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Albuterol
Molecular formula: C13H21NO3 Molecular weight: 239.3 CAS Registry No.: 18559-94-9, 51022-70-9 (sulfate)

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 jxL 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 226 CHROMATOGRAM Retention time: 3.37 Limit of detection: <120 ng/mL OTHER SUBSTANCES Extracted: acebutolol, acenocoumarol, acepromazine, aceprometazine, acetaminophen, aconitine, ajmaline, alimemazine, alminoprofen, alpidem, alprazolam, alprenolol, amisulpride, amitriptyline, amodiaquine, amoxapine, astemizole, benazepril, benperidol, benzocaine, benzoylecgonine, bepridil, betaxolol, bisoprolol, bromazepam, brompheniramine, bumadizone, bupivacaine, buprenorphine, buspirone, caffeine, carbamazepine, carbinoxamine, carpipramine, carteolol, celiprolol, cetirizine, chlorambucil, chlordiazepoxide, chlorophenacinone, chloroquine, chlorpheniramine, chlorpromazine, chlorpropamide, cibenzoline, cicletanine, clemastine, clobazam, clomipramine, clonazepam, clonidine, clorazepate, clozapine, cocaine, colchicine, cyamemazine, cyclizine, cycloguanil, cyproheptadine, cytarabine, dacarbazine, daunorubicin, debrisoquine, demexiptiline, desipramine, dextromethorphan, dextromoramide, dextropropoxyphene, diazepam, diazoxide, diclofenac, dihydralazine, diltiazem, diphenhydramine, dipyridamole, disopyramide, dosulepine, doxepin, doxylamine, droperidol, ephedrine, estazolam, etodolac, fenfluramine, fenoprofen, fentiazac, flecainide, floctafenine, flumazenil, flunitrazepam, fluoxetine, fluphenazine, flurbiprofen, fluvoxamine, glibenclamide, glibornuride, glipizide, glutethimide, haloperidol, histapyrrodine, hydroxychloroquine, hydroxyzine, ibuprofen, imipramine, indomethacin, iproniazid, ketamine, ketoprofen, labetalol, levomepromazine, lidocaine, lidoflazine, lisinopril, loperamide, loprazolam, loratadine, lorazepam, loxapine, maprotiline, medazepam, medifoxamine, mefenamic acid, mefenidramine, mefloquine, melphalan, meperidine, mephenesin, mephentermine, mepivacaine, metapramine, methadone, methaqualone, methocarbamol, methotrexate, metipranolol, metoclopramide, metoprolol, mexiletine, mianserine, midazolam, minoxidil, moclobemide, moperone, nadolol, nalbuphine, nalorphine, naloxone, naltrexone, naproxen, nialamide, nicardipine, nifedipine, niflumic acid, nimodipine, nitrazepam, nitrendipine, nizatidine, nomifensine, nortriptyline, omeprazole, opipramol, oxazepam, oxprenolol, penbutolol, penfluridol, pentazocine, phencyclidine, phenylbutazone, pimozide, pindolol, pipamperone, piroxicam,

prazepam, prazosin, prilocaine, procainamide, procarbazine, proguanil, promethazine, propafenone, propranolol, protriptyline, pyrimethamine, quinidine, quinine, quinupramine, ramipril, reserpine, secobarbital, sotalol, strychnine, sulfinpyrazole, sulindac, sulpride, suriclone, temazepam, tenoxicam, terfenadine, tetracaine, tetrazepam, thiopental, thioproperazine, thioridazine, tianeptine, tiaprofenic acid, ticlopidine, timolol, tioclomarol, tofisopam, tolbutamide, trazodone, triazolam, trifiuoperazine, trifluperidol, trimipramine, triprolidine, tropatenine, verapamil, viloxazine, vinblastine, vincristine, vindesine, warfarin, yohimbine, zolpidem, zopiclone, zorubicine Interfering: aspirin, atenolol, chlormezanone, codeine, metformin, morphine, phenobarbital, phenol, ranitidine, ritodrine, sultopride, terbutaline, tiapride, toloxatone 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 Sample preparation: Condition a Sep-Pak SPE cartridge with 10 mL MeOH and 10 mL water. 500 |xL Serum + 1 mL water + 15 |xL 100 ng/mL fenoterol in water, mix, force slowly through SPE cartridge, wash twice with 2 mL water, elute with 2 mL MeOH (discard first 2 drops). Evaporate eluate to dryness under a stream of nitrogen at 40, vortex for 1 min with 70 |xL buffer + 300 |xL 0.05% di(2-ethylhexyl) phosphate in ethyl acetate, centrifuge at 5000 g for 30 s, transfer organic phase to another tube and add 40 |xL buffer to it, vortex for 1 min, centrifuge at 5000 g for 30 s, transfer ethyl acetate layer to another tube and add 70 JJLL 10 mM HCl to it, vortex 1 min, centrifuge at 5000 g for 30 s, remove acid layer and wash it with 150 fxL chloroform, centrifuge at 5000 g for 30 s, inject a 40-60 |xL aliquot of the aqueous phase. (Buffer was 70 mM NaH2PO4 + 1 mM chloride + 2 mM 1-heptanesulfonic acid, pH 6.8.) HPLCVARIABLES Column: 75 X 4.6 3 jxm Ultrasphere ODS Mobile phase: MeOH: buffer 25:75 (Buffer was 70 mM NaH2PO4 + 1 mM chloride + 2 mM 1-heptanesulfonic acid, pH 6.8.) Flow rate: 0.5 Injection volume: 40-60 Detector: E, BioAnalytical System Model LC-4, TL-5 glassy carbon working electrode, Ag/AgCl reference electrode, +0.80 V, 10 nA full scale CHROMATOGRAM Retention time: 7 Internal standard: fenoterol (13) Limit of detection: 0.4 ng/mL OTHER SUBSTANCES Noninterfering: buphenine, carbamazepine, dobutamine, epinephrine, ethosuximide, gentamycin, isoproterenol, isoxsuprine, metaproterenol, metaraminol, oxymetazoline, phenobarbital, phentolamine, phenylephrine, phenytoin, primidone, terbutaline, theophylline, valproic acid KEYWORDS serum; heparin interferes with IS; SPE; pharmacokinetics

REFERENCE
Tan, YK.; Soldin, S.J. Determination of salbutamol in human serum by reversed-phase high-performance liquid chromatography with amperometric detection. J.Chromatogr., 1984, 311, 311-317

SAMPLE Matrix: blood, urine Sample preparation: Condition a 1 mL 100 mg (or 2.8 mL 500 mg) Extract-Clean silica SPE cartridge (Alltech) with 1 volume MeCN and 1 volume water. Add 1 mL urine or 3 mL plasma to the SPE cartridge, dry, wash with 1 volume water, wash with 1 volume MeCN, dry, elute with 2 volumes MeOH. Evaporate the eluate under reduced pressure at 45, reconstitute with 1 (urine) or 0.3 (plasma) mL mobile phase, vortex for 1 min, inject an aliquot. HPLCVARIABLES Guard column: 30 X 4 Chirex 3022 naphthyl urea (Phenomenex) Column: 250 X 4 Chirex naphthyl urea (Phenomenex) Mobile phase: Hexane:l,2-dichloromethane (sic):MeOH:trifluoroacetic acid 60.75:35: 4.25:0.25 Flow rate: 1 Injection volume: 200 Detector: F ex 220 em 309 CHROMATOGRAM Retention time: 22 (S-(+)), 27 (R-(-)) Limit of detection: 0.25 ng/mL KEYWORDS chiral; plasma; SPE; pharmacokinetics REFERENCE
Boulton, D.W.; Fawcett, J.P. Determination of salbutamol enantiomers in human plasma and urine by chiral high-performance liquid chromatography. J.Chromatogr.B, 1995, 672, 103-109

SAMPLE Matrix: blood, urine Sample preparation: Condition a 100 mg Baxter C18 SPE cartridge with one volume MeOH and two volumes water. Dilute 10 |xL urine to 500 |xL with water. 500 |xL Serum or diluted urine + 50 |xL water, vortex for 30 s, add to SPE cartridge, wash with three 200 |xL aliquots of water, elute with two 500 |xL aliquots of MeOH. Evaporate the eluates to dryness under a stream of air at 40-45, reconstitute the residue in 150 u,L water, vortex for 30 s, centrifuge at 14000 g for 4 min, inject a 50 \xL aliqu HPLC VARIABLES Guard column: 5 |xm Adsorbosphere C-18 Column: 250 X 4.6 5 |xm Adsorbosphere C-18 Mobile phase: MeCN: buffer 7:93 adjusted to pH 3.0 with 85% phosphoric acid (Buffer was 25 mM (NH4)H2PO4 and 1 mM N,N-dimethyloctylamine.) Flow rate: 1.5 Injection volume: 50 Detector: UV 224; F ex 228 em 310 CHROMATOGRAM Retention time: 7.1 Internal standard: albuterol

OTHER SUBSTANCES Extracted: atenolol

KEYWORDS

serum; SPE; albuterol is IS

REFERENCE
Chatterjee, D.J.; Li, W.Y; Hurst, A.K.; Koda, R.T. High-performance liquid chromatographic method for determination of atenolol from human plasma and urine: Simultaneous fluorescence and ultraviolet detection. J.Liq.Chromatogr., 1995, 18, 791-806

SAMPLE

Matrix: bulk Sample preparation: Inject a 5 |xL aliquot of a solution.

HPLCVARIABLES

Column: 250 X 4.6 5 u,m LiChrosphere Diol Mobile phase: Gradient. Carbon dioxide:MeOH containing 0.5% n-propylamine 70:30 for 9.5 min, to 55:45 over 12 min. Column temperature: 70 Flow rate: 1.5 Injection volume: 5 Detector: UV
CHROMATOGRAM

Retention time: 6.2 Limit of detection: 1.3 |xg/mL OTHER SUBSTANCES Simultaneous: impurities
KEYWORDS

300 bar; SFC

REFERENCE
Bernal, J.L.; del Nozal, M.J.; Rivera, J.M.; Serna, M.L.; Toribo, L. Separation of salbutamol and six related impurities by packed column supercritical fluid chromatography. Chromatographia, 1996,42, 89-94

SAMPLE

Matrix: formulations Sample preparation: Dilute with water to a concentration of 833 |Jig/mL, add a 300 |xL aliquot to 250 JJLL 2 mg/mL mepivacaine hydrochloride in water, vortex, inject a 10 u-L aliquot.
HPLCVARIABLES

Column: 100 X 8 4 |xm NovaPak C18 radial compression Mobile phase: Gradient. A was 2.5 mM PIC B-8 Low UV (Waters) in THF: water 40:60. B was water. C was MeOH: water 50:50. A:B:C 50:50:0 for 7.7 min, to 60:15:25 over 5.3 min, re-equilibrate at initial conditions for 5 min. Flow rate: 2 Injection volume: 10 Detector: UV 220
CHROMATOGRAM

Retention time: 3.2 Internal standard: mepivacaine (8.2)

OTHER SUBSTANCES Simultaneous: fenoterol, ipratropium bromide, terbutaline KEYWORDS nebulizer solutions; stability-indicating REFERENCE
Jacobson, G.A.; Peterson, G.M. High-performance liquid chromatographic assay for the simultaneous determination of ipratropium bromide, fenoterol, salbutamol and terbutaline in nebulizer solution. J.Pharm.Biomed.Anal, 1994, 12, 825-832

SAMPLE Matrix: formulations Sample preparation: Tablets, capsules. Mix tablets or capsules with 10 mL water, sonicate 30 min, centrifuge, inject an aliquot of the supernatant. Liquid formulations. Dilute liquid formulations with water, inject an aliquot. HPLCVARIABLES Column: 125 X 4 5 jxm LiChrospher 100 RP-18 endcapped Mobile phase: MeOH-.water 40:60 containing 2 mM KOH + 10 mM hexanoic acid Flow rate: 0.4 Injection volume: 20 Detector: UV 214 CHROMATOGRAM Retention time: 3.5 Limit of detection: 1760 ng/mL OTHER SUBSTANCES Also analyzed: terbutaline, fenoterol KEYWORDS tablets; capsules; liquid formulations REFERENCE
Ackermans, M.T.; Beckers, J.L.; Everaerts, RM.; Seelen, LG. Comparison of isotachophoresis, capillary zone electrophoresis and high-performance liquid chromatography for the determination of salbutamol, terbutaline sulphate and fenoterol hydrobromide in pharmaceutical dosage forms. J.Chromatogr., 1992, 590, 341-353

SAMPLE Matrix: blood Sample preparation: Condition a 1 mL Bond Elut silica (not C18) SPE cartridge twice with 1 mL MeOH and with 1 mL water. 1 mL Plasma + 200 jxL 50 \xg/mL bamethan sulfate in 1% potassium bicarbonate, add to SPE cartridge without applying vacuum, after 2 min apply vacuum to move samples through at 1 mL/min then increase vacuum to remove all liquid. Wash twice with 1 mL water and with 1 mL MeCN (draining completely each time). Elute with 1 mL MeOH, expelling last drop with positive pressure. Evaporate eluate under vacuum without heating, dissolve residue in 40 jxL mobile phase, vortex, centrifuge at 300 g for 20 s, inject whole sample. HPLCVARIABLES Guard column: 15 X 3.2 Brownlee 7 |xm C8 Column: 150 X 4.6 5 |xm Ultrasphere Octylsilica

Mobile phase: MeCN: MeOH: water: phosphoric acid: KH2PO4: octanesulfonic acid 50:150: 900:0.25:0.75:0.05 (v/v/v/v/w/w) Flow rate: 1.6 Injection volume: 40 Detector: F ex 275 em 310
CHROMATOGRAM Retention time: 7

Internal standard: bamethan sulfate (17.5) Limit of quantitation: 0.2 ng/mL

KEYWORDS

SPE; plasma
REFERENCE
Gupta, R.N.; Fuller, H.D.; Dolovich, M.B. Optimization of a column liquid chromatographic procedure for the determination of plasma salbutamol concentrations. J.Chromatogr.B, 1994, 654, 205-211

SAMPLE

Matrix: blood Sample preparation: Condition a Bond Elut Si SPE cartridge by washing twice with 1 mL MeOH, twice with 1 mL water, and once with 1 mL 100 mM pH 9.2 K2HPO4. Add 1 mL plasma + 100 |JLL 500 ng/mL atenolol in water, wash twice with 1 mL water, centrifuge at 1000 g for 5 min, elute with 1 mL MeOH. Evaporate MeOH to dryness at 40 under a stream of air and dissolve residue in 200 |xL mobile phase, inject an aliquot.
HPLCVARIABLES

Column: 250 X 4.6 Spherisorb S5 SCX Mobile phase: MeOH:MeCN: water 40:40:20 containing 0.2% perchloric acid (apparent pH 1.7) Flow rate: 1.5 Injection volume: 100 Detector: F ex 200 no emission filter
CHROMATOGRAM Retention time: 8

Internal standard: atenolol (13) Limit of detection: 1000 ng/mL

OTHER SUBSTANCES

Extracted: terbutaline Noninterfering: aminophylline, beclomethasone, cloprednol, dexamethasone, fenoterol, ipratropium bromide, methylprednisolone, orciprenaline, prednisolone, reproterol, rimiterol, salmeterol, sodium cromoglycate, theophylline
KEYWORDS

SPE; plasma
REFERENCE
McCarthy, P.T.; Atwal, S.; Sykes, A.P.; Ayres, J.G. Measurement of terbutaline and salbutamol in plasma by high performance liquid chromatography with fluorescence detection. Biomed.Chromatogr., 1993, 7, 25-28

SAMPLE Matrix: blood

Sample preparation: Condition a 1 mL Bond-Elut octadecylsilane SPE cartridge with 2 mL MeOH, 2 mL water, and 2 mL buffer (do not allow to dry). 1 mL Serum H - 10 jxL 100 (xg/mL bamethan in water + 2 mL buffer, mix, add to SPE cartridge, wash with 1 mL buffer, 2 mL water, 2 mL MeOHrMeCN 15:85. Dry under full vacuum for 10 min and elute with 1 mL MeOH. Evaporate the eluate to dryness under a stream of nitrogen at room temperature. Dissolve the residue in 200 JJLL MeCN: triethylamine 199:1, heat at 45for 20 min, add 10 jxL 5 mg/mL TAGIT in MeCN, heat at 45for 2 h. Evaporate at room temperature under a stream of nitrogen, reconstitute in 250 fxL mobile phase, inject a 100 |xL aliquot. (Buffer was 100 mM Na2HPO4 adjusted to pH 7.3 with concentrated phosphoric acid. The chiral derivatizing agent TAGIT was 2,3,4,6-tetra-O-acetyl-|3-D-glucopyranosyl isothiocyanate. Prepare solutions of TAGIT in MeCN weekly.) HPLCVARIABLES Column: 100 X 4.6 5 |xm Brownlee octadecylsilyl Mobile phase: MeCN: water 29:71 containing 0.1% triethylamine (pH adjusted to 4.0 with concentrated phosphoric acid) Flow rate: 0.8 Injection volume: 100 Detector: F ex 223 no emission filter CHROMATOGRAM Retention time: 5.77 (R(-)), 6.83 (S(+)) Internal standard: bamethan (9, 10) Limit of detection: 1 ng/mL KEYWORDS SPE; chiral; derivatization; serum REFERENCE
He, L.; Stewart, J.T. A high performance liquid chromatographic method for the determination of albuterol enantiomers in human serum using solid phase extraction and chemical derivatization. Biomed.Chromatogr., 1992, 6, 291-294

SAMPLE Matrix: solutions Sample preparation: Dilute 800 |xL solution to 10 mL with water, filter, inject a 20 |xL aliquot of the filtrate. HPLC VARIABLES Guard column: RP-18 Column: 125 X 4 5 |xm LiChrosorb RP-18 Mobile phase: Gradient. MeCN-.buffer 4:96 for 6 min, to 9:91 (step gradient). (Buffer was 40 mM NaH2PO4 containing 5.74 mM triethylamine, adjusted to pH 3.0 with phosphoric acid.) Flow rate: 1.5 Injection volume: 20 Detector: UV 265 KEYWORDS comparison with capillary electrophoresis REFERENCE
Malkki-Laine, L.; Hartikainen, E. Electrokinetic behaviour of salbutamol and its decomposition products and determination of salbutamol by micellar electrokinetic capillary chromatography. J.Chromatogr.A, 1996, 724, 297-306

SAMPLE Matrix: solutions HPLCVARIABLES Column: 250 X 4.6 CSP-4 (Prepare as follows. Add a solution of 1.07 g L-valyl-L-valyl-Lvaline isopropylester (Bunseki Kagaku 1979, 28, 125) in 30 mL dry dioxane (Caution! Dioxane is a carcinogen!) dropwise to a mixture of 2.2 g 2,4,6-trichloro-l,3,5-triazine (cyanuric chloride) in 20 mL dry dioxane stirred at 0, add 3 g anhydrous sodium carbonate at room temperature, stir, filter, evaporate to give a colorless solid. Dissolve 8.3 g of this solid in 30 mL dry dioxane, add 2 g N-(2-aminoethyl)-3-aminopropyltrimethoxysilane, add 1.5 g anhydrous sodium carbonate, reflux with stirring for 40 h, filter, add 3 g dried 10 juim LiChrosorb Si 100, reflux with slow stirring for 10 h, cool, filter. Wash the solid with dioxane, MeOH, and diethyl ether, dry under reduced pressure (J.Chromatogr. 1984, 292, 427).) Mobile phase: Hexane: 1,2-dichloroethane:MeOH:trifluoroacetic acid 60:37.5:3.75:0.25 Detector: UV CHROMATOGRAM Retention time: k' 5.84 (first enantiomer) KEYWORDS chiral; a = 1.06 REFERENCE
Oi, N.; Kitahara, H.; Matsushita, Y.; Kisu, N. Enantiomer separation by gas and high-performance liquid chromatography with tripeptide derivatives as chiral stationary phases. J.Chromatogr.A, 1996, 722, 229-232

SAMPLE Matrix: solutions Sample preparation: Inject an aliquot of a 200 |xM solution in MeOH. HPLCVARIABLES Column: 100 X 4.7 7 |xm Hypercarb (Shandon) Mobile phase: MeOH containing 5 mM N-benzyloxycarbonylglycyl-L-proline and 4.5 mM NaOH Column temperature: 17 Injection volume: 20 Detector: UV 270 CHROMATOGRAM Retention time: k' 3.2 (first enantiomer) KEYWORDS chiral; a = 1.09 REFERENCE
Huynh, N.-H.; Karlsson, A.; Pettersson, C. Enantiomeric separation of basic drugs using N-benzyloxycarbonylglyclyl-L-proline as counter ion in methanol. J.Chromatogr.A, 1995, 705, 275-287

SAMPLE Matrix: solutions HPLC VARIABLES Column: 250 x 4.6 5 |xm Supelcosil LC-DP (A) or 250 X 4 5 |xm LiChrospher 100 RP-8 (B)

Mobile phase: MeCN:0.025% 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, adjust pH to 3.4 with dilute phosphoric acid, make up to 1 L.) Flow rate: 0.6 Injection volume: 25 Detector: UV 229 CHROMATOGRAM Retention time: 5.57 (A), 3.27 (B) OTHER SUBSTANCES Also analyzed: acebutolol, acepromazine, acetaminophen, acetazolamide, acetophenazine, alprazolam, amitriptyline, amobarbital, amoxapine, antipyrine, atenolol, atropine, azatadine, baclofen, benzocaine, bromocriptine, brompheniramine, brotizolam, bupivacaine, buspirone, butabarbital, butalbital, caffeine, carbamazepine, cetirizine, chlorcyclizine, chlordiazepoxide, chlormezanone, chloroquine, chlorpheniramine, chlorpromazine, chlorpropamide, chlorprothixene, chlorthalidone, chlorzoxazone, cimetidine, cisapride, clomipramine, clonazepam, clonidine, clozapine, cocaine, codeine, colchicine, cyclizine, cyclobenzaprine, dantrolene, desipramine, diazepam, diclofenac, diflunisal, diltiazem, diphenhydramine, diphenidol, diphenoxylate, dipyridamole, disopyramide, dobutamine, doxapram, doxepin, droperidol, encainide, ethidium bromide, ethopropazine, fenoprofen, fentanyl, flavoxate, fluoxetine, fluphenazine, flurazepam, flurbiprofen, fluvoxamine, furosemide, glutethimide, glyburide, guaifenesin, haloperidol, homatropine, hydralazine, hydrochlorothiazide, hydrocodone, hydromorphone, hydroxychloroquine, hydroxyzine, ibuprofen, imipramine, indomethacin, ketoconazole, ketoprofen, ketorolac, labetalol, Ievorphanol, lidocaine, loratadine, lorazepam, lovastatin, loxapine, mazindol, mefenamic acid, meperidine, mephenytoin, mepivacaine, mesoridazine, metaproterenol, methadone, methdilazine, methocarbamol, methotrexate, methotrimeprazine, methoxamine, methyldopa, methylphenidate, metoclopramide, metolazone, metoprolol, metronidazole, midazolam, moclobemide, morphine, nadolol, nalbuphine, naloxone, naphazoline, naproxen, nifedipine, nizatidine, norepinephrine, nortriptyline, oxazepam, oxycodone, oxymetazoline, paroxetine, pemoline, pentazocine, pentobarbital, pentoxifylline, perphenazine, pheniramine, phenobarbital, phenol, phenolphthalein, phentolamine, phenylbutazone, phenyltoloxamine, phenytoin, pimozide, pindolol, piroxicam, pramoxine, prazepam, prazosin, probenecid, procainamide, procaine, prochlorperazine, procyclidine, promazine, promethazine, propafenone, propantheline, propiomazine, propofol, propranolol, protriptyline, quazepam, quinidine, quinine, racemethorphan, ranitidine, remoxipride, risperidone, salicylic acid, scopolamine, secobarbital, sertraline, sotalol, spironolactone, sulfinpyrazone, sulindac, temazepam, terbutaline, terfenadine, tetracaine, theophylline, thiethylperazine, thiopental, thioridazine, thiothixene, timolol, tocainide, tolbutamide, tolmetin, trazodone, triamterene, triazolam, trifluoperazine, triflupromazine, trimeprazine, trimethoprim, trimipramine, verapamil, warfarin, xylometazoline, yohimbine, zopiclone KEYWORDS details of plasma extraction also in paper REFERENCE
Koves, E.M. Use of high-performance liquid chromatography-diode array detection in forensic toxicology. J.Chromatogr.A, 1995, 692, 103-119

SAMPLE Matrix: solutions HPLCVARIABLES Column: 250 X 4.6 Sumchiral CSP 10 (Sumika Chemical Analysis Service) Mobile phase: n-Hexane: 1,2-dichloroethane: MeOH: trifluoroacetic acid 250:140:20:1

Flow rate: 1 Detector: UV 230-280 CHROMATOGRAM Retention time: k' 5.41 (first enantiomer) KEYWORDS chiral; a = 1.33 REFERENCE
Oi, N.; Kitahara, H.; Aoki, F. Direct enantiomer separations by high-performance liquid chromatography with chiral urea derivatives as stationary phases. J.Chromatogr.A, 1995, 694, 129-134

SAMPLE Matrix: solutions HPLCVARIABLES Column: 250 X 4.6 Zorbax RX Mobile phase: Gradient. A was 10 mL concentrated orthophosphoric acid and 7 mL triethylamine in 1 L water. B was 10 mL concentrated orthophosphoric acid and 7 mL triethylamine in 200 mL water, make up to 1 L with MeCN. A:B from 100:0 to 0:100 over 30 min, maintain at 0:100 for 5 min. Column temperature: 30 Flow rate: 2 Detector: UV 210 OTHER SUBSTANCES Also analyzed: 5-fluorouracil, acepromazine, acetaminophen, acetophenazine, aminophylline, amitriptyline, amobarbital, amoxapine, amphetamine, amylocaine, antipyrine, aprobarbital, aspirin, atenolol, atropine, avermectin, barbital, bebrisoquine, benzocaine, benzoic acid, benzotropine, benzphetamine, berberine, bibucaine, bromazepan, brompheniramine, buprenorphine, buspirone, butabarbital, butacaine, butethal, caffeine, carbamazepine, carbromal, chloramphenicol, chlordiazepoxide, chloroquine, chlorothiazide, chloroxylenol, chlorphenesin, chlorpheniramine, chlorpromazine, chlorpropamide, chlortetracycline, cimetidine, cinchonidine, cinchonine, clenbuterol, clonazepam, clonixin, clorazepate, cocaine, codeine, colchicine, cortisone, coumarin, cyclazocine, cyclobenzaprine, cyclothiazide, cyheptamide, cymarin, danazol, danthron, dapsone, desipramine, dexamethasone, dextromethorphan, dextropropoxyphene, diamorphine, diazepam, diclofenac, diethylpropion, diethylstilbestrol, diflunisal, digitoxin, digoxin, diltiazem, diphenhydramine, diphenoxylate, diprenorphine, dipyrone, disulfiram, dopamine, doxapram, doxepin, dronabinol, ephedrine, epinephrine, epinine, estradiol, estriol, estrone, ethacrynic acid, ethosuximide, etonitazene, etorphine, eugenol, famotidine, fenbendazole, fencamfamine, fenoprofen, fenproporex, fentanyl, flubendazole, flufenamic acid, flunitrazepam, fluoxymesterone, fluphenazine, furosemide, gentisic acid, gitoxigenin, glipizide, glunixin, glutethimide, glybenclamide, guaiacol, halazepam, haloperidol, hydrochlorothiazide, hydrocodone, hydrocortisone, hydromorphone, hydroxyquinoline, ibogaine, ibuprofen, iminostilbene, imipramine, indomethacin, isocarbostyril, isocarboxazid, isoniazid, isoproterenol, isoxsuprine, ivermectin, ketamine, ketoprofen, kynurenic acid, levorphanol, lidocaine, lorazepam, lormetazepam, loxapine, mazindol, mebendazole, meclizine, meclofenamic acid, medazepam, mefenamic acid, megestrol, mepacrine, meperidine, mephentermine, mephenytoin, mephesin, mephobarbital, mepivacaine, mescaline, mesoridazine, methadone, methamphetamine, methapyrilene, methaqualone, methazolamide, methocarbamol, methoxamine, methsuximide, methyl salicylate, methyldopa, methyldopamine, methylphenidate, methylprednisolone, methyltestosterone, methyprylon, metoprolol, mibolerone, morphine, nadolol, nalorphine, naloxone, naltrexone, naphazoline, naproxen, nefopam, niacinamide, nicotine, nicotinic acid, nifedipine, niflumic acid, nitrazepam, norepinephrine, nortriptyline, noscapine, nylidrin, oxazepam, oxycodone, oxymorphone,

oxyphenbutazone, oxytetracycline, papaverine, pargyline, pemoline, pentazocine, pentobarbital, persantine, phenacetin, phenazocine, phenazopyridine, phencyclidine, phendimetrazine, phenelzine, pheniramine, phenobarbital, phenothiazine, phensuximide, phentermine, phenylbutazone, phenylephrine, phenylpropanolamine, piperocaine, prazepam, prednisolone, primidone, probenecid, progesterone, propiomazine, propranolol, propylparaben, pseudoephedrine, puromycin, pyrilamine, pyrithyldione, quazepam, quinaldic acid, quinidine, quinine, ranitidine, recinnamine, reserpine, resorcinol, saccharin, albuterol, salicylamide, salicylic acid, scopolamine, scopoletin, secobarbital, strychnine, sulfacetamide, sufadiazine, sulfadimethoxine, sulfaethidole, sulfamerazine, sulfamethazine, sulfamethoxizole, sulfanilamide, sulfapyridine, sulfasoxizole, sulindac, tamoxifen, temazepam, testosterone, tetracaine, tetracycline, dronabinol, tetramisole, thebaine, theobromine, theophylline, thiabendazole, thiamine, thiamylal, thiobarbituric acid, thioridazine, thiosalicylic acid, thiothixene, thymol, tolazamide, tolazoline, tobutamide, tolmetin, tranylcypromine, triamcinolone, tribenzylamine, trichloromethiazide, trifluoperazine, trihexyphenidyl, trimethoprim, tripelennamine, triproilidine, tropacocaine, tyramine, verapamil, vincamine, warfarin, yohimbine, zoxazolamine REFERENCE
Hill, D.W.; Kind, A. J. Reversed-phase solvent gradient HPLC retention indexes of drugs. J.Anal.ToxicoL, 1994, 18, 233-242

SAMPLE Matrix: solutions Sample preparation: Prepare a 10 jjig/mL solution in MeOH, inject a 20 JULL aliquot. HPLCVARIABLES Column: 125 X 4.9 Spherisorb S5W silica Mobile phase: MeOH containing 10 mM ammonium perchlorate and 1 mL/L 100 mM NaOH in MeOH, pH 6.7

Flow rate: 2 Injection volume: 20

Detector: E, LeCarbone, V25 glassy carbon electrode, + 1.2 V CHROMATOGRAM Retention time: 1.76 OTHER SUBSTANCES Also analyzed: acebutolol, acepromazine, acetophenazine, N-acetylprocainamide, alprenolol, amethocaine, amiodarone, amitriptyline, antazoline, atenolol, azacyclonal, bamethane, benactyzine, benperidol, benzethidine, benzocaine, benzoctamine, benzphetamine, benzquinamide, bromhexine, bromodiphenhydramine, bromperidol, brompheniramine, brompromazine, buclizine, bufotenine, bupivacaine, buprenorphine, butacaine, butethamate, chlorcyclizine, chlorpheniramine, chlorphenoxamine, chlorprenaline, chlorpromazine, chlorprothixene, cimetidine, cinchonidine, cinnarizine, clemastine, clomipramine, clonidine, cocaine, cyclazocine, cyclizine, cyclopentamine, cyproheptadine, deserpidine, desipramine, dextromoramide, dextropropoxyphene, dicyclomine, diethylcarbamazine, diethylpropion, diethylthiambutene, dihydroergotamine, dimethindene, dimethothiazine, diphenhydramine, diphenoxylate, dipipanone, diprenorphine, dipyridamole, disopyramide, dothiepin, doxapram, doxepin, doxylamine, droperidol, ephedrine, ergocornine, ergocristine, ergocristinine, ergocryptine, ergometrine, ergosine, ergosinine, ergotamine, ethopropazine, etorphine, etoxeridine, fenethazine, fenfluramine, fenoterol, fentanyl, flavoxate, fluopromazine, flupenthixol, fluphenazine, flurazepam, haloperidol, hydroxyzine, hyoscine, ibogaine, imipramine, indapamine, iprindole, isothipendyl, isoxsuprine, ketanserin, laudanosine, lidocaine, lofepramine, loxapine, maprotiline, mecamylamine, meclophenoxate, meclozine, medazepam, mephentermine, mepivacaine, meptazinol, mepyramine, mesoridazine, metaraminol, methadone, methamphetamine, methapyrilene, methdilazene, methotrimeprazine, methoxamine, methoxyphenamine, methoxypromazine, meth-

ylephedrine, methylergonovine, methysergide, metoclopramide, metopimazine, metoprolol, mianserin, morazone, nadolol, nalorphine, naloxone, naphazoline, nicotine, nifedipine, nomifensine, nortriptyline, noscapine, orphenadrine, oxeladin, oxprenolol, oxymetazolin, papaverine, pargyline, pecazine, penbutolol, pentazocine, penthienate, pericyazine, perphenazine, phenadoxone, phenampromide, phenazocine, phenbutrazate, phendimetrazine, phenelzine, phenglutarimide, phenindamine, pheniramine, phenmetrazine, phenomorphan, phenoperidine, phenothiazine, phenoxybenzamine, phentolamine, phenylephrine, phenyltoloxamine, physostigmine, piminodine, pimozide, pindolol, pipamazine, pipazethate, piperacetazine, piperidolate, pipradol, pirenzepine, piritramide, pizotifen, practolol, pramoxine, prazosin, prenylamine, prilocaine, primaquine, proadifen, procainamide, procaine, prochlorperazine, procyclidine, proheptazine, prolintane, promazine, promethazine, pronethalol, properidine, propiomazine, propranolol, prothipendyl, protriptyline, proxymetacaine, pseudoephedrine, pyrimethamine, quinidine, quinine, ranitidine, rescinnamine, sotalol, tacrine, terazosin, terbutaline, terfenadine, thenyldiamine, theophylline, thiethylperazine, thiopropazate, thioproperazine, thioridazine, thiothixene, thonzylamine, timolol, tocainide, tolpropamine, tolycaine, tranylcypromine, trazodone, trifluoperazine, trifluperidol, trimeperidine, trimeprazine, trimethobenzamide, trimethbprim, trimipramine, tripelennamine, triprolidine, tryptamine, verapamil, xylometazoline REFERENCE Jane, L; McKinnon, A.; Flanagan, R. J. High-performance liquid chromatographic analysis of basic drugs on silica columns using non-aqueous ionic eluents. II. Application of UV, fluorescence and electrochemical oxidation detection. J.Chromatogr., 1985, 323, 191-225

ANNOTATED BIBLIOGRAPHY Tsai, CE.; Kondo, F. Liquid chromatographic determination of salbutamol and clenbuterol residues in swine serum and muscle. Microbios, 1994, 80, 251-258 Malkki, L.; Tammilehto, S. Optimization of the separation of salbutamol and its decomposition products by liquid chromatography with diode-array detection. J.Pharm.Biomed.AnaL, 1993, 11, 79-84 Nasr, M.M. Single-puff particle-size analysis of albuterol metered-dose inhalers (MDIs) by high-pressure liquid chromatography with electrochemical detection (HPLC-EC). Pharm.Res., 1993, 10, 1381-1384 Sagar, K.A.; Kelly, M.T.; Smyth, M.R. Simultaneous determination of salbutamol and terbutaline at overdose levels in human plasma by high performance liquid chromatography with electrochemical detection. Biomed.Chromatogr., 1993, 7, 29-33 Degroodt, J.M.; Wyhowski de Bukanski, B.; Srebrnik, S. Immunoaffinity-chromatography purification of salbutamol in liver and HPLC-fluorometric detection at trace residue level. Z.Lebensm. Unters.Forsch., 1992, 195, 566-568 Tamisier-Karolak, L.; Delhotal-Landes, B.; Jolliet-Riant, P.; Milliez, J.; Jannet, D.; Barre, J.; Flouvat, B. Plasma assay of salbutamol by means of high-performance liquid chromatography with amperometric determination using a loop column for injection of plasma extracts. Application to the evaluation of subcutaneous administration of salbutamol. Ther.Drug Monit., 1992, 14, 243248 Meyer, H.H.; Rinke, L.; Dursch, I. Residue screening for the beta-agonists clenbuterol, salbutamol and cimaterol in urine using enzyme immunoassay and high-performance liquid chromatography. J.Chromatogr., 1991, 564, 551-556 [extracted cimaterol, clenbuterol; urine; cow; SPE; enzyme immunoassay detection; UV detection] Wu, Y.Q.; Shi, R.; Williams, R.L.; Lin, E.T. High-performance liquid chromatographic assay for basic amine drugs in human plasma with a silica gel column and an aqueous mobile phase. IV. Albuterol. J.Liq.Chromatogr., 1991, 14, 253-264 [plasma; fluorescence detection; LOD 0.2 ng/mL; metaproterenol (IS)] Beaulieu, N.; Cyr, T.D.; Lovering, E.G. Liquid chromatographic methods for the determination of albuterol (salbutamol), albuterol sulphate and related compounds in drug raw materials, tablets and inhalers. J.Pharm.Biomed.AnaL, 1990, 8, 583-589 Bland, R.E.; Tanner, R.J.; Chern, WH.; Lang, J.R.; Powell, J.R. Determination of albuterol concentrations in human plasma using solid-phase extraction and high-performance liquid chromatography with fluorescence detection. J.Pharm.Biomed.AnaL, 1990, 8, 591-596

Ong, H.; Adam, A.; Perreault, S.; Marleau, S.; Bellemare, M.; Du Souich, P.; Beaulieu, N. Analysis of albuterol in human plasma based on immunoaffinity chromatographic clean-up combined with highperformance liquid chromatography with fluorimetric detection. J.Chromatogr., 1989, 497, 213221 Emm, T.; Lesko, L.J.; Leslie, J.; Perkal, M.B. Determination of albuterol in human serum by reversedphase high-performance liquid chromatography with electrochemical detection. J.Chromatogr., 1988, 427, 188-194 Tan, Y.K.; Soldin, S.J. Analysis of salbutamol enantiomers in human urine by chiral high-performance liquid chromatography and preliminary studies related to the stereoselective disposition kinetics in man. J.Chromatogr., 1987, 422, 187-195 Miller, L.G.; Greenblatt, D. J. Determination of albuterol in human plasma by high-performance liquid chromatography with fluorescence detection. J.Chromatogr., 1986, 381, 205-208 Kucharczyk, N.; Segelman, RH. Drug level monitoring of antiasthmatic drugs. J.Chromatogr., 1985, 340, 243-271 [review] Kurosawa, N.; Morishima, S.; Owada, E.; Ito, K. Reversed-phase high-performance liquid chromatographic determination of salbutamol in rabbit plasma. J.Chromatogr., 1984, 305, 485-488 [rabbit; plasma; column temp 60; SPE; LOD 4 ng/mL; pharmacokinetics] Eggers, N.J.; Saint-Joly, CM. The effect of amine modifiers on the chromatographic behavior of salbutamol on reversed phase chemically bonded silica gel. J.Liq.Chromatogr., 1983, 6, 1955-1967 Hutchings, M.J.; Paull, J.D.; Morgan, D.J. Determination of salbutamol in plasma by high-performance liquid chromatography with fluorescence detection. J.Chromatogr., 1983, 277, 423-426 [plasma; fluorescence detection; LOD 1 ng/mL; pharmacokinetics] Agostini, 0.; Chiari, A.; Ciofi Baffoni, D. Simultaneous high-performance liquid chromatographic determination of salbutamol sulphate, theophylline, and saccharin in a hydroalcoholic formulation. Boll.Chim.Farm., 1982, 121, 612-618 Oosterhuis, B.; van Boxtel, CJ. Determination of salbutamol in human plasma with bimodal highperformance liquid chromatography and a rotated disc amperometric detector. J.Chromatogr., 1982, 232, 327-334 [SPE; electrochemical detection; plasma; LOD 0.5 ng/mL; pharmacokinetics]