Previous pageNorgestrel Molecular formula: C21H28O2 Molecular weight: 312.5 CAS Registry No.: 797-63-7, 797-64-8 ((-) form), 6533-00-2 SAMPLE Matrix: blood Sample preparation: 1 mL Serum + 3 mL MTBE, vortex for 1 min, centrifuge at 1500 rpm for 5 min. Remove the organic layer and evaporate it to dryness under a stream of nitrogen at room temperature, reconstitute the residue in 100 jxL MeOH, inject an aliquot. HPLCVARIABLES Guard column: 18 mm long (Brownlee) Column: 300 X 3.6 10 |xm jxBondapak C18 Mobile phase: MeOH: water 80:20 Flow rate: 1 Detector: UV 254; RIA CHROMATOGRAM Retention time: 5.6 OTHER SUBSTANCES Extracted: metabolites, norgestimate KEYWORDS serum REFERENCE Wong, F.A.; Juzwin, S.J.; Tischio, N.S.; Flor, S.C. Determination of norgestimate in serum by automated high-performance liquid chromatography and subsequent radioimmunoassay. J.Liq.Chromatogr., 1995,28, 1851-1861 SAMPLE Matrix: bulk HPLCVARIABLES Column: 250 X 4 10 |xm LiChrosorb RP-18 Mobile phase: MeOH: water 70:30 Flow rate: 1 Injection volume: 25 Detector: UV 240 CHROMATOGRAM Retention time: 9 OTHER SUBSTANCES Simultaneous: impurities, norethindrone Interfering: ethinyl estradiol REFERENCE Gorog, S.; Herenyi, B. Analysis of steroids. XXXVIII. The use of high-performance liquid chromatography with diode-array UV detection for estimating impurity profiles of steroid drugs. J.Chromatogr., 1987, 400, 177-186 SAMPLE Matrix: culture medium Sample preparation: Extract culture medium twice with 2 volumes of ether, combine the extracts and evaporate them to dryness, reconstitute with MeOH, inject an aliquot. HPLCVARIABLES Column: 300 X 3.9 Techopak 10 C18 (HPLC Technology) Mobile phase: MeOH: water 70:30 Flow rate: 1.5 Detector: UV 240; Radioactivity CHROMATOGRAM Retention time: 5 OTHER SUBSTANCES Extracted: metabolites, norgestimate KEYWORDS tritium labeled REFERENCE Wild, M.J.; Rudland, RS.; Back, D.J. Metabolism of the oral contraceptive steroids ethynylestradiol and norgestimate by normal (Huma 7) and malignant (MCF-7 and ZR-75-1) human breast cells in culture. J.Steroid Biochem.Mol.BioL, 1991, 39, 535-543 SAMPLE Matrix: formulations Sample preparation: Centrifuge oil formulation at 30° at 2000 rpm for 30 min, filter (Whatman No. 1 paper), collect the last 4 mL of the nitrate. Dilute a 10 |xL aliquot to 10 mL with MeCN: water 60:40 containing 0.3% Tween 80, remove a 2 mL aliquot and add it to 1 mL 3.33 |xg/mL progesterone, vortex for 10 s, inject a 50 |xL aliquot. HPLCVARIABLES Column: 300 X 3.9 Novapak C18 Mobile phase: MeCN: water 60:40 Flow rate: 2 Injection volume: 50 Detector: UV 248 CHROMATOGRAM Internal standard: progesterone KEYWORDS oils REFERENCE Gao, Z.-H.; Shukla, A. J.; Johnson, J.R.; Crowley, W.R. Controlled release of a contraceptive steroid from biodegradable and injectable gel formulations: In vitro evaluation. Pharm.Res., 1995, 12, 857—863 SAMPLE Matrix: formulations Sample preparation: Oils. 1 mL Sample + 25 mL MeOH-.water 90:10, shake vigorously for 5 min, centrifuge, inject a 10 |JLL aliquot of the supernatant. Tablets. Grind a tablet to a fine powder, add 25 mL MeOH, sonicate for 5-10 min, filter (0.45 |min), discard first 5 mL of filtrate, inject a 10 |xL aliquot of the remaining filtrate. Suspensions (aqueous). Make up 5 mL to 50 mL with MeOH, filter (0.45 jjim), discard first 5 mL of filtrate, inject a 10 |xL aliquot of the remaining filtrate. HPLCVARIABLES Column: 250 X 4.6 5 |xm Zorbax ODS Mobile phase: MeOH: water 75:25 Flow rate: 1.5 Injection volume: 10 Detector: UV 240 CHROMATOGRAM Retention time: 5.9 Limit of detection: 5 |xg/mL OTHER SUBSTANCES Simultaneous: aspirin, benzyl alcohol, benzyl benzoate, boldenone, caffeine, caluster6ne, cortisone, dehydroepiandrosterone (UV 210), fluoxymesterone, formebolone, mesterolone (UV 210), methandriol (UV 210), methenolone acetate, methyltestosterone, mibolerone, nandrolone acetate, nandrolone propionate, norethandrolone, norethindrone, norethindrone acetate, oxandrolone (UV 210), oxymetholone, stanozolol, testolactone, testosterone acetate, testosterone propionate, trenbolone acetate Interfering: ethisterone, methandrostenolone, nandrolone, testosterone KEYWORDS oils; tablets; suspensions REFERENCE Walters, M.J.; Ayers, R.J.; Brown, D.J. Analysis of illegally distributed anabolic steroid products by liquid chromatography with identity confirmation by mass spectrometry or infrared spectrophotometry J.Assoc.OffAnaLChem., 1990, 73, 904-926 SAMPLE Matrix: microsomal incubations, mucosal fluid Sample preparation: Mucosal fluid. Extract 1 mL mucosal fluid twice with 5 mL diethyl ether, evaporate extracts to dryness, resuspend residue in 100 |xL MeOH, inject an aliquot. Microsomal incubations. Extract 2.5 mL microsomal preparation with 5 mL diethyl ether, proceed as before. HPLCVARIABLES Guard column: on-line guard column Column: 100 X 8 ixBondapak radial compression module Mobile phase: MeOH: water 70:30 Flow rate: 1.5 Injection volume: 100 Detector: UV 240 CHROMATOGRAM Retention time: 6 OTHER SUBSTANCES Simultaneous: 3-ketonorgestimate, 17-deacetylnorgestimate, norgestimate REFERENCE Madden, S.; Back, D.J. Metabolism of norgestimate by human gastrointestinal mucosa and liver microsomes in vitro. J.Steroid Biochem.Mol.Biol., 1991, 38, 497-503 Inc. 18 (D(-)) KEYWORDS chiral REFERENCE Lamparczyk.A.water 50:50 Flow rate: 2 Detector: UV 243 CHROMATOGRAM Retention time: 6. 668. RK.0 . J.. norethindrone acetate. A130 SAMPLE Matrix: solutions Sample preparation: Inject an aliquot of a 10 |xg/mL solution. HPLC VARIABLES Column: 150 X 4.6 Supelco ODS Mobile phase: MeCN: water 25:75 containing 14 mM cyclodextrin Column temperature: 0 Flow rate: 1-3 Injection volume: 20 Detector: UV 240 CHROMATOGRAM Retention time: 16 (D(+)).SAMPLE Matrix: solutions HPLC VARIABLES Column: 50 X 4. norethindrone. 1996. norethynodrel acetate REFERENCE Supelco Catalog. Supelco.. H. Effect of temperature on separation of norgestrel enantiomers by high-performance liquid chromatography. Nowakowska.Chromatogr. Bellefonte PA.. 1994.6 5 |xm Supelcosil LC-18 Mobile phase: MeOH: THF: water 10:20:70 Flow rate: 2 Injection volume: 20 Detector: UV 220 CHROMATOGRAM Retention time: 5.6 10 ^m Partisil C-18 ODS-3 Mobile phase: MeCN-. J. HPLCVARIABLES Column: 250 X 4.5 OTHER SUBSTANCES Simultaneous: ethinyl estradiol. p. Zarzycki. 413-417 SAMPLE Matrix: solutions Sample preparation: Direct injection. Brinkman. In vitro evaluations of transdermal levonorgestrel.. Farjam.6 10 jxm Nucleosil C18 Mobile phase: MeCN:THF: water 12. 78. D. F..Chromatogr.R. J.7 Flow rate: 1 Detector: UV 240 .. Frei.4:64. R.water 50:50 Flow rate: 2 Detector: UV 243 CHROMATOGRAM Retention time: 6. A.. Transdermal delivery of levonorgestrel IV: Evaluation of membranes.A.6 10 jim Partisil ODS-3 C18 Mobile phase: MeCN-. 1989..W.R.A. trenbolone (at UV 340) REFERENCE Haasnoot.. Catz. 489.Pharm. 6. P. A. 1989. R..KEYWORDS see also J. J. Drug Des. Heller. 157-171 SAMPLE Matrix: solutions HPLCVARIABLES Column: 250 X 4.Deliv.R. 4 9 60 SAMPLE Matrix: solutions HPLCVARIABLES Column: 250 X 4.Pharm. 1990. 477-480 SAMPLE Matrix: solutions HPLCVARIABLES Guard column: Chromsep reverse phase guard column (Chrompack) Column: 100 X 3 5 |xm Chromspher glass column Mobile phase: MeCN: water 35:65 Flow rate: 0...4 Detector: UV 247 CHROMATOGRAM Retention time: 20 OTHER SUBSTANCES Simultaneous: nandrolone. U. 477 REFERENCE Catz. Okagaki. D. Friend. Determination of p-19-nortestosterone and its metabolite a-19-nortestosterone in biological samples at the sub parts per billion level by high-performance liquid chromatography with on-line immunoaffinity sample pretreatment. M..0 REFERENCE Friend.Sci. 1989. P. Schilt. Hamers.. J.. W. 78. Huf.Sci.9:22. Chromatogr. mestranol. Phillips.6 5 \xm LiChrosorb Si 60 Mobile phase: Hexane: dioxane: isopropanol 95: 3:2 Flow rate: 1 Detector: UV 254 CHROMATOGRAM Retention time: 13 OTHER SUBSTANCES Simultaneous: estrone. Szepesi.6 jmBondapak C18 Mobile phase: Dioxane: water 50:50 (Caution! Dioxane is a carcinogen!) Flow rate: 1.W. 1988. 32. M. .. Szeleczki. reconstitute in a small volume of MeOH. M. The affinity of norgestimate for uterine progestogen receptors and its direct action on the uterus. I. evaporate to dryness. Hahn. extract medium twice with 2 volumes of diethyl ether. norethindrone acetate REFERENCE Gazdag.. G. inject an aliquot.S..L. Hetyei. J..4 Detector: UV 254 OTHER SUBSTANCES Simultaneous: norgestimate REFERENCE Killinger. Contraception. norethindrone.. 83-94 SAMPLE Matrix: solutions HPLCVARIABLES Column: 250 X 4.. A. ethinyl estradiol... Fabian-Varga. 311-319 SAMPLE Matrix: tissue Sample preparation: Incubate endometrial tissue with buffer. norethindrone.. 95-107 SAMPLE Matrix: solutions HPLCVARIABLES Column: 250 X 4. II. G. Szepesi. N. J. 454. 1988. Selection of high-performance liquid chromatographic methods in pharmaceutical analysis. D. Selection of high-performance liquid chromatographic methods in pharmaceutical analysis. McGuire. remove tissue. norethindrone acetate KEYWORDS normal phase REFERENCE Gazdag. Optimization for selectivity in reversed-phase chromatography. 454. J.CHROMATOGRAM Retention time: 13 OTHER SUBSTANCES Simultaneous: estrone. ethinyl estradiol.. Optimization for selectivity in normal-phase systems. J.Chromatogr. K. E. 1985. mestranol. D.5 Detector: UV 240 CHROMATOGRAM Retention time: 6 OTHER SUBSTANCES Simultaneous: metabolites. norgestimate and 3-ketodesogestrel by a human endometrial cancer cell line (HEC-IA) and endometrial tissue in vitro.9 Technopak 10 C18 Mobile phase: MeOH: water 70:30 Flow rate: 1. Rudland..BioL.HPLC VARIABLES Column: 300 X 3. norgestimate KEYWORDS endometrial tissue REFERENCE Wild.. 407-420 . M.J. Back. RS. 1993. J.J. 45. Metabolism of the oral contraceptive steroids ethynylestradiol.Steroid Biochem.Mol. : 72-69-5. amitriptyline. levomepromazine. 894-71-3 (HCI) SAMPLE Matrix: blood Sample preparation: 1 mL Serum + 500 |xL 750 mM pH 10 sodium bicarbonate/carbonate buffer + 50 |JLL IS in EtOH: water 50:50 + 8 mL heptane: isoamyl alcohol 98:2.03% phosphoric acid. Copenhagen) (8. shake at 250 cycles/min for 5 min.5 KH2PO4/phosphoric acid buffer. inject an aliquot of the aqueous phase. clozapine.V. citalopram Simultaneous: chlorprothixene. centrifuge at 1500 g for 10 min. zuclopenthixol Noninterfering: benzodiazepines Interfering: desmethyllevomepromazine KEY WORDS serum REFERENCE Olesen.5:2.6 . K. J.6 Supelco C18 Mobile phase: MeCN: buffer 45:55 (Buffer was 44 mM KH2PO4 containing 1. Linnet. adjusted to pH 2. centrifuge at 1500 g for 10 min. HPLCVARIABLES Column: 250 X 4. 675.4 CAS Registry No.. extract. HPLC VARIABLES Guard column: C18 Column: 100 X 8 10 |xm Resolve C8 (Waters) Mobile phase: MeCN: MeOH: 56 mM ammonium acetate :1 M ammonium hydroxide 100: 10:4. 1996.33) OTHER SUBSTANCES Extracted: metabolites.Chromatogr.) Flow rate: 1.5 with phosphoric acid. Discard the organic layer. Remove the organic layer and add it to 150 |xL 22 mM pH 2.5 Injection volume: 65 Detector: UV 240 CHROMATOGRAM Retention time: 9.Nortriptyline Molecular formula: C19H21N Molecular weight: 263. flupenthixol.B.73 Internal standard: l-(3-(dimethylamino)propyl)-l-(p-chlorophenyl)-l. clomipramine. 83-88 SAMPLE Matrix: blood Sample preparation: 1 mL Plasma + doxepin + NaOH + hexane: isoamyl alcohol 98:2.3-dihydroisobenzofuran-5-carbonitrile (LU 10-202) (Lundbeck. Remove the organic phase and add it to 0. inject a 65 JJLL aliquot of the aqueous layer. perphenazine. Simplified high-performance liquid chromatographic method for the determination of citalopram and desmethylcitalopram in serum without interference from commonly used psychotropic drugs and their metabolites. O. shake at 250 cycles/min for 5 min. freeze in dry ice/EtOH. extract.5 mL/L triethylamine. haloperidol. freeze in dry ice/EtOH. nordiazepam.Pharmacol. dothiepin.Flow rate: 2.. 36-41 . nordothiepin. norclomipramine. haloperidol... diazepam. nortriptyline. doxepin. chlorpromazine. Paton. nordoxepin.5 Detector: UV 220 CHROMATOGRAM Retention time: 31 Internal standard: doxepin (11. imipramine.. inject a 50 JJLL aliquot of the organic layer. fluphenazine. maprotiline. HPLCVARIABLES Guard column: 10 X 4. Chaleby.T. lorazepam.6 Spherisorb S5 SCX (sulfopropyl-bonded silica) cation exchange Mobile phase: 35 mM ammonium perchlorate in MeOH adjusted to an apparent pH of 6.5 Injection volume: 50 Detector: UV 215 CHROMATOGRAM Retention time: 9 Internal standard: nortriptyline hydrochloride OTHER SUBSTANCES Extracted: clozapine Simultaneous: amitriptyline. K. remoxipride. P. clomipramine. 17-21 SAMPLE Matrix: blood Sample preparation: 200 \xJL Plasma or serum + 100 jxL 2 M pH 10.A. S. fluoxetine. mianserin. A. paroxetine. flunitrazepam. J. vortex for 30 s. Hughes. trazodone Noninterfering: carbamazepine. clonazepam.6 Tris buffer + 200 IJiL MTBE.. serum. Biomed. fluvoxamine. fluoxetine. norfluoxetine. C. Gad.Chromatogr. nortriptyline is IS REFERENCE McCarthy. centrifuge at 9950 g for 3 min..6 SCX-10C5 (Hichrom) Column: 150 X 4. sulpride. Steady-state kinetics of fluoxetine and amitriptyline in patients treated with a combination of these drugs as compared with those treated with amitriptyline alone. 9.6) OTHER SUBSTANCES Extracted: amitriptyline. D. 35. 1995. theophylline Interfering: sertraline KEYWORDS plasma. Raines. A. norfluoxetine KEY WORDS plasma REFERENCE el-Yazigi.7 with 100 mM NaOH in MeOH Flow rate: 1.CHn. thioridazine. Measurement of clozapine and norclozapine in plasma/serum by high-performance liquid chromatography with ultraviolet detection.. 1995. warfarin. disopyramide. methocarbamol. sulfinpyrazole. terfenadine. phenylbutazone. glipizide. clobazam. tetrazepam. re-equilibrate for 30 min. haloperidol. ritodrine. clonazepam. medifoxamine. triazolam. quinupramine. desipramine. protriptyline. droperidol. lorazepam. cicletanine. nialamide. carbamazepine. metoprolol. omeprazole. atenolol. doxylamine. dextropropoxyphene. dextromoramide. centrifuge at 2800 g for 5 min.) (At the end of each session wash the column with water for 1 h and MeOH for 1 h. chlorpheniramine. hydroxyzine. benazepril. nicardipine. pyrimethamine. bumadizone. zolpidem. ketamine. floctafenine. aconitine. reconstitute the residue in 100 fxL mobile phase. imipramine. niflumic acid. loprazolam. dextromethorphan. hydroxychloroquine. iproniazid. prazepam. strychnine. estazolam. ketoprofen. chlorpromazine. fenfluramine. alpidem. Iisinopril. quinidine. nitrazepam. nalbuphine. medazepam. loratadine. oxprenolol. pipamperone. zorubicine . zopiclone. carbinoxamine. mexiletine. centrifuge at 2800 g for 10 min. prazosin. tolbutamide. chlorambucil. fluphenazine. clonidine. alimemazine. pentazocine. betaxolol. tianeptine. thiopental. secobarbital. chlorpropamide. buspirone. diazoxide. benzoylecgonine. cyclizine. amoxapine. sultopride. buprenorphine. debrisoquine. metoclopramide. naproxen. cocaine. levomepromazine. sulpride. diazepam. fentiazac. celiprolol. nitrendipine. toloxatone. proguanil. cyamemazine. clozapine. midazolam. propafenone. cycloguanil. methadone. penbutolol. flunitrazepam. mianserine. tiapride. naltrexone. ramipril. thioridazine. colchicine. naloxone. clemastine.9 4 \xm NovaPack C18 Mobile phase: MeOH:THF:buffer 65:5:30 (Buffer was 0. trazodone. minoxidil. (Buffer was saturated ammonium chloride solution 25% diluted with water. sulindac. tetracaine.SAMPLE Matrix: blood Sample preparation: 2 mL Whole blood or plasma + 2 mL buffer + 5 mL chloroform: isopropanol: n-heptane 60:14:26. oxazepam. melphalan.68 g/L (10 mM (sic)) KH2PO4 adjusted to pH 2. mephenesin. tofisopam. demexiptiline. amodiaquine. chlormezanone. vinblastine. sotalol. tenoxicam. verapamil. inject a 50 |xL aliquot of the supernatant.6 with concentrated orthophosphoric acid. vincristine. cetirizine. thioproperazine. flecainide. carteolol. mephentermine. nizatidine. ranitidine. quinine. terbutaline. mepivacaine. suriclone. alminoprofen. acepromazine. chlordiazepoxide. fluvoxamine.) HPLCVARIABLES Column: 300 X 3. dipyridamole. metformin. bromazepam. dosulepine. chloroquine. fenoprofen. mefenamic acid. piroxicam. nifedipine. loperamide. temazepam. acenocoumarol.28 Limit of detection: <120 ng/mL OTHER SUBSTANCES Extracted: acebutolol. amisulpride. cibenzoline. ephedrine. aceprometazine. cytarabine. viloxazine. lidocaine. trifluperidol. trifluoperazine. astemizole. flumazenil.8 Injection volume: 50 Detector: UV 239 CHROMATOGRAM Retention time: 9. mefenidramine. methotrexate. triprolidine. pindolol. metapramine. glutethimide. carpipramine. moperone. dacarbazine. timolol. meperidine. glibornuride. ticlopidine.) Column temperature: 30 Flow rate: 0. lidoflazine. dihydralazine. benzocaine. clomipramine. adjusted to pH 9. metipranolol. brompheniramine. diltiazem. methaqualone. nadolol. diphenhydramine. propranolol. penfluridol. phenobarbital. ajmaline. doxepin. promethazine. bupivacaine. tiaprofenic acid. flurbiprofen. codeine. ibuprofen. albuterol. caffeine. glibenclamide.5 with 25% ammonia solution. clorazepate. reserpine. pimozide. chlorophenacinone. labetalol. nalorphine. nomifensine. shake gently horizontally for 10 min. alprenolol. morphine. procainamide. phenol. phencyclidine. opipramol. benperidol. acetaminophen. nimodipine. prilocaine. aspirin. Remove the lower organic layer and evaporate it to dryness under vacuum at 45°. procarbazine. histapyrrodine. cyproheptadine. yohimbine. moclobemide. loxapine. vindesine. bisoprolol. alprazolam. bepridil. Worldwide Monitoring) with 2 mL MeOH then 2 mL water. 1 mL Plasma + 1 mL 400 ng/mL protriptyline in water. A. Mangin. wash with 3 mL 750 mL/L methanol. 40. daunorubicin. Potential interference of cyclobenzaprine and norcyclobenzaprine with HPLC measurement of amitriptyline and nortriptyline: resolution by GC-MS analysis. centrifuge at 3000 rpm for 5 min.5 M NaOH and 4 mL 50 mL/L isopropanol in heptane to eluate.Forensic ScL. Systematic toxicological analysis using HPLC/DAD.7 5 |xm Supelcosil LC-PCN cyanopropyl Mobile phase: MeCN: MeOH: 10 mM pH 7. mix. 1995.74 g/L K2HPO4. tioclomarol.36 g/L KH2PO4 with 274 mL 1.. maprotiline. add to the SPE cartridge. wash with 3 mL water. 1995.5 mL 0. J. J. Turk. mix thoroughly. 218-224 SAMPLE Matrix: blood Sample preparation: Automated SPE by ASPEC system. 19. cyclobenzaprine Interfering: norcycyclobenzaprine KEYWORDS serum REFERENCE Wong. 254-262 SAMPLE Matrix: blood Sample preparation: 1 mL Serum + 500 |xL 250 |xg/mL protriptyline hydrochloride + 1 mL 500 mM NaOH + 4 mL toluene: n-hexane: isoamyl alcohol 77:22:3.. trimipramine. inject a 100 |xL aliquot of the aqueous phase. J. Condition a C18 Clean-Up SPE cartridge (CEC 18111. tropatenine KEYWORDS whole blood.. P. HPLCVARIABLES Column: 150 X 4. vortex. Koenig. E.C.6 LC-8-DB (Supelco) . mix for 10 min. inject a 50 |xL aliquot. plasma REFERENCE Tracqui. Kintz. separate.5). reconstitute the residue in 200 |xL MeOH. Add 0. HPLCVARIABLES Guard column: LC-8-DB (Supelco) Column: 150 x 4.1) OTHER SUBSTANCES Extracted: amitriptyline. diclofenac. Remove the upper organic layer and evaporate it to dryness under a stream of air at 40°. Elute with three aliquots of 300 IxL 0.95 Internal standard: protriptyline (8.C. J.1 M phosphoric acid (pH 2. ToxicoL. P. Remove upper heptane phase and add it to 300 JJLL 0. Allow 5 min for phase separation.Interfering: amitriptyline.) Flow rate: 2 Injection volume: 50 Detector: UV 254 CHROMATOGRAM Retention time: 6. indomethacin.Anal. mefloquine.2 potassium phosphate buffer 60:15:25 (Prepare buffer by mixing 194 mL 1. fluoxetine. etodolac.1 M ammonium acetate in MeOH. 6 5 jxm Ultrasphere Octyl Mobile phase: MeCN: water 37. centrifuge at 1500 g for 5 min. nordiazepam. imipramine. trifluoperazine. Clin. fluoxetine. Automated HPLC assay of fluoxetine and norfluoxetine in serum. MHPG.R.5 with glacial acetic acid. dextromethorphan. hydrocodone. trichloromethiazide. warfarin Interfering: imipramine. cyclothiazide. SPE REFERENCE Nichols. propafenone. salicylic acid. mephentermine.5 containing 0. THC-COOH. elute with 250 |xL MeOH: 35% perchloric acid 20:1 by gravity (10 min) then centrifuge for 20 s to remove rest of eluant. J. norfluoxetine. mexiletine.. ethosuximide. inject a 50 |JLL aliquot of the eluate. propranolol. ethchlorvynol. encainide. methamphetamine. quinidine. ethacrynic acid. oxymorphone. theophylline. cotinine. temazepam. polythiazide. furosemide. methsuximide. pentobarbital. carbamazepine. benzocaine. 1994. verapamil Noninterfering: acetaminophen. maprotiline. thioridazine. 1 mL water. metharbital. cyclosporine. methadone. meprobamate. metoprolol. oxazepam. ephedrine. 1312-1316 SAMPLE Matrix: blood Sample preparation: Condition a 1 mL BondElut C18 SPE cartridge with 1 mL 1 M HCl. hydrochlorothiazide. thiazolam. norchlorimipramine. trazodone. methoxyphenteramine.. 1 mL MeOH. protriptyline. 700 \xL Serum + 50 |xL 5 (xg/mL trimipramine in 5% potassium bicarbonate + 700 |xL MeCN. benzthiazide. methylcyclothiazide.. amitriptyline. desalkylflurazepam. promazine. dicumerol. butalbital. and 1 mL 1% potassium carbonate. diazepam. sulfanilamide. diamorphine. norverapamil. amiodarone. clonazepam. fentanyl. lorazepam. maprotiline. acetylmorphine.5 mL/L 7% perchloric acid Flow rate: 1. monoacetylmorphine. chlorothiazide. phencyclidine. chlordiazepoxide. tocainide. trimipramine. bendroflumethiazide. hydroflumethiazide. 1 mL/min). Wash with 2 mL water and 1 mL MeCN. lidocaine. diphenhydramine. doxepin.5 g/L tetramethylammonium perchlorate and 0. normethsuximide.Chem. phenteramine. benzoylecgonine. phenytoin. cocaine. codeine. haloperidol. thiopental.) Flow rate: 2 Injection volume: 100 Detector: UV 228 CHROMATOGRAM Retention time: 4. add supernatant to SPE cartridge (at ca. methoxsalen. desipramine. vortex. phenylephrine. Charlson.M.5:62. morphine. HPLCVARIABLES Guard column: 15 mm 7 |jim Brownlee RP-8 Column: 150 X 4. oxycodone. chlorpromazine. glutethimide. ethanol. propoxyphene. methaqualone. ibuprofen. verapamil KEYWORDS plasma. hydroxyethylflurazepam. J. hydromorphone. fturazepam. 40.Mobile phase: MeCN: buffer 35:65 (Buffer was 10 mL/L triethylamine in water adjusted to pH 5.8 Internal standard: protriptyline (4) OTHER SUBSTANCES Extracted: acetazolamide. chlorimipramine. amphetamine. flecainide.5 Injection volume: 50 Detector: UV 215 .H. midazolam. valproic acid. primidone. nordoxepin. Lawson. pentazocine. G. prochlorperazine. amobarbital. HPLC VARIABLES Column: A Guard-Pak 10 |xm Resolve CN (Waters).6) Limit of quantitation: 5 ng/mL OTHER SUBSTANCES Extracted: amitriptyline.N. inject a 250 JULL aliquot of the supernatant onto column A with mobile phase A. 291-297 SAMPLE Matrix: blood Sample preparation: Add 10 |xL 20 |xg/mL oxaprotiline in MeOH to 990 JJLL plasma or serum.Chromatogr.CHROMATOGRAM Retention time: 7. maprotiline.. SPE REFERENCE Gupta. elute with mobile phase A for 6 min. column-switching REFERENCE Dolezalova.Liq. 50 mM ammonium phosphate. and 28 mM diethylamine. J. Elute column B with mobile phase B for 6 min and conduct analysis. J. fluoxetine. pH 2. B 150 X 3 7 jxm Separon SGX CN (Tessek) Mobile phase: A MeCN: water 3:97. B MeCN: buffer 26:74 (Buffer was 50 mM phosphoric acid. after 15 min elute column A onto column B with mobile phase B for 2 min. R. Inject 100 jxL plasma or serum onto column A with mobile phase A and elute to waste. desipramine. doxepin. Remove . protriptyline Interfering: imipramine KEYWORDS serum.. An improved solid phase extraction procedure for the determination of antidepressants in serum by column liquid chromatography.Chromatogr.55. On-line solid-phase extraction and high-performance liquid chromatographic determination of nortriptyline and amitriptyline in serum. 16. clomipramine. 579. When not in use flush column A with mobile phase A. backflush contents of column A onto column B with mobile phase B for 4 min. fluvoxamine.) Flow rate: 1 Injection volume: 250 Detector: UV 210 CHROMATOGRAM Retention time: 10 Limit of detection: 15-20 ng/mL OTHER SUBSTANCES Extracted: amitriptyline KEYWORDS serum. M. Every eight injections backflush column A with MeCN: water 70:30. centrifuge at 2500 g for 8 min. 1992.4 Internal standard: trimipramine (9. 1993. 2751-2765 SAMPLE Matrix: blood Sample preparation: 500 \xL Serum + 250 |xL 100 mM lauryl sulfate. trifluperidol KEYWORDS plasma. B MeOH: MeCN: 10 mM pH 6.6 5 |xm Nucleosil 100 CN Mobile phase: A MeOH: water 5:95. clomipramine. C.column A from circuit and re-equilibrate it with mobile phase A for 5 min.) Flow rate: 1. lorazepam.. B MeCN: MeOH: buffer 578:188:235 (Buffer was 10 mM K2HPO4 adjusted to pH 6. amitriptyline. fluvoxamine. After 15 min elute column A onto column B (foreflush) with mobile phase B. desipramine. fluvoxamine. After 2 min remove column A from the circuit. haloperidol. elute column B with mobile phase B. metoclopramide. perazine. 38. fluoxetine. S. oxazepam.8 with 85% phosphoric acid. chlordiazepoxide.5 Injection volume: 100 Detector: UV 214 CHROMATOGRAM Retention time: 14. Re-equilibrate column A with mobile phase A.Chem. nitrazepam.5 Internal standard: oxaprotiline (9. Chromatograph on column B with mobile phase B.6 5 |xm Hypersil CPS CN + 250 x 4. Clin. H.5) Limit of detection: 20 ng/mL OTHER SUBSTANCES Extracted: amitriptyline. elute with mobile phase A to waste. Hiemke. B 20 X 4. pimozide. Inject serum or plasma directly onto column A with mobile phase A.. clobazam.5 Injection volume: 100 Detector: UV 214 CHROMATOGRAM Retention time: 14. maprotiline . Wetzel.6 10 |xm Hypersil MOS C8. clozapine. monitor the effluent from column B. doxepin.6 10 jxm Hypersil MOS C8. clomipramine. diazepam. 1992. imipramine.6 5 [xm Nucleosil 100 CN Mobile phase: A MeOH: water 5:95. imipramine. spiroperidol. norfluoxetine Noninterfering: carbamazepine. B 20 X 4. HPLCVARIABLES Column: A 20 X 4. nordiazepam. flurazepam. maprotiline. Automated determination of fluvoxamine in plasma by columnswitching high-performance liquid chromatography.5) Limit of detection: 5-10 ng/mL OTHER SUBSTANCES Extracted: metabolites.8 potassium phosphate buffer 188:578:235 Flow rate: 1. serum. fluspirilene. desipramine.6 5 |xm Hypersil CPS CN + 250 x 4. 2082-2086 SAMPLE Matrix: blood Sample preparation: For each 1 mL plasma or serum add 10 ^L 14 jxg/mL trimipramine in MeOH.54 Internal standard: trimipramine (6. column-switching REFERENCE Hartter. HPLCVARIABLES Column: A 20 X 4. doxepin.. Fatmi. column-switching.6 K2HPO4. clozapine. vortex for 30 s. fluspirilene.2 potassium phosphate 85:15 Flow rate: 1. let stand at room temperature at 22° for 15 min. J. Evaporate under a stream of nitrogen at 45°. vortex. 1992.Noninterfering: chlordiazepoxide. centrifuge at 1900 g for 10 min.. evaporate at 45° in a vacuum . centrifuge at 1900 g for 5 min. reconstitute the residue in 250 fxL 40 mM sodium bicarbonate.8 carbonate buffer + 40 |JLL 5 |xg/mL maprotiline in 10 mM HCl + 5 mL 200 g/L ethyl acetate in n-heptane. serum. centrifuge at 1500 g for 10 min.A. S. add 6 mL ethyl acetate. derivatization. add 750 |xL acetone. haloperidol. Remove the organic layer and evaporate it to dryness under a stream of nitrogen at 45°.3 carbonate buffer and 25 |JLL 10 mg/mL dansyl chloride in MeCN.6 5 jxm Supelcosil LC-18-DB Mobile phase: MeCN: 10 mM pH 7. mix 10 min. perazine. spiroperidol. flurazepam. pimozide. allow to react at room temperature for 45 min. LOD can be lowered to 1 ng/mL with 3 injections onto column A before switching REFERENCE Hartter.6 M pH 9.H. Column switching and high-performance liquid chromatography in the analysis of amitriptyline. nitrazepam. Hiemke. R. vortex for 1 min. Take up residue in 50 jxL 1 M pH 10. HPLCVARIABLES Guard column: 15 X 3. mix by rocking for 10 min. 578. reconstitute in 1 mL mobile phase. diazepam.. oxazepam.7 Internal standard: nortriptyline OTHER SUBSTANCES Extracted: fluvoxamine Simultaneous: desipramine KEYWORDS plasma. Discard organic layer and evaporate aqueous layer at 45° in a vacuum centrifuge for 1 h. 101-107 SAMPLE Matrix: blood Sample preparation: 1 mL Plasma + 1 mL 0.Chromatogr. Remove organic layer and add it to 150 |xL 100 mM HCl. vortex for 1 min. inject a 100 |xL aliquot of the supernatant. vortex for 5 s. nortriptyline and hydroxylated metabolites in human plasma or serum. C..Chromatogr. centrifuge at 1500 g for 10 min. trifluperidol KEYWORDS plasma. 273-282 SAMPLE Matrix: blood Sample preparation: 1 mL Plasma + 100 |xL 1 M pH 7. 1992. Determination of fluvoxamine in human plasma by high-performance liquid chromatography with fluorescence detection. 574. add 20 jxL 10 mg/mL dansyl chloride in acetone. J.2 7 jxm NewGuard RP-8 (Brownlee) Column: 250 X 4. nortriptyline is IS REFERENCE Pullen. clobazam..5 Injection volume: 100 Detector: F (wavelengths not given) CHROMATOGRAM Retention time: 9. A. M. diazepam. HPLCVARIABLES Guard column: 20 mm long Pelliguard LC-8 40 |xm (Supelco) Column: 150 X 4.2 mL butylamine in 1 L 10 mM NaH2PO4. clomipramine.Chem. triazolam .B.) Flow rate: 1 Injection volume: 10 Detector: UV 254 CHROMATOGRAM Retention time: k' 2. metoprolol. desipramine. clovoxamine. pH adjusted to 3 with phosphoric acid. 1756-1761 SAMPLE Matrix: blood Sample preparation: 1 mL Serum + 3 |xL 20 ng/mL clobazam + 1 mL saturated sodium borate (adjusted to pH 11 with 6 M NaOH) + 5 mL n-hexane. sertraline Noninterfering: amitriptyline. desipramine.6 5 jim Supelcosil LC-18 Mobile phase: MeCN: 25 mM KH2PO4 75:25 containing 500 |xL/L orthophosphoric acid and 600 fxL/L n-butylamine Flow rate: 2 Injection volume: 25-40 Detector: F ex 235 em 470 (cut-off) CHROMATOGRAM Retention time: 14. lorazepam. tranylcypromine.F. chlordiazepoxide. Cooper..F. fenfiuramine. 1992. bupropion. thioridazine. clozapine. centrifuge at 3000 g for 10 min. moclobemide. protriptyline. fluoxetine. fluvoxamine.460 Internal standard: clobazam (k' 1.18 Internal standard: maprotiline (12. carbamazepine. loxapine.344) Limit of detection: 10 ng/mL OTHER SUBSTANCES Extracted: amitriptyline. Sensitive and selective liquid-chromatographic assay of fluoxetine and norfluoxetine in plasma with fluorescence detection after precolumn derivatization.8) OTHER SUBSTANCES Simultaneous: amoxapine. pindolol..6 C8 5 \xm (Supelco) Mobile phase: MeCN: buffer 50:50 (Buffer was 1.water 75:25. citalopram. maprotiline. reconstitute in 125 |JLL MeCN-. vortex.centrifuge for 20 min. doxepin. 38. nomifensine. haloperidol. Remove organic phase and evaporate to dryness under a stream of helium at 30°. Reconstitute in 20 |xL mobile phase. propranolol. cyclobenzaprine. trimipramine KEYWORDS plasma REFERENCE Suckow. clomipramine. trazodone. norfluoxetine. Zhang. T. centrifuge for 3-5 min. HPLCVARIABLES Column: 250 X 4. mianserin. atenolol. R. inject a 25-40 |xL aliquot.. clonazepam. Clin. flunitrazepam. mix 2 min. imipramine. inject a 10 |xL aliquot. nitrazepam. imipramine Simultaneous: alprazolam. Separation of tricyclic and tetracyclic antidepressants and their metabolites. Remove column A from circuit and wash with MeCN: water 60:40 for 6 min then with mobile phase A for 10 min. Clin.. Grossi. maprotiline... Automated determination of drugs in serum by column-switching high-performance liquid chromatography. Lucarelli. F. pH 7 Flow rate: A 0. HPLCVARIABLES Column: A 37-50 |xm 10 X 1. Rapid and simple high-performance liquid chromatographic determination of tricyclic antidepressants for routine and emergency serum analysis. B 150 X 4 TSKgel ODS-80TM (Tosoh) Mobile phase: A 50 mM pH 7. H.5. Elute column B with mobile phase B and monitor the effluent. 1989. containing 0. H.P. Mangiarotti.Chromatogr. mix. amoxapine. After 1. B 100 X 4 Techsphere 3CN (HPLC Technology) Mobile phase: A water. IV.. Yuki. B MeCN: 50 mM acetate buffer 60:40. C. monitor the effluent from column B. K.7 potassium phosphate 32... Nisi. Kanba. use gradient to determine metabolites REFERENCE Matsumoto. B MeCN: 100 mM pH 2.5 potassium phosphate. J. M..KEYWORDS serum REFERENCE Segatti. G.5 Corasil RP C18. B 0.. Kubo.. clomipramine.5:67. G. 536. 319-325 SAMPLE Matrix: blood Sample preparation: Inject 200 |xL serum onto column A and elute with mobile phase A for 10 min then back-flush column A onto column B with mobile phase B for 4 min. doxepin..8. trimipramine Interfering: imipramine KEYWORDS serum. 1991. inject a 250 |xL aliquot of this mixture onto column A and elute to waste with mobile phase A. H.. M.Chem. 453-456 SAMPLE Matrix: blood Sample preparation: 1 mL Plasma + 50 [xL MeOH: water 50:50 + 50 |xL 10 |xg/mL desmethyldoxepin in MeOH: water 50:50.9 Injection volume: 250 Detector: UV 215 .5 min backflush the contents of column A onto column B with mobile phase B. column-switching. 35. HPLCVARIABLES Column: A 40 X 4 TSKprecolumn PW (Tosoh). desipramine. Iri. S. Yagi.2 g/L sodium 1-heptanesulfonate Flow rate: 1 Injection volume: 200 Detector: UV 210 CHROMATOGRAM Retention time: 15 Limit of detection: 10 ng/mL OTHER SUBSTANCES Extracted: amitriptyline. haloperidol. amitriptyline Simultaneous: chloripramine. trimipramine Simultaneous: atropine. phenobarbital.5) Limit of detection: 5-10 ng/mL OTHER SUBSTANCES Extracted: metabolites. add to the SPE cartridge. morphine. desipramine. fluphenazine. 500 JULL Serum + 50 JULL 1 |xg/mL N-propionylprocainamide in 2. clonazepam. droperidol.0 Internal standard: N-propionylprocainamide (6) Limit of quantitation: 25 ng/mL OTHER SUBSTANCES Extracted: amitriptyline. chlorpromazine. ethinamate. Add 200 jxL 10 mM acetic acid and 5 mM diethylamine in MeOH to column. verapamil . phenytoin. I. High-performance liquid chromatographic determination of amitriptyline and its metabolites in human plasma. carbamazepine. reconstitute in 100 |xL mobile phase. ethinamate.2 Injection volume: 40 Detector: UV 254 CHROMATOGRAM Retention time: 14.5 mM HCl. naloxone. kanamycin.Chromatogr. quinidine. tobramycin. neomycin. chlorpropamide. prochlorperazine. propranolol.. D. trimeprazine Noninterfering: acetaminophen. amytal. valproic acid. ethosuximide.5 mM HCl 10:90. amoxapine. methotrexate. mephobarbital. ibuprofen. allopurinol. primidone. doxepin. Power. HPLCVARIABLES Guard column: Pelliguard LC-CN (Supelco) Column: 150 X 4. meprobamate. A. propoxyphene. promethazine. trifluoperazine. doxepin. methadone. hydrochlorothiazide. amikacin. plasma REFERENCE Dadgar. repeat. norpropoxyphene. protriptyline Noninterfering: tranylcypromine Interfering: cianopramine. procainamide. perphenazine. 99-109 SAMPLE Matrix: blood Sample preparation: Condition a Bond Elut C-18 SPE cartridge twice with MeOH and twice with water. clomipramine.. maprotiline. trimipramine KEYWORDS column-switching. flurazepam. thiopental. imipramine. chloramphenicol. bretylium. protriptyline. procaine.CHROMATOGRAM Retention time: 10. wash with 2 volumes 0. inject a 40 |JLL aliquot. nafcillin. codeine. gentamicin. desipramine. furosemide.0 phosphate buffer 58:14:28 Flow rate: 1. thioridazine. imipramine. wash with 1 volume MeOH: 2. Applications of column-switching technique in biopharmaceutical analysis. evaporate eluents to dryness under nitrogen at room temperature. caffeine. salicylic acid. 1987. lidocaine. methaqualone. chlordiazepoxide. disopyramide. prazepam. secobarbital. wash with 2 volumes water.1 M acetic acid. elute under vacuum. spironolactone. phenacetin.6 5 [xm Supelcosil LC-PCN Mobile phase: MeCN:MeOH: 10 mM pH 7. carisoprodol. J. let stand 1 min. phenylpropanolamine. hydroxyzine. loxapine. 416. salicylamide. theophylline. reserpine. meperidine.0 Internal standard: desmethyldoxepin (8. diazepam. butalbital. 313-316 SAMPLE Matrix: blood Sample preparation: 1 mL Serum + 1 mL 450 mM NaOH + 5 mL hexane: isopropanol 95:5. centrifuge 5 min. 448-455 SAMPLE Matrix: blood Sample preparation: 500 |xL Serum + 250 |xL di-iso-propyl ether: n-butyl alcohol 7:3 containing 800 ng/mL minaprine.5 Injection volume: 50 Detector: UV 240 CHROMATOGRAM Retention time: 6. 1987. HPLCVARIABLES Column: 100 X 3 octyl CP-tm-Spher C8 glass column (Chrompack) Mobile phase: MeCN: 500 mM NaH2PO4 35:65 adjusted to pH 2. Chromatographia. RD.Drug Monit. inject 50 |xL aliquot of top organic layer. Simple and practical high-performance liquid chromatographic assay of some tricyclic drugs. 1987.6 5 |xm Altex ultrasphere cyano Mobile phase: MeCN: THF: water: 2 M ammonium formate (pH 4.0) 700:100:195:5 Column temperature: 20 Flow rate: 1. 9. propafenone.2 with phosphoric acid Flow rate: 0. Ther. Inject a 20 |xL aliquot of the aqueous layer.-N. and amiodarone. shake for 2 min. diltiazem Also analyzed: amiodarone. Simultaneous quantitation of eight tricyclic antidepressants in serum by highperformance liquid chromatography. HPLCVARIABLES Guard column: 30 X 4.5) Limit of detection: 20 ng/mL OTHER SUBSTANCES Simultaneous: amitriptyline. W. verapamil. diltiazem.8 Injection volume: 20 Detector: UV 210 CHROMATOGRAM Retention time: 4.5 Limit of detection: 10 ng/mL . shake. haloperidol. Remove 4 mL of the organic layer and add it to 50 |JLL 200 mM HCl. verapamil KEYWORDS serum REFERENCE Mazzi. propafenone. Frade. centrifuge. SPE REFERENCE Lin. desipramine. centrifuge 2 min. shake for 5 min. haloperidol..6 5 |xm Brownlee cyano spheri-5 Column: 250 X 4. imipramine.KEYWORDS serum. clomipramine.5 Internal standard: minaprine (5. G. centrifuge. 24. HPLCVARIABLES Column: 250 X 4 Bio-Sil ODS-10 (Bio-Rad) Mobile phase: MeCN :pH 4. J.9) Limit of detection: 1 ng/mL OTHER SUBSTANCES Extracted: desipramine. Remove upper organic layer. lorazepam.0 with 6 M NaOH and store at 35-37°. 1652-1655 SAMPLE Matrix: blood Sample preparation: 500 jxL Plasma + 37 |JLL 2 |xg/mL IS in MeOH + 500 ^xL pH 10 borate buffer +1. Useful sample handlings for reversed phase high performance liquid chromatography in emergency toxicology. F.5 with orthophosphoric acid. S. inject a 50 |xL aliquot.5 mL hexane. plasma REFERENCE McCormick. shake for 10 min. Evaporate the organic layer to dryness under a stream of nitrogen..OTHER SUBSTANCES Simultaneous: amitriptyline.Chem.9 g KH2PO4 in 1 L adjusted to pH 4. chlorpromazine. centrifuge for 5 min. flurazepam. P.. add 0.. L.R. centrifuge for 5 min. propranolol. discard upper hexane layer. 1984. vortex for 2 min.) Column temperature: 45 Flow rate: 2... evaporate under a stream of nitrogen at 37°. Abi Khalil. Molle. Add 630 mL of this solution to 370 mL 106 g/L sodium carbonate solution. 30. Clin.4 Internal standard: U-31485 (6.) . procainamide. vortex briefly. chlordiazepoxide.Toxicol.8 g boric acid and 74. reconstitute in 100 IJLL MeOH. Quantification of alprazolam in serum or plasma by liquid chromatography.Clin. 23.6 g KCl in 1 L water. imipramine. doxepin KEYWORDS serum REFERENCE Van Damme. oxazepam.5 Injection volume: 100 Detector: UV 202 CHROMATOGRAM Retention time: 8. Prepare a solution of 61. vortex.5 mL water. 1985. M. J.ToxicoL. triazolam KEYWORDS serum. prazepam. Jatlow. inject a 100 jxL aliquot of the lower layer. extract with 10 mL toluene: isoamyl alcohol 99:1 for 10 min on a rotator. diazepam. thioridazine Interfering: alprazolam. amitriptyline. take up in 150 |xL mobile phase. Adjust pH to 10. (The borate buffer was prepared as follows. protriptyline Noninterfering: N-acetylprocainamide. Nielsen. caffeine.5 mL hexane: isoamyl alcohol 95:5.5 50 mM phosphate buffer 30:70 (Buffer was 6. 589-614 SAMPLE Matrix: blood Sample preparation: 2 mL Serum or plasma + 100 |JLL 1 |xg/mL IS in water + 0. Chem.water 65:35 plus 25 jxL concentrated HCl.1 M acetic acid. inject 75-100 |xL aliquot. 471-474 SAMPLE Matrix: blood Sample preparation: Condition a Bond-Elut C18 column with 2 volumes MeOH then 2 volumes water.9 Internal standard: promazine (5. desmethyldoxepin. R. Jusko.9 mL t-butylamine (EtOH: MeCN: t-butylamine 98:2:0..A. doxepin. vortex 10 s. dextropropoxyphene. repeat elution process two more times. protriptyline Simultaneous: N-acetylprocainamide. diazepam. Liquid-chromatographic determination of eight tri. chlorpheniramine. amoxapine. desmethylchlordiazepoxide.05) Flow rate: 2 Injection volume: 75-100 Detector: UV 254 CHROMATOGRAM Retention time: 6. desipramine. desipramine. 2-hydroxydesipramine. wash with MeOH/water. chlorimipramine. wash with 2 volumes 0. T. 30. W. Add 1 mL serum then 200 |xL 700 ng/mL promazine in MeOH: 0. desmethylclomipramine. imipramine. chlordiazepoxide. di- . 2-hydroxyimipramine. Clin. oxazepam. amitriptyline. desmethyldoxepin.) HPLC VARIABLES Column: 250 X 4. wait for 30 s. diazepam. D'Ambrosio.6 5 fim Supelco Mobile phase: 1 gal EtOH + 77 mL MeCN + 1. doxepin.HPLCVARIABLES Column: 250 X 4. desmethyldisopyramide. thioridazine KEYWORDS plasma REFERENCE Sutfin..6 Zorbax SiI Mobile phase: MeOH: ammonium hydroxide 998:2 Flow rate: 1.J. buprion. Reconstitute with 200 |xL mobile phase. add 200 |xL 10 mM ammonium acetate in MeOH. imipramine Also analyzed: clomipramine. cocaine. 1984.. (MeOH/water was 500 mL MeOH-.1 M HCl 13:87 to each column. wash with 2 volumes water.2) Limit of detection: 4 ng/mL OTHER SUBSTANCES Extracted: amitriptyline. chlorpromazine. Combine eluates and evaporate them to dryness at 56-8° under compressed air. amphetamine. protriptyline Noninterfering: chlordiazepoxide. demoxepam. codeine. elute with vacuum.5 Injection volume: 50 Detector: UV 254 CHROMATOGRAM Retention time: 9 Internal standard: N-desmethylclomipramine hydrochloride (10) Limit of quantitation: 20 ng/mL OTHER SUBSTANCES Extracted: metabolites.and tetracyclic antidepressants and their major active metabolites. maprotiline. flurazepam. trifluopromazine. vortex for 30 s. trifluoperazine.. diazepam. 10-hydroxynortriptyline. 5. methadone. Voris.9:0. trifluoperazine Interfering: haloperidol. Remove the organic layer and add it to 100 |xL 250 mM HCl. desmethylchlordiazepoxide. promethazine. Tricyclics. zimeldine Noninterfering: thiopropazine Interfering: prochlorperazine KEYWORDS serum. J.Liq.1% diethylamine + 5 mL hexane: isoamyl alcohol 97:3. 2761-2773 SAMPLE Matrix: blood . propoxyphene.6 40 (xm C8 (Supelco) Column: 250 X 4. 1983.18) Limit of detection: 2. centrifuge at 500 g for 3 min. mianserin. pyrilamine.Chromatogr.Drug Monit. desipramine.4.C. maprotiline.. oxazepam Noninterfering: molindone. oxaprotiline. oxapam.45 Internal standard: loxapine (k' 7. hydroxyamoxapine. morphine. inject a 50 |JLL aliquot of the aqueous phase. vortex for 30 s.5 ng/mL OTHER SUBSTANCES Extracted: amitriptyline. desmethyldoxepin. desmethldiazepam... Abramson.6 5 jxm Supelcosil C8 Mobile phase: MeCN:water:diethylamine:85% phosphoric acid 53. imipramine. thioridazine. HPLCVARIABLES Guard column: 50 X 4.1:1:0. phenteramine. trimipramine. norzimeldine. quinidine. chlordiazepoxide. J. doxepin. procainamide.L. Ther.. R.1 + 250 |xL 25% potassium carbonate containing 0. perphenazine. Hubbard. meperidine. chlorpromazine. Morgan. perphenazine. A rapid high performance liquid chromatographic method for the simultaneous measurement of six tricyclic antidepressants. prolixin.3:45. fluphenazine. 279-292 SAMPLE Matrix: blood Sample preparation: 2 mL Plasma + 100 JULL 1 |mg/mL loxapine in isopropanol: diethylamine 99. loxepin. 2-hydroxyimipramine. pH adjusted to 7. fluphenazine. iprindole. trimeprazine. Liquid chromatographic separation of antidepressant drugs: I.S. J.2 with NaOH or phosphoric acid Flow rate: 2 Injection volume: 50 Detector: UV 254 CHROMATOGRAM Retention time: k' 3.W. thiothixene KEYWORDS plasma REFERENCE Kiel. RA.K. normal phase REFERENCE Beierle. 6. S. R. iminostilbene.sopyramide. 1983. 2-hydroxydesipramine. centrifuge for 5 min. HPLCVARIABLES Column: 300 X 4 10 |xm jjiBondapak CN Mobile phase: MeCN:MeOH: 5 mM phosphate buffer 60:15:25. promethazine. Brown. fluphenazine. Hu.5 mL aliquot of the organic layer and evaporate it to dryness.5 Injection volume: 50 Detector: UV 254 CHROMATOGRAM Retention time: 10. reconstitute the residue in 1 mL 100 mM HCl. vortex for 15 s. trifluoperazine. propoxyphene. trimeprazine KEYWORDS plasma. adjusted to pH 7. butaperazine. piperacetazine. maprotiline. inject a 50 IxL aliquot. S. procainamide. carphenazine. Reconstitute in 100 JULL mobile phase. triflupromazine. thioxanthene and butyrophenone neuroleptics and antihistamines in blood and plasma with conventional and radial compression columns and UV and electrochemical detection. trihexyphenidyl. benztropine. inject a 50 (JLL aliquot.Chromatogr. Liquid chromatographic assay of phenothiazine. (It is implied. desipramine. thioridazine.10 Internal standard: protriptyline (12. doxepin.Sample preparation: 10 mL Plasma or whole blood + 1 mL 1 M NaOH. haloperidol.H. but not explicitly stated in the paper. promazine. amitriptyline.7 Limit of detection: 10 ng/mL OTHER SUBSTANCES Simultaneous: acetophenazine. orphenadrine. J. 231. desmethyldoxepin. thioridazine. J.) HPLCVARIABLES Column: 10 fxm Micropak CN (Varian) Mobile phase: MeCN: 20 mM ammonium acetate 90:10 Flow rate: 2.0 Flow rate: 2 Injection volume: 50 Detector: UV 254 CHROMATOGRAM Retention time: 7. 361-376 SAMPLE Matrix: blood Sample preparation: 1 mL Serum + 200 |xL 10 fxg/mL protriptyline in water + 200 fxL 80 g/L NaHCO3 + 5 mL hexane.. propranolol. 1982. extract twice with 10 mL hexane for 30 min. trimipramine . vortex for 1 min. Remove the hexane layer and evaporate it in a stream of nitrogen at 60°. mesoridazine. that this extraction procedure works for this compound.-R. vortex for 15 s. whole blood REFERENCE Curry. reconstitute the residue in 100 jxL mobile phase.. Perrin. chlorpromazine. add 5 mL chloroform. O..H.Y. Remove a 4.A. imipramine. E. thiothixene.20) Limit of detection: 10 ng/mL OTHER SUBSTANCES Extracted: amitriptyline. imipramine. centrifuge. Remove the organic layers and evaporate them to dryness under a stream of nitrogen. chlorpromazine. doxepin.5) Limit of detection: 0. secobarbital.Y.. dialysate Sample preparation: Adjust pH of serum samples to 7. Inject 1 mL mobile phase.Chromatogn. prochlorperazine. 4. thioridazine. chlorpromazine.7 with dilute KOH. salicylic acid. pentobarbital. Elute column A onto column B with mobile phase for 30 s then remove it from the circuit.Noninterfering: acetaminophen.055 g Hg(NO3)2 in 1 L water. Clin.Chem. and 1 mL MeCN: water 50:50 onto column A. Reversed phase high-performance liquid chromatographic analysis of tricyclic antidepessants in plasma. caffeine.) Column temperature: 50 Flow rate: 2 Injection volume: 50 Detector: UV 254 CHROMATOGRAM Retention time: 4. R. propoxyphene. codeine. lorazepam.775 g NaH2PO4 + 2. Mullins. diazepam. trifluoperazine Interfering: disopyramide KEYWORDS serum REFERENCE Koteel. centrifuge at 1686 g for 5 min. oxazepam.Liq. HPLCVARIABLES Guard column: ixBondapak/Porasil Column: jxBondapak C18 Mobile phase: MeCN:buffer 40:60 (Buffer was 13. 1 mL water. 462-466 SAMPLE Matrix: blood Sample preparation: 2 mL Plasma + 1600 ng clomipramine in MeOH + 2 mL 1 M NaOH + 5 mL hexane: isoamyl alcohol 99:1.4. Sample preparation and liquid-chromatographic analysis for tricyclic antidepressants in serum. inject a 50 JJLL aliquot of the aqueous phase. meperidine KEYWORDS plasma REFERENCE Wong.2H2O + 0. R. clomipramine.) . chlordiazepoxide. phenobarbital. shake for 15 min. McCauley..H. pH was 7. imipramine Simultaneous: chlordiazepoxide.5 Internal standard: clomipramine (7. cimetidine. trifluoperazine Noninterfering: acetaminophen. shake mechanically for 15 min. flurazepam. J. theophylline. phenytoin.E.. 1 mL water. S. 1981. T.H. methaqualone.4 and dialyze 3 mL serum against 5 mL dialysis buffer at 37° in PTFE chambers for 4 h.998 g Na2HPO4. Remove the organic phase and add it to 200 |xL 0. diazepam. Gadsden.05% orthophosphoric acid. Elute column B with mobile phase and monitor the effluent.68 g KH2PO4 in 2 L water. 849-862 SAMPLE Matrix: blood. 28.. centrifuge for 5 min. (Dialysis buffer was 3.250 g NaCl + 0. adjusted to pH 4. perphenazine.6 ng OTHER SUBSTANCES Extracted: amitriptyline. desipramine. P. 2 mL dialysate. 1982. 5 with concentrated HCl.65 Injection volume: 1000-2000 Detector: UV 238 CHROMATOGRAM Retention time: 3. diazepam.5 nM (5 mL sample) OTHER SUBSTANCES Extracted: amitriptyline Simultaneous: alprazolam. lorazepam. oxazepam. fluphenazine.5 mM NaOH in MeOH. Remove the organic layer and evaporate it to dryness under a stream of nitrogen. UV 254 CHROMATOGRAM Retention time: 19 OTHER SUBSTANCES Extracted: alprenolol. flunitrazepam. J. diazepam. clonazepam. mix on a rotary mixer for 10 min. G. pH adjusted to 9. or gastric contents or 1 g tissue homogenate + 500 |xL buffer + 8 mL n-hexane: ethyl acetate 70:30. trimipramine. centrifuge at 3000 g for 8 min. chlorpromazine. desipramine. B was 12. zolpidem . A:B 10:90 for 5 min. maintain at 90:10 for 5 min. bromazepam. Nyberg. levomepromazine.55:0. High-performance liquid chromatographic quantitation of amitriptyline and nortriptyline in dialysate from plasma or serum using on-line solid-phase extraction. thioridazine sulfone. thioridazine. zuclopenthixol Noninterfering: carbamazepine.8 g potassium carbonate in 100 mL water. B 100 X 4 3 iJtm Spherisorb ODS Superpac Mobile phase: MeCN: 85% phosphoric acid: triethylamine: water 49. chlorprothixene. reconstitute the residue in 100 |xL 12. C. urine Sample preparation: 1 mL Blood. (Buffer was 13.5 mM NaOH in water. return to initial conditions over 1 min. desmethylimipramine.. clomipramine. amitriptyline.Chromatogr. clonazepam. zimeldine. phenytoin Interfering: maprotiline. imipramine.. perphenazine. pindolol.225:50 Flow rate: 0. protriptyline.225:0. urine. desclomipramine. haloperidol. flunitrazepam. gastric contents. 620303). Martensson. A was 12. chlorpromazine. nitrendipine. re-equilibrate for 5 min. haloperidol. nitrazepam.85 Limit of detection: 0. inject a 50 |xL aliquot. no. 363-369 SAMPLE Matrix: blood. promethazine. carbamazepine.) HPLCVARIABLES Guard column: 4 X 4 30 |xm LiChrocart Aluspher RP-select B (Merck) Column: 125 X 4 5 fxm Aluspher RP-select B (Merck) Mobile phase: Gradient.5 mM NaOH in MeOH: water 50:50. Flow rate: 1 Injection volume: 50 Detector: UV 230.HPLCVARIABLES Column: A10 X 6 packed with 40 |xm material from a Bond Elut cartridge (cat. nordiazepam. E. to 90:10 over 15 min. tissue. column-switching REFERENCE Svensson. thioridazine sulfoxide KEYWORDS serum. 432. chlordiazepoxide. 1988. norfluoxetine. quinine. dihydroergotamine. Remove the organic layer and inject a 30 |JLL aliquot of the aqueous layer.6 5 |xm Brownlee Spheri-5 RP-18 Mobile phase: MeCN: 100 mM NaH2PO4: diethylamine 40:57. practolol. brompheniramine. dihydrocodeine.27 Internal standard: cianopramine (8. metoclopramide. norphetidine. droperidol. sotalol. hydrochlorothiazide.E. HPLCVARIABLES Guard column: 15 X 3. norpropoxyphene. vortex. tissue Sample preparation: Whole blood. Remove the organic layer and inject a 30 |xL aliquot of the aqueous layer. nitrazepam. amphetamine. flurazepam. A. thioridazine. clomipramine. desipramine. methylphenidate. meperidine.Also analyzed: acebutolol. prazepam. fluoxetine. chloroquine. piritramide. chlorpromazine. Tissue. fluoxetine. methaqualone. caffeine. metoclopramide. papaverine.ToxicoL. 19. prochlorperazine. methadone. doxepin. mepyramine. 1 mL Whole blood or serum + 1 jxg cianopramine + 1 mL water.5:2. minoxidil. metoprolol. trazodone. serum. centrifuge at 2500 g for 5 min. phenoxybenzamine. vortex. tranylcypromine. gently agitate for 30 min. northiaden. ethyl loflazepate. 0. quinidine. agitate gently for 30 min. sulpride.93) Limit of detection: 50 ng/mL OTHER SUBSTANCES Simultaneous: amitriptyline. domperidone. dihydralazine. doxepin. midazolam. trazodone. flupentixol. mesoridazine. maprotiline. cocaine. De Leenheer.2% phosphoric acid. Meyer. chlorpheniramine. imipramine. alprazolam. tripelennamine. trimipramine. lormetazepam. 1995. W. thioridazine. pentazocine. mianserin. benztropine. codeine. camazepam. protriptyline. nordoxepin. propranolol. atenolol. cyproheptadine. methadone. 73-78 SAMPLE Matrix: blood. Remove the organic layer and add it to 400 |xL 0. prazosin. moclobemide. propoxyphene. methyldopa. gliclazide. clotiazepam. triprolidine Noninterfering: dextromethorphan. agitate gently for 30 min. fenethylline. propranolol. clothiapine. prothipendyl. cloxazolam. ibuprofen. medazepam. sulforidazine. haloperidol. mianserin. centrifuge for 5 min. lorazepam. pentobarbital. add 1 mL 200 mM sodium carbonate. promazine. diphenhydramine. furosemide. mexiletine.2% phosphoric acid. propoxyphene. imipramine. Systematic toxicological analysis of basic drugs by gradient elution of an alumina-based HPLC packing material under alkaline conditions.. dothiepin.. J. trifluoperazine Interfering: diphenhydramine . amoxapine. ketazolam.P.5 mL Liver homogenate + 10 |xg cianopramine + 500 |xL 2% sodium tetraborate + 8 mL hexane: 1-butanol 95:5. E. verapamil. clomipramine. thiothixene. add 6 mL hexane: 1-butanol 95:5. promethazine. phenprocoumon. brotizolam. quinine. loxapine. clobazam. captopril. hydroxyzine. acetaminophen. oxprenolol. trihexyphenidyl. centrifuge for 5 min. yohimbine REFERENCE Lambert. ergotamine. pheniramine. gently agitate for 30 min. phenylbutazone. promethazine. triazolam. trimipramine. loprazolam.5 Flow rate: 2 Injection volume: 30 Detector: UV 220 CHROMATOGRAM Retention time: 7.2 7 |xm RP-18 Newguard (Applied Biosystems) Column: 100 X 4. tyramine. betaxolol. nomifensine. maprotiline. diclofenac. Remove the organic layer and add it to 100 |xL 0. centrifuge at 2500 g for 5 min. morphine.Anal. nadolol. pipamperone. Yoshida.0 with phosphoric acid. liver REFERENCE Mclntyre. tissue Sample preparation: Serum. Add supernatant to 4 mL 4 M KOH. nortiptyline is IS REFERENCE Sugita.5% perchloric acid. 1987. weigh. centrifuge at 11000 g for 15 min. rat. Add supernatant (9 mL) to 10 mL diethyl ether:ethyl acetate 85:15. S. S. heat at 70° for 30 min. shake vigorously. I.. O. Add supernatant to 1 mL 4 M KOH. imipramine KEYWORDS serum.2 Internal standard: nortriptyline Limit of detection: 10 ng/g (tissue) OTHER SUBSTANCES Extracted: desipramine. Remove 8 mL of organic phase and evaporate it to dryness under a stream of nitrogen.. Remove the organic layer and add it to 100 jxL 0.KEYWORDS serum. extract with hexane: butanol 95:5 for 20 min. 1 mL Extract + 1 |xg protriptyline + 1 mL water + 1 mL 200 mM sodium carbonate buffer. adjust pH to 9. A.H. Kobayashi.ethyl acetate 3:1. Drummer. whole blood. Tissue.V. inject 100 |xL aliquot. mix for 20 min. Dual ultraviolet wavelength high-performance liquid chromatographic method for the forensic or clinical analysis of seventeen antidepressants and some selected metabolites. mix.) Column temperature: 40 Flow rate: 1 Injection volume: 100 Detector: UV 254 CHROMATOGRAM Retention time: 14. centrifuge. 412-417 SAMPLE Matrix: hair Sample preparation: Wash hair in water. King. J.M.. K.. 621. 421. inject 100 |JLL aliquot. centrifuge at 11000 g for 15 min.. Remove 8 mL of organic phase and evaporate it to dryness under a stream of nitrogen. 215-223 SAMPLE Matrix: blood.Chromatogr.Chromatogr.2% orthophosphoric acid. 2 g Brain tissue + 10 mL 2. Nakazawa. HPLCVARIABLES Column: 250 X 4.. T. rinse 3 times with MeOH. Skafidis. Dissolve residue in 200 JJLL mobile phase buffer: MeOH 9:1. 1993. C. homogenize.5-10.6 5 |jim Cosmosil 5C18 Mobile phase: MeOH: THF: buffer 45:17:88 (Buffer was 1% triethylamine adjusted to pH 3. shake for 15 min. Add supernatant to 20 mL diethyl ether-. 5-25 mg Washed hair + 1 mL 1 M NaOH. 1 mL Serum + 4 mL MeOH + 5 mL 2. dry. inject a 30 |xL aliquot of the aqueous layer. centrifuge. Suzuki. S. shake for 15 min. High-performance liquid chromatographic determination of imipramine and its metabolites in rat brain.2 7 \xm Newguard RP-18 ..5% perchloric acid + 8 mL MeOH. HPLCVARIABLES Guard column: 15 X 3. J. Dissolve residue in 200 |xL mobile phase buffer:MeOH 9:1. R.5 Internal standard: desipramine (9) Limit of detection: LOD 50 pmole OTHER SUBSTANCES Extracted: amitriptyline Noninterfering: ketoconazole. liver REFERENCE Schmider. 40.Forensic ScL. HPLCVARIABLES Column: 300 X 3. Shader. L.J. inject an aliquot of the supernatant. O.. doxepin.) Flow rate: 2 Injection volume: 30 Detector: UV 214 CHROMATOGRAM Retention time: 5 Internal standard: protriptyline (4) OTHER SUBSTANCES Extracted: amitriptyline.. LM. centrifuge at 16000 g for 5 min.0 NaH2PO4 + 30 mL diethylamine. Harmatz. dothiepin. a-naphthoflavone. 1995. clomipramine. Mclntyre. von Moltke.2 L 100 mM pH 7.. mianserin KEYWORDS may be interferences REFERENCE Couper. RJ.. 592-597 SAMPLE Matrix: solutions HPLCVARIABLES Column: 250 X 4. desipramine.6 Spheri-5 RP-C18 Mobile phase: MeCN: buffer 40:60 (Buffer was 1.L N-Demethylation of amitriptyline in vitro: Role of cytochrome P-450 3A (CYP3A) isoforms and effect of metabolic inhibitors... 83-86 SAMPLE Matrix: microsomal incubations Sample preparation: 250 |JLL Microsomal incubation + 50 |xL 1 M HCl.Column: 100 X 4.H. imipramine. Greenblatt.L. 275. J. J. quinidine KEYWORDS human.4 Detector: UV 220 CHROMATOGRAM Retention time: 10.Pharm.Exp.9 jxBondapak C18 Mobile phase: MeCN: 50 mM pH 6 potassium phosphate buffer 35:65 Flow rate: 1.Ther. 1995. D. cool on ice. Extraction of psychotropic drugs from human scalp hair.. haloperidol.6 5 jxm Supelcosil LC-DP (A) or 250 X 4 5 |xm LiChrospher 100 RP-8 (B) . J.S. add desipramine. J. Drummer. paroxetine. bromocriptine. albuterol. pentazocine. acetaminophen. thiothixene. triflupromazine. doxapram. 103-119 SAMPLE Matrix: solutions HPLCVARIABLES Guard column: 30 X 2. pemoline. clonazepam. chlorcyclizine.1 Spheri-5 RP-8 Column: 220 X 2. tolmetin. nifedipine. diphenoxylate. pindolol. propofol. acetazolamide. propranolol. ketoprofen. clonidine. trimeprazine. chlorpheniramine. triazolam. dantrolene. zopiclone KEYWORDS some details of plasma extraction REFERENCE Koves. flurbiprofen. phenyltoloxamine. ibuprofen. imipramine. 1995. procainamide. mefenamic acid. baclofen. trimipramine. methylphenidate. amitriptyline. verapamil. amoxapine. glutethimide. ranitidine. fenoprofen. diphenidol. mazindol. 6. sulfinpyrazone. fluvoxamine. chlorpropamide. sulindac. codeine. hydromorphone. pentobarbital. tetracaine. droperidol. make up to 1 L. loxapine. naphazoline. metformin. diltiazem. Use of high-performance liquid chromatography-diode array detection in forensic toxicology. risperidone. propafenone. quinine. acepromazine. brompheniramine. trimethoprim. dobutamine. atenolol. moclobemide. methoxamine. atropine. buspirone. glyburide. metoclopramide.70 (A). procyclidine. chlorprothixene. encainide. scopolamine. xylometazoline. ethopropazine. fluoxetine. oxazepam. terbutaline. procaine. cimetidine. hydroxychloroquine.A. ketoconazole. mephenytoin. triamterene. methotrimeprazine. phenolphthalein. mepivacaine. thiopental. spironolactone. ethidium bromide. acetophenazine.Chromatogr. metolazone. amobarbital. hydrocodone. disopyramide. prazepam. phenol. guaifenesin. yohimbine. levorphanol. pentoxifylline. cocaine. diclofenac. piroxicam. trazodone. antipyrine. temazepam. midazolam. J. morphine. methdilazine. haloperidol. butabarbital. methadone. cetirizine. alprazolam. chlormezanone. propantheline. perphenazine. chlorpromazine. sotalol. doxepin. butalbital. naproxen. norepinephrine.025% phosphoric acid:buffer 25:10:5 (A) or 60:25:15 (B) (Buffer was 9 mL concentrated phosphoric acid and 10 mL triethylamine in 900 mL water.Mobile phase: MeCN:0. terfenadine. tocainide. cisapride. diflunisal. quinidine. pheniramine.) Flow rate: 0. azatadine. warfarin. flurazepam. bupivacaine. hydroxyzine. oxycodone. sertraline. tolbutamide. nizatidine. phenytoin. hydrochlorothiazide. mesoridazine. trifluoperazine. phenylbutazone. metaproterenol. methotrexate. promethazine. thiethylperazine. naloxone. caffeine. chlordiazepoxide. nalbuphine. timolol. diazepam. ketorolac. indomethacin. benzocaine. racemethorphan. protriptyline. phenobarbital. meperidine. E. chloroquine. metoprolol. methocarbamol.75 (B) OTHER SUBSTANCES Also analyzed: acebutolol. clozapine. desipramine. quazepam.M. dipyridamole. metronidazole. diphenhydramine. salicylic acid. theophylline. adjust pH to 3. cyclobenzaprine. methyldopa. colchicine. carbamazepine. lidocaine. lorazepam. nadolol. chlorthalidone. probenecid.4 with dilute phosphoric acid. furosemide. pimozide. pramoxine. loratadine. fluphenazine.1 Spheri-5 RP-8 . prazosin. brotizolam. labetalol. remoxipride. homatropine. clomipramine. cyclizine. lovastatin.6 Injection volume: 25 Detector: UV 229 CHROMATOGRAM Retention time: 13. fentanyl. flavoxate. secobarbital. thioridazine. promazine. propiomazine. 692. phentolamine. oxymetazoline. hydralazine. chlorzoxazone. prochlorperazine. hydroxyzine. Antidepressants. perphenazine. to 0:100 over 15 min (?). mesoridazine.03 OTHER SUBSTANCES Simultaneous: amitriptyline. p. flurazepam. chlorpromazine.5 Detector: UV 200 CHROMATOGRAM Retention time: 13. pH 2. thiothixene.A. A:B from 100:0 to 0:100 over 30 min. A:B 95:5 for 2 min. Rainin Instrument Co. make up to 1 L with MeCN. protriptyline.Pharm.09% phosphoric acid.6 Zorbax RX Mobile phase: Gradient. desmethyldoxepin.8 OTHER SUBSTANCES Simultaneous: amitriptyline. 83. desipramine. desipramine. imipramine. thioridazine. 1994. B was 10 mL concentrated orthophosphoric acid and 7 mL triethylamine in 200 mL water. phenylpropanolamine. desalkylflurazepam. inject a 5 |xL aliquot. T. Woburn MA. prazepam. 1994. fenfiuramine.Mobile phase: Gradient. nordiazepam. phentermine. Column temperature: 50 Flow rate: 0. HPLCVARIABLES Column: 250 X 4.. buclizine. pressure 200 bar REFERENCE Berger. W.09% phosphoric acid in water. 2.6 5 |xm Lichrosphere cyanopropyl Mobile phase: Carbon dioxide: MeOH: isopropylamine 90:10:0.08% diethylamine and 0. norchlordiazepoxide. A was 0.ScL.H. A was 10 mL concentrated orthophosphoric acid and 7 mL triethylamine in 1 L water. J. trifluoperazine REFERENCE Rainin Catalog Ci-94.3.08% diethylamine and 0. chlordiazepoxide. Separation of drugs by packed column supercritical fluid chromatography.05 Column temperature: 50 Flow rate: 3 Injection volume: 5 Detector: UV 220 CHROMATOGRAM Retention time: 4. promazine. doxepin. 1994-5. 287-290 SAMPLE Matrix: solutions HPLCVARIABLES Column: 250 X 4. diazepam. maintain at 0:100 for 5 min. ephedrine. diethylpropion. benactyzine. . 7. imipramine Also analyzed: amphetamine. B was MeCN: water 90:10 containing 0. maintain at 0:100 for 5 min. oxazepam. thioridazine KEYWORDS SFC. methamphetamine. Wilson.24 SAMPLE Matrix: solutions Sample preparation: Prepare a 1 mg/mL solution in MeOH.. tetramisole. amobarbital.Anal. butacaine. methamphetamine. trichloromethiazide. lorazepam. propylparaben. buspirone. triprolidine. trihexyphenidyl. epinine. tolmetin. reserpine. pentobarbital. oxazepam. methapyrilene. morphine. ethacrynic acid. naproxen. clonazepam. fenproporex. doxepin.Column temperature: 30 Flow rate: 2 Detector: UV 210 OTHER SUBSTANCES Also analyzed: acepromazine. thioridazine. phencyclidine. chlorpheniramine. nifedipine. tropacocaine. trimethoprim. tobutamide. propiomazine. yohimbine. ibogaine. secobarbital. furosemide. flunitrazepam. quinine. benzphetamine. mephesin. mepivacaine. sulfadimethoxine. estriol. phenazocine. aprobarbital. noscapine. haloperidol. thiamine. flubendazole. cyclothiazide. phenylbutazone. bromazepan. A. desipramine. hydroxyquinoline. epinephrine. aspirin. fenoprofen. sulindac. isocarboxazid. methyldopamine. mesoridazine. kynurenic acid. famotidine. diprenorphine. nitrazepam. quinidine. saccharin. dexamethasone. chlorothiazide. ketamine. thiobarbituric acid. caffeine. pentazocine. salicylamide. vincamine. isoproterenol. methyl salicylate. iminostilbene. butabarbital. nalorphine. diethylpropion. warfarin. oxymorphone. tyramine. fentanyl. niacinamide. phenylephrine. papaverine. clonixin. sulfaethidole. J. pargyline. buprenorphine. 18. diltiazem. cinchonine. J. verapamil. pheniramine. sulfamethazine. acetaminophen. amitriptyline. avermectin. diclofenac. thiabendazole. doxapram. danazol. dronabinol. lormetazepam. methyltestosterone.. scopolamine. recinnamine. digitoxin. glunixin. phenelzine. methoxamine. berberine. medazepam. glipizide. ranitidine. sulfapyridine. W. clenbuterol. oxytetracycline. hydromorphone. sulfamerazine. amylocaine. butethal. cinchonidine. metoprolol. phenothiazine. chlorphenesin. prazepam. brompheniramine. phenazopyridine. acetophenazine. carbamazepine. nicotinic acid. thiosalicylic acid. mazindol. chlorpropamide. tamoxifen. halazepam. diazepam. tripelennamine. sulfamethoxizole. ephedrine. benzocaine. propranolol. methocarbamol. fenbendazole. Iidocaine. cortisone. fluphenazine. phendimetrazine. quinaldic acid. dopamine. tetracycline. phenacetin. disulfiram. chlortetracycline. imipramine. dextromethorphan. estradiol. theophylline. tribenzylamine. 233-242 SAMPLE Matrix: solutions . theobromine. levorphanol. meperidine. fencamfamine. sufadiazine. thiothixene. ethosuximide. gitoxigenin. piperocaine. methyprylon. debrisoquine. diphenoxylate. phenobarbital. mephenytoin. mephentermine. carbromal. methylprednisolone. mebendazole.ToxicoL. isoxsuprine. flufenamic acid. naltrexone. benzotropine. temazepam. etorphine. isoniazid. cyclobenzaprine. scopoletin. indomethacin. ivermectin. chloroxylenol. niflumic acid. strychnine. quazepam. clorazepate. cimetidine. oxyphenbutazone. nadolol. sulfanilamide. cyheptamide. thymol. glybenclamide. mibolerone. phentermine. 1994. tetracaine. aminophylline. glutethimide. etonitazene. norepinephrine. coumarin. dextropropoxyphene. hydrocodone. sulfasoxizole. sulfacetamide. mephobarbital. colchicine. diphenhydramine. fluoxymesterone. methadone. dapsone. diflunisal. digoxin. D. methazolamide. triamcinolone. progesterone. prednisolone. cymarin. gentisic acid. chloroquine. meclizine. cyclazocine. methaqualone. zoxazolamine REFERENCE Hill. pemoline. methylphenidate. Kind. salicylic acid. meclofenamic acid. isocarbostyril. nicotine. persantine. antipyrine. diamorphine. methsuximide. testosterone. chlorpromazine. eugenol. nylidrin. resorcinol. thiamylal. albuterol. oxycodone. 5-fluorouracil. bibucaine. pseudoephedrine. cocaine. probenecid. tolazoline. methyldopa. albuterol. trifluoperazine. amoxapine. loxapine. phensuximide. nefopam. atropine. Reversed-phase solvent gradient HPLC retention indexes of drugs. mescaline. chloramphenicol. diethylstilbestrol. mefenamic acid. mepacrine. hydrocortisone. naloxone. atenolol. pyrithyldione. megestrol. phenylpropanolamine. guaiacol. ibuprofen. pyrilamine. primidone. benzoic acid. danthron. puromycin. tolazamide. amphetamine. estrone. thebaine. codeine. ketoprofen. hydrochlorothiazide. dipyrone. tranylcypromine. barbital. naphazoline. chlordiazepoxide. W. inject a 10 |xL aliquot. carbamazepine. J. imipramine.2 KH2PO4 23. loxapine. imipramine Also analyzed: desipramine.HPLCVARIABLES Column: 150 X 4. p.Liq.. desmethyldoxepin.6 containing 0.6 5 ixm Adsorbosphere C18 (PEEK column) (retention times are longer and peaks broader with stainless steel column) Mobile phase: MeCN: 20 mM pH 3. amoxapine.Chromatogr. 440 SAMPLE Matrix: solutions Sample preparation: Inject an aliquot of a solution in mobile phase.2 Detector: UV 214 CHROMATOGRAM Retention time: 12 OTHER SUBSTANCES Simultaneous: amitriptyline. T. Deerfield IL. Alltech Associates. maprotiline. desipramine. HPLCVARIABLES Column: 300 X 3. cyclobenzaprine.9 Limit of quantitation: < 1 jig/mL OTHER SUBSTANCES Simultaneous: amitriptyline.4:76. 1545-1560 SAMPLE Matrix: solutions Sample preparation: Dissolve in MeOH: water 1:1 at a concentration of 50 |xg/mL. doxepin.6 Econosil C8 Mobile phase: MeCN: buffer 30:70 (Buffer was 20 mM KH2PO4 and 14 mM triethylamine adjusted to pH 3.05% nonylamine Flow rate: 1.5:0.5:38 Flow rate: 1. 16.) Injection volume: 20 Detector: UV 210 CHROMATOGRAM Retention time: 9. trazodone REFERENCE Alltech Chromatography Catalog 300. Identification and quantification of tricyclic antidepressants by UV-photodiode array detection with multicomponent analysis. doxepin.0 with phosphoric acid.. 1993.9 10 |xm jjuBondapak C18 Mobile phase: MeOH: acetic acid: triethylamine: water 60:1. protriptyline KEYWORDS UV spectra given REFERENCE Ryan. maprotiline. 1993. Inc.5 Injection volume: 10 Detector: UV . HPLCVARIABLES Column: 250 X 4. benzocaine. phenoperidine. fenoterol. proxymetacaine. phendimetrazine. ergosinine. pyrimethamine. butacaine. indapamine. dimethothiazine. chlorcyclizine. pecazine. etorphine. phenothiazine. haloperidol. piritramide. dextromoramide. LeCarbone. primaquine. fluopromazine. dipyridamole. 370. cyclazocine. meclozine. protriptyline. chlorphenoxamine. ehlorprenaline. ehlorpheniramine. ergosine. phenoxybenzamine. alprenolol. acetophenazine. pericyazine. . ergocornine. phenazocine. chlorprothixene. phenindamine. nicotine. benactyzine. methoxyphenamine. piperacetazine. prothipendyl. V25 glassy carbon electrode. methotrimeprazine.CHROMATOGRAM Retention time: k' 2. buclizine. brompheniramine. metaraminol. proheptazine. J. bufotenine. doxylamine. prochlorperazine. ibogaine. practolol. ergotamine. mianserin. iprindole. fentanyl. methoxamine. dothiepin. nomifensine. phenomorphan. doxapram. oxprenolol. Lau-Cam. dextropropoxyphene. pirenzepine. disopyramide. nalorphine. oxeladin. piminodine. hyoscine. proadifen. benperidol. pH 6. metoprolol. clomipramine.. methdilazene. procyclidine. lofepramine. mephentermine. propiomazine. bamethane. mepyramine. amiodarone. laudanosine. bromperidol. oxymetazolin. prilocaine. medazepam. naphazoline. meclophenoxate. butethamate. General reversed-phase high-performance liquid chromatographic method for the separation of drugs using triethylamine as a competing base. pipazethate. cyproheptadine. nadolol. clemastine. methysergide. nifedipine. procainamide. N-acetylprocainamide. pronethalol. phenadoxone. methylephedrine. ergocristine. bromhexine. morazone. + 1. promethazine. phentolamine. prolintane.6 OTHER SUBSTANCES Also analyzed: acebutolol. perphenazine. methoxypromazine. benzethidine. hydroxyzine. brompromazine. CA.. pseudoephedrine. maprotiline. clonidine. pizotifen. ephedrine. mesoridazine. diphenhydramine. naloxone. antazoline. phenampromide. metoclopramide. azacyclonal. isoxsuprine. acepromazine. ethopropazine.7 Flow rate: 2 Injection volume: 20 Detector: E. cinchonidine. metopimazine. pipradol.9 Spherisorb S5W silica Mobile phase: MeOH containing 10 mM ammonium per chlorate and 1 mL/L 100 mM NaOH in MeOH. pargyline.60 REFERENCE Roos. lidocaine. dipipanone. inject a 20 \xL aliquot. quinidine. pramoxine. methapyrilene.Chromatogr. noscapine. ergocristinine. bromodiphenhydramine. pheniramine. doxepin. amethocaine. physostigmine. dimethindene. cimetidine. etoxeridine. methamphetamine. deserpidine. buprenorphine. meptazinol. mecamylamine. propranolol. flurazepam. ketanserin. imipramine. fenfluramine. pipamazine. 1986. properidine. cyclopentamine. papaverine. pimozide. phenbutrazate. methylergonovine. flupenthixol. dicyclomine. bupivacaine. 403-418 SAMPLE Matrix: solutions Sample preparation: Prepare a 10 |xg/mL solution in MeOH. isothipendyl. penbutolol. promazine. orphenadrine. benzphetamine. pentazocine. ergocryptine. ergometrine.W. cinnarizine. diprenorphine. phenelzine. phenylephrine. pindolol. phenmetrazine. cyclizine. amitriptyline. droperidol. dihydroergotamine. atenolol. diphenoxylate. loxapine. fluphenazine. chlorpromazine. diethylcarbamazine. benzquinamide. benzoctamine. R. prazosin. flavoxate. mepivacaine. phenglutarimide. desipramine. penthienate. piperidolate. prenylamine. procaine. methadone. albuterol. nortriptyline. diethylpropion.2 V CHROMATOGRAM Retention time: 2. HPLCVARIABLES Column: 125 X 4. fenethazine. diethylthiambutene. cocaine. phenyltoloxamine. centrifuge at 11000 g for 30 s. S.. xylometazoline REFERENCE Jane. thioproperazine. inject a 500 |xL aliquot onto column A with mobile phase A. trifluoperazine.5 mL 1% trichloroacetic acid. codeine (different gradient). J. 1994. with 200 JJLL mobile phase C. S. meperidine REFERENCE Li. RJ. McKinnon. tolycaine. trazodone. 323. remove it from the circuit. tryptamine. II. rescinnamine. trimethobenzamide. diphenhydramine.6 min.2 5 jxm C8 (Phenomenex) + 150 X 4. thenyldiamine. trimeperidine. High-performance liquid chromatographic analysis of basic drugs on silica columns using non-aqueous ionic eluents. Briley.. verapamil. tolpropamine..B.2 11 |xm Aminex A-28 (Bio-Rad). ephedrine. phenylpropanolamine Also analyzed: amitriptyline. after 0.0 with 2 M KOH. J. theophylline. Identification and quantitation of drugs of abuse in urine using the generalized rank annihilation method of curve resolution. thonzylamine. centrifuge at 5200 g for 10 min. trimeprazine. Gemperline. L.2 |xm). fluorescence and electrochemical oxidation detection. HPLCVARIABLES Column: 250 X 4 Lichrospher 5 |xm 60 RP-select B Mobile phase: Gradient. mobile phase D. triprolidine. B 10 X 3. 655. J. tranylcypromine. 191-225 SAMPLE Matrix: urine Sample preparation: 1 mL Urine + 0. Elute column B to waste until drugs start to emerge. Elute column A to waste until drugs start to emerge then elute onto column B. terfenadine. filter (0. Flush column B with 5 mL mobile phase E then with mobile phase D. timolol. then elute onto column C. nordiazepam. C 25 X 3. thioridazine. MeCN: 50 mM pH 3. R. amphetamine. K. monitor the effluent from column C. trimethoprim. elute column C with mobile phase D. elute column A with 250 JJIL mobile phase B. norpropoxyphene. 213-223 SAMPLE Matrix: urine Sample preparation: 500 jiL Urine + N-ethylnordiazepam + chlorpheniramine + 100 |JLL buffer. trifluperidol. cocaine. thiothixene. Application of UV.) HPLCVARIABLES Column: A 10 X 2.quinine.1 12-20 (xm PRP-I spherical poly(styrene-divinylbenzene) (Hamilton). tocainide. inject a 20 |xL aliquot of the nitrate. thiethylperazine. Flanagan.15 mL mobile phase D.5 Injection volume: 20 Detector: UV 190-370 CHROMATOGRAM Retention time: 15 OTHER SUBSTANCES Extracted: benzoylecgonine.2 potassium phosphate buffer from 10:90 to 50:50 over 15 min. terbutaline.. 1985. sotalol. lidocaine.Chromatogr. tripelennamine. ranitidine. A. terazosin. trimipramine. Kazmierczak.6 5 |xm silica (Macherey-Nagel) .6 min backflush column A with mobile phase A to waste for 1.. and mobile phase A. and with 1. morphine. Flow rate: 1.Chromatogr. When all the drugs have emerged from column B. thiopropazate. Flush column A with 7 mL mobile phase E. (Buffer was 6 M ammonium acetate adjusted to pH 8. tacrine. pH adjusted to 6. diazepam. and 2 mM dimethyloctylamine. Elute with 3 mL MeOH and push air through to remove as much as possible. and 2 mM dimethyloctylamine. (Reagent was isopropanol: nheptane: 1 M sulfuric acid 40:320:1.) HPLCVARIABLES Guard column: 50 X 4.0 potassium borate buffer. add to a C18 SepPak attached to a 5 mL syringe. Mazhar.. secobarbital. D MeCN: buffer 33:67 (Buffer was 6 mM KH2PO4 containing 5 mM tetramethylammonium hydroxide.0022 Flow rate: 2. phenmetrazine.50 with phosphoric acid. ephedrine. phenobarbital. pentazocine. and 2 mM dimethyloctylamine. Evaporate eluate in vacuum at 37°. pH adjusted to 6.5 Internal standard: desmethylclomipramine Limit of detection: 16. Automated liquid chromatographic analysis of drugs in urine by on-line sample cleanup and isocratic multi-column separation.3 Internal standard: N-ethylnordiazepam (k' 2. inject 25 |xL aliquot. amitriptyline. allow to flow through (10-15 min).50 with phosphoric acid. methamphetamine KEYWORDS column.50 with phosphoric acid. 1989. chlorpheniramine (k' 5.9) Limit of detection: 300 ng/mL OTHER SUBSTANCES Extracted: amphetamine. Wash with 1 mL 0.6 5-6 |xm Zorbax cyanopropyl Mobile phase: MeCN: 0.1 M NaCl. M. E MeCN: buffer 70:30 (Buffer was 6 mM KH2PO4 containing 5 mM tetramethylammonium hydroxide. imipramine.1). Biaggi-McEachern. codeine.). Regalia.50 with phosphoric acid. cotinine.. M.1% pH 8. 473. flurazepam. lidocaine.Chromatogr.7 ng/mL . diphenhydramine.Mobile phase: A 0. UV 235 CHROMATOGRAM Retention time: k' 3.switching REFERENCE Binder. B-E 1 Injection volume: 500 Detector: UV 210. 325-341 SAMPLE Matrix: vitreous humor Sample preparation: 600 |xL Vitreous humor + 3 mL 0. mix for a few s.5 M acetic acid: n-butylamine 40:60:0.1 M NaCl + 50 |JLL 4 |xg/mL desmethylclomipramine in water.. B 6 mM KH2PO4 containing 5 mM tetramethylammonium hydroxide. morphine Interfering: desipramine.). pH adjusted to 6.6 30 ynn Permaphase ETH Column: 250 X 4. phentermine. oxazepam. methadone.R. S. wash with 3 mL reagent by gravity. nordiazepam. pH adjusted to 6. J. and 2 mM dimethyloctylamine. hydromorphone.) Column temperature: 40 (B. C MeCN: buffer 40:60 (Buffer was 6 mM KH2PO4 containing 5 mM tetramethylammonium hydroxide. M. caffeine. phenylpropanolamine.. benzoylecgonine. wash with 1 mL water. vortex with 50 |xL mobile phase for 1 min.5 Injection volume: 25 Detector: UV 254 CHROMATOGRAM Retention time: 20. hydrocodone. C only) Flow rate: A 5. N.. chlorpheniramine. R. pentazocine. tobramycin. chloramphenicol. haloperidol. hydroxyamoxapine. 391-400 Jensen. valproic acid.Anal. K.. desmethyldoxepin. 183. oxazepam. protriptyline.. amobarbital. 21-25 [rat. haloperidol. methyprylon. muscle. Cohen. theophylline. propxyphene. secobarbital. J. interfering phenytoin. Parissi-Poulou. methotrexate. maprotiline. 22. amikacin. 2511-2538 [also acetaminophen. liver.. 1986. nitrazepam. propranolol. J. D. oxazepam.230. A SepPak HPLC method for tricyclic antidepressant drugs in human vitreous humor. tissue. Tissue distribution of amitriptyline after repeated administration in rats. 1986. dialysate.Chromatogr.Chromatogr. 1994. M. brain. Iga. codeine. liver] Wong.. glutethimide. J. column temp 35. carbamazepine. tocainide. flurazepam. pharmacokinetics] Piperaki. tissue. lidocaine. Kotaki. 1989.Liq. disopyramide. quinidine. non-interfering alprazolam. streptomycin. bromazepam. salicylic acid.. TB. An investigation of the metabolism of amitriptyline using high performance liquid chromatography. lorazepam. chlorpromazine. Tricyclic antidepressant analysis by reversed-phase liquid chromatography using phenyl columns. phenytoin. Simultaneous determination of amitriptyline. McHugh.OTHER SUBSTANCES Simultaneous: metabolites. amitriptyline. imipramine. amitriptyline and nortriptyline in serum and plasma by high-performance liquid chromatography. barbital.Chromatogr.Liq. J. phenobarbital. 1993.. propranolol. J. J. S. J.ToxicoL.H.M. amitriptyline. Morgan. Drug Metab.. protriptyline. lorazepam. amoxapine. phenytoin. Engstrand. digoxin. M. netilmicin. diazepam. perphenazine.Dispos.Chromatogr.K. propoxyphene.. H. Tsarpalis. maprotiline. M. ethosuximide. 3487-3508 [also amitriptyline. procainamide. prazepam. 9. A. doxepin. meperidine.. Dolan. meprobamate. Koutselinis. nortriptyline and their respective isomeric 10-hydroxy metabolites in plasma by liquid chromatography. phenobarbital. theophylline. methapyriline. kidney. artane.A. 1980. cyclosporine. methaqualone. kanamycin. doxepin. vancomycin REFERENCE Evenson. protriptyline] Smith. 1727-1745 [extracted amitriptyline.. 1982. LOQ 10 ng/mL. triazolam] Oshima. simultaneous chlordiazepoxide. T. pentobarbital. S. clomipramine.Liq. flurazepam. 321-329 . Cooper..L. primidone. desipramine. CS. K. imipramine.Y. Abramson. doxepin.. clomipramine. imipramine. Koupparis. caffeine.. pseudoephedrine.F. lung. A separation study of tricyclic antidepressant drugs by HPLC with (3-cyclodextrin bonded stationary phase. chloripramine. maprotiline. pentobarbital. chlordiazepoxide. clonazepam. 9. K.Liq. Determination of amitriptyline-N-oxide.L. phenobarbital. R.Chromatogr.. clomipramine (IS). secobarbital. S. diazepam.A. doxepin. Sawada. A modified simple and rapid reversed phase high performance liquid chromatographic method for quantification of amitriptyline and nortriptyline in plasma.Chromatogr.. J. cimetidine.. 13. 322-325 • • • ANNOTATED BIBLIOGRAPHY Atta-Politou. J. trazodone] Suckow. 1994. thioridazine. heart. 17. S. Y. gentamicin. plasma.A. N-acetylprocainamide. chlorpromazine. LOD 5 ng/mL. 3969-3982 [extracted amitriptyline. diazepam... 16. rat. fluphenazine.. imipramine Noninterfering: acetaminophen.