fluridol, pentazocine, phencyclidine, phenobarbital, phenol, phenylbutazone, pimozide, pindolol, pipamperone, piroxicam, prazepam, prazosin, prilocaine, procainamide, procarbazine,

proguanil, promethazine, propafenone, propranolol, protriptyline, pyrimethamine, quinidine, quinine, quinupramine, ramipril, ranitidine, reserpine, ritodrine, secobarbital, sotalol, strychnine, sulfinpyrazole, sulindac, sulpride, sultopride, suriclone, temazepam, tenoxicam, terbutaline, terfenadine, tetracaine, tetrazepam, thiopental, thioproperazine, thioridazine, tianeptine, tiapride, tiaprofenic acid, ticlopidine, timolol, tioclomarol, tofisopam, tolbutamide, toloxatone, trazodone, triazolam, trifluoperazine, trifluperidol, trimipramine, triprolidine, tropatenine, verapamil, viloxazine, vincristine, vindesine, warfarin, yohimbine, zolpidem, zopiclone, zorubicine Interfering: bisoprolol, cetirizine, chlorpheniramine, cibenzoline, diltiazem, glibornuride, ioprazolam, medifoxamine, moperone, nicardipine, vinblastine KEYWORDS whole blood; plasma REFERENCE
Tracqui, A.; Kintz, P.; Mangin, P. Systematic toxicological analysis using HPLC/DAD. J.Forensic ScL, 1995, 40, 254-262

SAMPLE Matrix: blood, tissue Sample preparation: Plasma. 2 mL Plasma + 100 jxL 1 jxg/mL IS in MeOH + 2 mL 50 mM borax solution + 4 mL heptane: isoamyl alcohol 95:5, rotate at 10 rpm for 10 min, centrifuge at 1000 g for 5 min. Remove upper organic layer and repeat extraction of aqueous layer. Combine extracts, add 3 mL 50 mM sulfuric acid, extract. Remove acidic aqueous phase and make it alkaline with concentrated ammonia, extract twice with 2 mL heptane: isoamyl alcohol 95:5, combine organic layers and evaporate them to dryness under a stream of nitrogen at 55, take up in 50 |xL MeOH, inject the whole sample. Tissue. Grind tissue in a Waring blender, homogenize 1:4 in water. 2 mL homogenate + 100 |xL 1 |xg/mL IS in MeOH + 2 mL 50 mM borax solution + 4 mL heptane: isoamyl alcohol 95:5, rotate at 10 rpm for 10 min, centrifuge at 1000 g for 5 min. Remove upper organic layer and repeat extraction of aqueous layer. Combine extracts, add 3 mL 50 mM sulfuric acid, extract. Remove acidic aqueous phase and make it alkaline with concentrated ammonia, extract twice with 2 mL heptane: isoamyl alcohol 95:5, combine organic layers and evaporate them to dryness under a stream of nitrogen at 55, take up in 50 |xL MeOH, inject the whole sample. HPLCVARIABLES Column: 150 X 2.1 5 |xm Alltech RSiL C18HL Mobile phase: MeCN.water 50:50 + 0.05% diethylamine Flow rate: 0.6 Injection volume: 50 Detector: UV 254 CHROMATOGRAM Retention time: 5.8 Internal standard: l-[(4-fluorophenyl)methyl]-N-{l-[2-(4-ethoxyphenyl)ethyl]-4-piperidinyl}-lH-benzimidazol-2-amine (R 44 180) (8.3) Limit of detection: 1 ng/mL (plasma); 5 ng/g (tissue) OTHER SUBSTANCES Extracted: metabolites, desmethylastemizole KEYWORDS plasma; human; dog

Astemizole
Molecular formula: C28H31FN4O Molecular weight: 458.6 CAS Registry No.: 68844-77-9

SAMPLE Matrix: blood Sample preparation: 2 mL Whole blood or plasma + 2 mL buffer + 5 mL chloroform: isopropanol: n-heptane 60:14:26, shake gently horizontally for 10 min, centrifuge at 2800 g for 10 min. Remove the lower organic layer and evaporate it to dryness under vacuum at 45, reconstitute the residue in 100 |xL mobile phase, centrifuge at 2800 g for 5 min, inject a 50 |xL aliquot of the supernatant. (Buffer was saturated ammonium chloride solution 25% diluted with water, adjusted to pH 9.5 with 25% ammonia solution.) HPLCVARIABLES Column: 300 X 3.9 4 |xm NovaPack C18 Mobile phase: MeOH: THF: buffer 65:5:30 (Buffer was 0.68 g/L (10 mM (sic)) KH2PO4 adjusted to pH 2.6 with concentrated orthophosphoric acid.) (At the end of each session wash the column with water for 1 h and MeOH for 1 h, re-equilibrate for 30 min.) Column temperature: 30 Flow rate: 0.8 Injection volume: 50 Detector: UV 278 CHROMATOGRAM Retention time: 5.73 Limit of detection: <120 ng/mL OTHER SUBSTANCES Extracted: acebutolol, acenocoumarol, acepromazine, aceprometazine, acetaminophen, aconitine, ajmaline, albuterol, alimemazine, alminoprofen, alpidem, alprazolam, alprenolol, amisulpride, amitriptyline, amodiaquine, amoxapine, aspirin, atenolol, benazepril, benperidol, benzocaine, benzoylecgonine, bepridil, betaxolol, bromazepam, brompheniramine, bumadizone, bupivacaine, buprenorphine, buspirone, caffeine, carbamazepine, carbinoxamine, carpipramine, carteolol, celiprolol, chlorambucil, chlordiazepoxide, chlormezanone, chlorophenacinone, chloroquine, chlorpromazine, chlorpropamide, cicletanine, clemastine, clobazam, clomipramine, clonazepam, clonidine, clorazepate, clozapine, cocaine, codeine, colchicine, cyamemazine, cyclizine, cycloguanil, cyproheptadine, cytarabine, dacarbazine, daunorubicin, debrisoquine, demexiptiline, desipramine, dextromethorphan, dextromoramide, dextropropoxyphene, diazepam, diazoxide, diclofenac, dihydralazine, diphenhydramine, dipyridamole, disopyramide, dosulepine, doxepin, doxylamine, droperidol, ephedrine, estazolam, etodolac, fenfluramine, fenoprofen, fentiazac, flecainide, floctafenine, flumazenil, flunitrazepam, fluoxetine, fluphenazine, flurbiprofen, fluvoxamine, glibenclamide, glipizide, glutethimide, haloperidol, histapyrrodine, hydroxychloroquine, hydroxyzine, ibuprofen, imipramine, indomethacin, iproniazid, ketamine, ketoprofen, labetalol, levomepromazine, lidocaine, lidoflazine, lisinopril, loperamide, loratadine, lorazepam, loxapine, maprotiline, medazepam, mefenamic acid, mefenidramine, mefloquine, melphalan, meperidine, mephenesin, mephentermine, mepivacaine, metapramine, metformin, methadone, methaqualone, methocarbamol, methotrexate, metipranolol, metoclopramide, metoprolol, mexiletine, mianserine, midazolam, minoxidil, moclobemide, morphine, nadolol, nalbuphine, nalorphine, naloxone, naltrexone, naproxen, nialamide, nifedipine, niflumic acid, nimodipine, nitrazepam, nitrendipine, nizatidine, nomifensine, nortriptyline, omeprazole, opipramol, oxazepam, oxprenolol, penbutolol, pen-

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REFERENCE
Woestenborghs, R.; Embrechts, L.; Heykants, J. Simultaneous determination of astemizole and its demethylated metabolite in animal plasma and tissues by high-performance liquid chromatography J.Chromatogr., 1983, 278, 359-366

SAMPLE

Matrix: solutions Sample preparation: Inject an aliquot of a solution in MeOH.

HPLCVARIABLES

Column: 150 X 4.6 5 p,m MicroPack MCH-5 Mobile phase: MeOH: 30 mM pH 3.0 phosphate buffer 85:15 Flow rate: 1.5 Injection volume: 20 Detector: UV 276
REFERENCE
Fernandez Otero, G.C.; Lucangioli, S.E.; Carducci, CN. Adsorption of drugs in high-performance liquid chromatography injector loops. J.Chromatogr.A, 1993, 654, 87-91