of Dental Iodine Glycerin in a glassstoppered test tube.0 mL each of the test solution and the standard solution.0% of Iodine (I: 126. Separately. Cool the condenser again and continue distillation for 5 minutes. Determine the absorption spectrum of this solution as directed under the Ultraviolet-visible Spectrophotometry: it exhibits maxima between 618 nm and 622 nm (zinc sulfate hydrate). add 300 mL of water and 100 mL of dilute sulfuric acid and distil with steam until the distillate becomes clear. After adding about 15 g of powdered calcium chloride for drying in small volumes with frequent shaking. Dental Iodine Glycerin Dental Iodine Glycerin contains not less than 9. until the distillate reaches 90 mL.58).8% of potassium iodide (KI: 166. Allow the Cassia flask to stand in warm water for 15 minutes to dissolve the sodium chloride with frequent shaking.00) and not less than 0. using a mixture of chloroform and hexane (2 : 1) as the blank and make any necessary corrections. allow to stand and collect the separated clear oil layer. Cool to 15 o C . Amount (mg) of zinc sulfate hydrate (ZnSO4 ·7H20)3 = amount (mg) of zinc in 10 mL of A standard zinc stock solution × T × 4. Packaging and Storage tight containers.1238 Monographs. Separately. add d-Camphor or dlCamphor and mix.5% of zinc oxide (ZnO: 81. respectively. Preserve in light-resistant. add water to make exactly 100 mL and use this solution as the test solution. Method of Preparation Zinc Oxide 200 g Liquid Paraffin 30 g White Ointment a sufficient quantity ⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯ To make 1000 g Prepare as directed under Ointments.397 AS Packaging and Storage tight containers. Pipet 3 mL each of tile water layers.0. Zinc Oxide Ointment contains not less than 18. Ethanol for Disinfection is miscible with water.9vol% and not more than 81.41). Alcohol for disinfection Ethanol for Disinfection contains not less than 76. colorless liquid. pipet 10 mL of standard zinc stock solution. AT and AS . Method of Preparation Ethanol 830 mL Purified water a sufficient quantity ⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯ To make 1000 mL Prepare by mixing the above ingredients. Description Ethanol for Disinfection is clear. d15 Purity Proceed as directed in the Purity under Ethanol. Pipet 5 mL of this solution. Preserve in light-resistant. Ethanol for Disinfection Preserve in light-resistant. add to each add 2 mL of boric acid-potassium chloride-sodium hydroxide buffer solution. Determine the absorbances. Zinc Oxide Ointment Dental Phenol with Camphor Method of Preparation Phenol 35g d-or dl-Camphor 65g ⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯ 100g Melt Phenol by warming. pH 10.5% and not more than 21.873. and has characteristic odor.07) at 15 o C . at 620 nm as directed under the Ultraviolet-visible Spectrophotometry.860 and 0. using the solution prepared in the same manner with 3 mL of water as the blank and make any necessary corrections. Ethanol for Disinfection is volatile. using a mixture of chloroform and hexane (2 : 1) as the blank and make any necessary corrections. of the filtrates obtained from the test solution and the standard solution. melt by warming. and 2 mL of zincon TS and water to make exactly 25 mL.4vol% (by specific gravity) of ethanol (C2H6O: 46. Identification Place 1 g of Zinc Oxide Ointment in a crucible. (2) Heat 1 mL of Ethanol with 1 mL of glacial acetic acid and 3 drops of sulfuric acid: the odor of ethyl acetate is perceptible. add diluted ethanol (3 in 200) to make exactly 1000 mL and use this solution as the standard solution. Amount (mg) of potassium iodide (KI) = amount (mg) of Potassium Iodide RS × AT AS (3) Zinc sulfate hydrate—Pipet 5 mL of Dental Iodine Glycerin and add diluted ethanol (3 in 10) to make exactly 50 mL. Ethanol for Disinfection burns with a pale blue flame on ignition. to each add 10 mL of a mixture of chloroform and hexane (2 : 1). Pipet 10 mL each of the test solution and the standard solution. Identification (1) Mix 1 mL of Ethanol with 2 mL of iodine TS and 1mL of sodium hydroxide TS: a pale yellow precipitate is produced. with the above ingredients. at 512 nm of directed under the Ultraviolet-visible Spectrophotometry. heat gradually raising the temperature until the mass is thoroughly charred and then ignite: a yellow color is observed and disappears . obtained from the test solution and the standard solution. Packaging and Storage tight containers. respectively. Part II AS . Specific Gravity 15 : Between 0. shake and allow to stand. Description Zinc Oxide Ointment is white. Description Dental Phenol with Camphor is colorless or pale red liquid. 5 mL of hydrochloric acid and add water to make exactly 100 mL. add 80 mL of water and add a solution of sodium hydroxide (1 in 50) until a small amount of precipitates begin to form in the solution. magnesium and other foreign inorganic matters⎯Place 2. pH 10. Add 5 mL of ammonia-ammonium chloride buffer solution. Add 6 mL of dilute hydrochloric acid and heat on a water-bath for 5 to 10 minutes: the solution is colorless and clear. place in a crucible. Assay Weigh accurately about 2 g of Zinc Oxide Ointment. Filter the solution. add 2 to 3 drops of potassium ferrocyanide TS: a white precipitate is produced (zinc oxide). heat gradually raising the temperature until the mass is thoroughly charred and then ignite until the residue becomes uniformly yellow and cool. add 10 mL of water to the filtrate and add ammonia TS until the precipitate first formed redissolves. To the residue. Add 2 mL each of ammonium oxalate TS and dibasic sodium phosphate TS to this solution: the solution remains unchanged or becomes very slightly turbid within 5 minutes. until the mass is thoroughly charred. Pipet exactly 20 mL of this solution.05 mol/L disodium ethylene diaminetetraacetate VS (indicator: 40 mg of eriochrome black T-sodium chloride indicator) Each mL of 0.071 mg of ZnO Packaging and Storage Preserve in tight containers. Ignite the mass strongly until the residue becomes uniformly yellow and cool. . melt by warming. and titrate with 0. shake well and filter. To the filtrate. melt by warming and heat gradually raising the temperature.0 g of Zinc Oxide Ointment in a crucible. add 10 mL of water and 5 mL of dilute hydrochloric acid.7. Dissolve the residue in 1 mL of water and 1.KP VIII 1239 on cooling. Purity Calcium.05 mol/L disodium ethylenediaminetetraacetate VS = 4. 1240 Monographs. Part II . KP VIII 1241 .