hplc analysis of albuterol

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    SAMPLEMatrix: bloodSample preparat ion: 2 mL Whole blood or plasma + 2 mL buffer + 5 mL chloroform:isopropanol: n-he ptan e 6 0:1 4:2 6, sh ak e gently horizontally for 10 min, centrifuge at 2800g for 10 min. Remove the lower organic layer and evaporate it to dryness under vacuumat 45, reconstitute the residue in 100 |xL mobile phase, centrifuge at 2800 g for 5 min,inject a 50 jxL aliquot of th e su pe rn ata nt. (Buffer w as sat ur ate d a mm onium chloridesolution 25% diluted with w ater, adjusted to pH 9.5 with 25% amm onia solution.)HPLCVARIABLESColumn: 300 X 3.9 4 |xm NovaPack C18Mobi le phase: M eOH :TH F:buffer 65 :5 :3 0 (Buffer wa s 0.68 g/L (10 mM (sic)) KH 2PO 4adjusted to pH 2.6 with concentrated orthophosphoric acid.) (At the end of each sessionwash the column with water for 1 h and MeOH for 1 h, re-equilibrate for 30 min.)Colum n tem peratu re: 30Flow rate: 0 .8Inject ion volum e: 50Detector: UV 226CHROMATOGRAMRetent ion t ime: 3.37Limit of detect ion:

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    prazepam, prazosin, prilocaine, procainamide, procarbazine, proguanil, promethazine,propafenone, propranolol, protriptyline, pyrimethamine, quinidine, quinine, quinupra-mine, ramipril, reserpine, secobarbital, sotalol, strychnine, sulfinpyrazole, sulindac, sul-pride, suriclone, temazepam, tenoxicam, terfenadine, tetracaine, tetrazepam, thiopental,thiopropera zine, th ioridazine , tian epti ne, tiaprofenic acid, ticlopidine, timolol, tioclomarol,tofisopam, tolbutamide, trazodone, triazolam, trifiuoperazine, trifluperidol, trimipramine,triprolidine, tropatenine, verapamil, viloxazine, vinblastine, vincristine, vindesine, war-farin, yohimbine, zolpidem, zopiclone, zorubicineInterfering: aspirin, atenolol, chlormezanone, codeine, metformin, morphine, phenobarbi-tal , phenol, ranitidine, ritodrine, sultopride, terbutaline, tiapride, toloxatone

    KEYWORDSwhole blood; plasmaREFERENCETracqui, A.; Kintz, P.; Mangin, P. Systematic toxicological analysis using HPLC/DAD. J.Forensic ScL,1995, 40, 254-262

    SAMPLEMatrix: bloodSample preparat ion: Condition a Sep-Pak SPE cartridge with 10 mL MeOH and 10 mLwater. 500 |xL Seru m + 1 mL w ate r + 15 |xL 100 ng/mL fenoterol in water, m ix, forceslowly 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 m in with 70 |xL buffer + 300 |xL 0.05% di(2-ethylhexyl) pho sp ha te in e thy lacetate, 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, trans fer ethy l ace tate layerto another tube and add 70 JJLL 10 mM HCl to it, vortex 1 min, centrifuge at 5000 g for30 s, remove acid layer and wash it with 150 fxL chloroform, centrifuge at 5000 g for 30s, inject a 40-60 |xL aliquot of the aqueous phase. (Buffer was 70 mM NaH 2PO 4 + 1 mMchloride + 2 mM 1-heptanesulfonic acid, pH 6.8.)HPLCVARIABLESColumn: 75 X 4.6 3 jxm Ultrasphere ODSMobile phase: M eOH : buffer 25 :75 (Buffer wa s 70 mM NaH 2PO 4 + 1 mM chloride + 2mM 1-heptanesulfonic acid, pH 6.8.)Flow rate: 0.5Inject ion volume: 40-60Detector: E, BioAnalytical System Model LC-4, TL-5 glassy carbon working electrode,Ag/AgCl reference electrode, +0.80 V, 10 nA full scaleCHROMATOGRAMRetention time: 7Internal s tandard: fenoterol (13)Limit of detect ion: 0.4 ng/mLOTHER SUBSTANCESNoninterfer ing : buphen ine, carbamazepine, do butamine, epineph rine, ethosuximide, gen-tamycin, isoproterenol, isoxsuprine, metaproterenol, metaraminol, oxymetazoline, phen-obarbital, phen tolamine, pheny lephrine, phenytoin, primidone, terbutaline, theophylline,valproic acidKEYWORDSserum; heparin interferes with IS; SPE; pharmacokinetics

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    REFERENCETan, YK.; Soldin, S.J. Determination of salbutamol in human serum by reversed-phase high-perfor-mance liquid chromatography with amperometric detection. J.Chromatogr., 1984, 311, 311-317SAMPLEMatrix: blood, urineSample preparat ion: Condition a 1 mL 100 mg (or 2.8 mL 500 mg) Extract-Clean silicaSPE cartridge (Alltech) with 1 volume MeCN and 1 volume water. Add 1 mL ur ine or 3mL plasm a to the SPE c artridge, dry, wa sh with 1 volume water, wash w ith 1 volumeMeCN, dry, elute with 2 volumes MeOH. Evaporate the eluate under reduced pressureat 45, reconstitute with 1 (urine) or 0.3 (plasma) mL mobile phase, vortex for 1 min,inject an aliquot.HPLCVARIABLESGuard co lumn: 30 X 4 Chirex 3022 naphthyl urea (Phenomenex)Column: 250 X 4 Chirex naphthyl u rea (Phenomenex)Mobile phase: Hexane:l,2-dichloromethane (sic):MeOH:trifluoroacetic acid 60.75:35:4.25:0.25Flow rate: 1Inject ion vo lume: 200Detector: F ex 220 em 309CHROMATOGRAMRetent ion t ime: 22 (S-(+)), 27 (R-(-))Limit o f detect ion: 0.25 ng/mLKEYWORDSchiral; plasma; SPE; pharmacokineticsREFERENCEBoulton, D.W.; Fawcett, J.P. Determination of salbutamol enantiomers in human plasma and urine bychiral high-performance liquid chromatography. J.Chromatogr.B, 1995, 672, 103-109

    SAMPLEMatrix: blood, urineSample preparat ion: Condition a 100 mg Baxter C18 SPE cartridge with one volumeMeOH and two volumes water. Dilute 10 |xL urine to 500 |xL with water. 500 |xL Serumor diluted uri ne + 50 |xL water, vortex for 30 s, add to SPE cartridg e, wash w ith t hre e200 |xL aliquots of water, elute w ith two 500 |xL aliquots of M eOH. E vap orate the elua testo 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 aliquHPLC VARIABLESGuard co lumn: 5 |xm Adsorbosphere C-18Column: 250 X 4.6 5 |xm Adsorbosphere C-18Mobile phas e: M eCN : buffer 7:9 3 adjus ted to pH 3.0 with 85% phosphoric acid (Buffer wa s25 mM (NH4)H 2PO 4 and 1 mM N,N-dimethyloctylamine.)Flow rate: 1.5Inject ion volume: 50Detector: UV 224; F ex 228 em 310CHROMATOGRAMRetent ion t ime: 7 .1Internal s tandard: albuterol

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    OTHER SUBSTANCESExtracted: atenololKEYWORDSserum; SPE; albuterol is ISREFERENCEChatterjee, D.J.; Li, W.Y; Hurst, A.K.; Koda, R.T. High-performance liquid chromatographic method fordetermination of atenolol from human plasma and urine: Simultaneous fluorescence and ultravioletdetection. J.Liq.Chromatogr., 1995, 18, 791-806SAMPLEMatrix: bulkSample preparation: Inject a 5 |xL aliquot of a solution.HPLCVARIABLESColumn: 250 X 4.6 5 u,m LiChrosphere DiolMobile phase: Gradient. Carbon dioxide:MeOH containing 0.5% n-propylamine 70:30 for9.5 min, to 55:45 over 12 min.Column temperature: 70Flow rate: 1.5Injection volume: 5Detector: UVCHROMATOGRAMRetention time: 6.2Limit of detection: 1.3 |xg/mLOTHER SUBSTANCESSimultaneous: impuritiesKEYWORDS300 bar; SFCREFERENCEBernal, J.L.; del Nozal, M.J.; Rivera, J.M.; Serna, M.L.; Toribo, L. Separation of salbutamol and sixrelated imp urities by packed column supercritical fluid chromatography. Chromatographia, 1996,42 ,8 9 - 9 4SAMPLEMatrix: formulationsSample preparation: Dilute with water to a concentration of 833 |Jig/mL, add a 300 |xL ali-quot to 250 JJLL 2 mg/mL mepivacaine hydrochloride in water, vortex, inject a 10 u-L aliquot.HPLCVARIABLESColumn: 100 X 8 4 |xm NovaPak C18 radial compressionMobile phase: Gradient. A was 2.5 mM PIC B-8 Low UV (Waters) in TH F: water 40:60. Bwas water. C was MeOH: water 50:50. A:B:C 50:50:0 for 7.7 min, to 60:15:25 over 5.3min, re-equilibrate at initial conditions for 5 min.Flow rate: 2Injection volume: 10Detector: UV 220CHROMATOGRAMRetention time: 3.2Internal standard: mepivacaine (8.2)

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    OTHER SUBSTANCESSimultaneous: fenoterol, ipratropium bromide, terbutalineKEYWORDSnebulizer solutions; stability-indicatingREFERENCEJacobson, G.A.; Peterson, G.M. High-performance liquid chromatographic assay for the simultaneousdetermination of ipratropium bromide, fenoterol, salbutamol and terbutaline in nebulizer solution.J.Pharm.Biomed.Anal, 1994, 12, 825-832SAMPLEMatrix: formulationsSample preparation: Tablets, capsules. Mix tablets or capsules with 10 mL water, sonicate30 min, centrifuge, inject an aliquot of the supernatant. Liquid formulations. Dilute liquid

    formulations with water, inject an aliquot.HPLCVARIABLESColumn: 125 X 4 5 jxm LiChrospher 100 RP-18 endcappedMobile phase: MeOH-.water 40:60 containing 2 mM KOH + 10 mM hexanoic acidFlow rate: 0.4Injection volume: 20Detector: UV 214CHROMATOGRAMRetention time: 3.5Limit of detection: 1760 ng/mLOTHER SUBSTANCESAlso analyzed: terbutaline, fenoterolKEYWORDStablets; capsules; liquid formulationsREFERENCEAckermans, M.T.; Beckers, J.L.; Everaerts , RM.; Seelen, LG. Comparison of isotachophoresis, capillaryzone electrophoresis and high-performance liquid chromatography for the determination of salbu-tamol, terbutaline sulphate and fenoterol hydrobromide in pharmaceutical dosage forms.J.Chromatogr., 1992, 590, 3 4 1 - 3 5 3SAMPLEMatrix: bloodSample 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 bamethansulfate 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 vacuumto remove all liquid. Wash twice with 1 mL water and with 1 mL MeCN (draining com-pletely 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.HPLCVARIABLESGuard column: 15 X 3.2 Brownlee 7 |xm C8Column: 150 X 4.6 5 |xm Ultrasphere Octylsilica

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    Mobile phase: MeCN: MeOH: water: phosphoric acid: KH2PO 4: octanesulfonic acid 50 :150:900:0.25:0.75:0.05 (v/v/v/v/w/w)Flow rate: 1.6Injection volume: 40Detector: F ex 275 em 310CHROMATOGRAMRetention time: 7Internal standard: bamethan sulfate (17.5)Limit of quantitation: 0.2 ng/mLKEYWORDSSPE; plasmaREFERENCEGupta, 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, 2 0 5 - 2 1 1SAMPLEMatrix: bloodSample preparation: Condition a Bond Elut Si SPE cartridge by washing twice with 1mL MeOH, twice with 1 mL water, and once with 1 mL 100 mM pH 9.2 K2HPO4. Add 1mL plasma + 100 |JLL 500 ng/mL atenolol in water, wash twice with 1 mL water, centrifugeat 1000 g for 5 min, elute with 1 mL MeOH. Evaporate MeOH to dryness at 40 under astream of air and dissolve residue in 200 |xL mobile phase, inject an aliquot.HPLCVARIABLESColumn: 250 X 4.6 Spherisorb S5 SCXMobile phase: MeOH:MeCN: water 40:40:20 containing 0.2% perchloric acid (apparentpH 1.7)Flow rate: 1.5Injection volume: 100Detector: F ex 200 no emission filterCHROMATOGRAMRetention time: 8Internal standard: atenolol (13)Limit of detection: 1000 ng/mLOTHER SUBSTANCESExtracted: terbutalineNoninterfering: aminophylline, beclomethasone, cloprednol, dexamethasone, fenoterol,ipratropium bromide, methylprednisolone, orciprenaline, prednisolone, reproterol, rimi-terol, salmeterol, sodium cromoglycate, theophyllineKEYWORDSSPE; plasmaREFERENCEMcC arthy, P.T.; Atwal, S.; Sykes, A.P.; Ayres, J.G. M easu rem ent of terb uta line and salbutam ol in p lasm aby high performance liquid chromatography with fluorescence detection. Biomed.Chromatogr., 1993,7 , 25-28SAMPLEMatrix: blood

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    Sample preparat ion: Condition a 1 mL Bond-Elut octadecylsilane SPE cartridge with 2mL M eOH, 2 m L w ater, an d 2 mL buffer (do not allow to dry ). 1 mL Seru m H- 10 jxL 100(xg/mL bamethan in water + 2 mL buffer, mix, add to SPE cartridge, wash with 1 mLbuffer, 2 mL water, 2 mL MeOHrMeCN 15:85. Dry under full vacuum for 10 min andelute with 1 mL MeOH. Evaporate the elu ate to dryness under a stream of nitrogen a troom temperature. Dissolve the residue in 200 JJLL MeCN: tr ie thylamine 199:1, heat a t45for 20 min, add 10 jxL 5 mg/mL TAGIT in MeCN, heat at 45for 2 h. Evaporate atroom tem pe ratu re u nd er a stre am of nitrogen, rec ons titute in 250 fxL mobile pha se, injecta 100 |xL aliquot. (Buffer was 100 mM Na2HPO 4 adjusted to pH 7.3 with concentratedphosphoric acid. The chiral derivatizing agent TAGIT was 2,3,4,6-tetra-O-acetyl-|3-D-glu-copyranosyl isothiocyanate. Prepare solutions of TAGIT in MeCN weekly.)

    HPLCVARIABLESColumn: 100 X 4.6 5 |xm Brownlee octadecylsilylMobi le phase: MeC N: wa ter 29: 71 containing 0.1% triethylam ine (pH adjusted to 4.0 w ithconcentrated phosphoric acid)Flow rate: 0 .8Inject ion vo lume : 100Detector: F ex 223 no emission filterCHROMATOGRAMRetent ion t ime: 5.77 (R(-)) , 6.83 (S(+))Internal s tandard: bamethan (9, 10)Limit of detect ion: 1 ng/mLKEYWORDSSPE; chiral; derivatization; serumREFERENCEHe, L.; Stewart, J.T. A high performance liquid chromatographic method for the determination of al-buterol enantiomers in human serum using solid phase extraction and chemical derivatization. Bio-med.Chromatogr., 1992, 6, 2 9 1 - 2 9 4SAMPLEMatrix: solutionsSample preparat ion: Dilute 800 |xL solution to 10 mL with water, filter, inject a 20 |xLaliquo t of th e filtrate.HPLC VARIABLESGuard column: RP-18Column: 125 X 4 5 |xm LiChrosorb RP-18Mobile phase: Gradient. MeCN-.buffer 4:96 for 6 min, to 9:91 (step gradient). (Buffer was40 mM NaH 2PO 4 containing 5.74 mM triethylamine, adjusted to pH 3.0 with phosphoricacid.)Flow rate: 1.5Inject ion volume: 20Detector: UV 265KEYWORDScomparison with capillary electrophoresisREFERENCEMalkki-Laine, L.; Hartikainen, E. Electrokinetic behaviour of salbutamol and its decomposition prod-ucts and determination of salbutamol by micellar electrokinetic capillary chromatography.J.Chromatogr.A, 1996, 724, 297-306

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    SAMPLEMatrix: solutionsHPLCVARIABLESColumn: 250 X 4.6 CSP-4 (Prepare as follows. Add a solution of 1.07 g L-valyl-L-valyl-L-

    valine 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 (cy-anuric chloride) in 20 mL dry dioxane stirred at 0, add 3 g anhydrous sodium carbonateat room temperature, stir, filter, evaporate to give a colorless solid. Dissolve 8.3 g of thissolid in 30 mL dry dioxane, add 2 g N-(2-aminoethyl)-3-aminopropyltrimethoxysilane, add1.5 g anhydrous sodium carbonate, reflux with stirring for 40 h, filter, add 3 g dried 10juim LiChrosorb Si 100, reflux with slow stirring for 10 h, cool, filter. Wash the solid withdioxane, MeOH, and diethyl ether, dry under reduced pressure (J.Chromatogr. 1984, 292,427).)Mobile phase: H exa ne : 1,2-dichloroethane:MeO H:trifluoroacetic acid 60 :37. 5:3.7 5:0 .25Detector: UVCHROMATOGRAMRetent ion t ime: k' 5.84 (first enantiomer)KEYWORDSchiral; a = 1.06REFERENCEOi, N.; Ki taha ra, H .; M atsu shit a, Y.; Kisu, N. En antio m er separa tion by gas and high-performance liquidchromatography with tripeptide derivatives as chiral stationary phases. J.Chromatogr.A, 1996, 722,229-232SAMPLEMatrix: solutionsSample preparat ion: Inject an aliquot of a 200 |xM solution in MeOH.HPLCVARIABLESColumn: 100 X 4.7 7 |xm Hypercarb (Shandon)Mobile phase: MeOH containing 5 mM N-benzyloxycarbonylglycyl-L-proline and 4.5 mM

    NaOHColumn temperature: 17Inject ion vo lum e: 20Detector: UV 270CHROMATOGRAMRetent ion t ime: k' 3.2 (first enantiomer)KEYWORDSchiral; a = 1.09REFERENCEHuynh, N.-H.; Karlsson, A.; Pettersson, C. Enantiomeric separation of basic drugs using N-benzyloxy-carbonylglyclyl-L-proline as counter ion in methanol. J.Chromatogr.A, 1995, 705, 2 7 5 - 2 8 7SAMPLEMatrix: solutionsHPLC VARIABLESColumn: 250 x 4.6 5 |xm Supelcosil LC-DP (A) or 250 X 4 5 |xm LiCh rosp her 100 RP-8 (B)

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    Mobile phase: MeCN:0.025% phosphoric acid:buffer 25:10:5 (A) or 60:25:15 (B) (Bufferwa s 9 mL concentrated phosp horic acid and 10 mL triethy lam ine in 900 mL water, adjustpH to 3.4 with dilute phosphoric acid, make up to 1 L.)Flow rate: 0 .6Inject ion volume: 25Detector: UV 229CHROMATOGRAMRetent ion t ime: 5.57 (A), 3.27 (B)OTHER SUBSTANCESAlso analyzed: acebutolol, acepromazine, acetaminophen, acetazolamide, acetophenazine,alprazolam, amitriptyline, amobarbital, amoxapine, antipyrine, atenolol, atropine, aza-tadine, baclofen, benzocaine, bromocriptine, brompheniramine, brotizolam, bupivacaine,buspirone, butabarbital, butalbital, caffeine, carbamazepine, cetirizine, chlorcyclizine,chlordiazepoxide, chlormezanone, chloroquine, chlorpheniramine, chlorpromazine, chlor-

    propamide, chlorprothixene, chlorthalidone, chlorzoxazone, cimetidine, cisapride, clomi-pramine, clonazepam, clonidine, clozapine, cocaine, codeine, colchicine, cyclizine, cyclo-benzaprine, 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, fu-rosemide, glutethimide, glyburide, guaifenesin, haloperidol, homatropine, hydralazine,hydrochlorothiazide, hydrocodone, hydromorphone, hydroxychloroquine, hydroxyzine,ibuprofen, imipramine, indomethacin, ketoconazole, ketoprofen, ketorolac, labetalol, Ie-vorphanol, lidocaine, loratadine, lorazepam, lovastatin, loxapine, mazindol, mefenamicacid, meperidine, mephenytoin, mepivacaine, mesoridazine, metaproterenol, methadone,methdilazine, methocarbamol, methotrexate, methotrimeprazine, methoxamine, methyl-dopa, methylphenidate, metoclopramide, metolazone, metoprolol, metronidazole, mida-zolam, moclobemide, morphine, nadolol, nalbuphine, naloxone, naphazoline, naproxen,nifedipine, nizatidine, norepinephrine, nortriptyline, oxazepam, oxycodone, oxymetazo-line, paroxetine, pemoline, pentazocine, pentobarbital, pentoxifylline, perphenazine,pheniramine, phenobarbital, phenol, phenolphthalein, phentolamine, phenylbutazone,phenyltoloxamine, phenytoin, pimozide, pindolol, piroxicam, pramoxine, prazepam, pra-zosin, probenecid, pro cainam ide, p rocaine, proch lorperazine, procyclidine, promazine, pro-methazine, propafenone, propantheline, propiomazine, propofol, propranolol, protripty-line, quazepam, quinidine, quinine, racem ethorphan , ra nitidine, remoxipride, risperidone,salicylic acid, scopolamine, secobarbital, sertraline, sotalol, spironolactone, sulfinpyra-zone, sulindac, temazepam, terbutaline, terfenadine, tetracaine, theophylline, thiethyl-perazine, thiopental, thioridazine, thiothixene, timolol, tocainide, tolbutamide, tolmetin,trazodone, triamterene, triazolam, trifluoperazine, triflupromazine, trimeprazine, tri-methoprim, trimipramine, verapamil, warfarin, xylometazoline, yohimbine, zopiclone

    KEYWORDSdetails of plasma extraction also in paperREFERENCEKoves, E.M. Use of high-performance liquid chromatography-diode array detection in forensic toxicology.J.Chromatogr.A, 1995, 692, 103-119SAMPLEMatrix: solutionsHPLCVARIABLESColumn: 250 X 4.6 Sumchiral CSP 10 (Sumika Chemical Analysis Service)Mobile phase: n-H exan e: 1,2-dichloroethane: M eOH : trifluoroacetic acid 25 0: 14 0: 20 :1

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    Flow rate: 1Detector: UV 230-280CHROMATOGRAMRetent ion t ime: k' 5.41 (first enantiomer)KEYWORDSchiral; a = 1.33REFERENCEOi, N.; Kita hara , H.; Aoki, F. Direct enantiom er se para tion s by high-performance liquid chrom atograp hywith chiral urea derivatives as stationary phases. J.Chromatogr.A, 1995, 694, 129-134SAMPLEMatrix: solutionsHPLCVARIABLESColumn: 250 X 4.6 Zorbax RXMobile phase: Grad ient. A was 10 mL co ncentrated orthophosphoric acid and 7 mL trie-thylamine in 1 L water. B was 10 mL concentrated orthophosphoric acid and 7 mL trie-thylam ine in 200 mL water, ma ke up to 1 L with M eCN. A :B from 100:0 to 0:100 over30 min, maintain at 0:100 for 5 min.Colum n tem peratu re: 30Flow rate: 2Detector: UV 210OTHER SUBSTANCESAlso analyzed: 5-fluorouracil, acepromazine, acetaminophen, acetophenazine, aminophyl-line, amitriptyline, amobarbital, amoxapine, am phetam ine, am ylocaine, antipyrine, apro-barbital, aspirin, atenolol, atropine, avermectin, barbital, bebrisoquine, benzocaine,benzoic acid, benzotropine, benzphetamine, berberine, bibucaine, bromazepan,brom pheniramine, bu prenorphine, buspirone, butab arbital, butacaine, buteth al, caffeine,carbamazepine, carbromal, chloramphenicol, chlordiazepoxide, chloroquine, chlorothia-zide, chloroxylenol, chlorphenesin, chlorpheniramine, chlorpromazine, chlorpropamide,chlortetracycline, cimetidine, cinchonidine, cinchonine, clenbuterol, clonazepam, clonixin,clorazepate, cocaine, codeine, colchicine, cortisone, coumarin, cyclazocine, cyclobenza-prine, cyclothiazide, cyheptamide, cymarin, danazol, danthron, dapsone, desipramine,dexamethasone, dextromethorphan, dextropropoxyphene, diamorphine, diazepam, diclo-fenac, diethylpropion, diethylstilbestrol, diflunisal, digitoxin, digoxin, diltiazem, diphen-hydramine, diphenoxylate, diprenorphine, dipyrone, disulfiram, dopamine, doxapram,doxepin, dronabinol, ephedrine, epinephrine, epinine, estradiol, estriol, estrone, ethac-rynic acid, ethosuximide, etonitazene, etorphine, eugenol, famotidine, fenbendazole, fen-camfamine, fenoprofen, fenproporex, fentanyl, flubendazole, flufenamic acid, flunitraze-pam, fluoxymesterone, fluphenazine, furosemide, gentisic acid, gitoxigenin, glipizide,glunixin, glutethim ide, glybenclamide, guaiacol, halaze pam , haloperidol, hydrochlorothia-zide, hydrocodone, hydrocortisone, hydromorphone, hydroxyquinoline, ibogaine, ibupro-

    fen, im inostilbene, imip ram ine, ind om ethacin, isocarbostyril, isocarboxazid, isoniazid, is-oproterenol, isoxsuprine, ivermectin, ketamine, ketoprofen, kynurenic acid, levorphanol,lidocaine, lorazepam, lorm etazepam , loxapine, mazindol, m ebendazole, meclizine, meclo-fenamic acid, medazepam, mefenamic acid, megestrol, mepacrine, meperidine, mephen-termin e, m ephenytoin, m ephesin, m ephobarbital, mepivacaine, mescaline, mesoridazine,methadone, methamphetamine, methapyrilene, methaqualone, methazolamide, metho-carbamol, methoxam ine, methsuxim ide, methyl salicylate, methyldopa, m ethyldopamine,methy lphenidate, methylprednisolone, m ethyltestosterone, m ethyprylon, m etoprolol, mi-bolerone, morphine, nadolol, nalorphine, naloxone, naltrexone, naphazoline, naproxen,nefopam, niacinamide, nicotine, nicotinic acid, nifedipine, niflumic acid, nitrazepam,norepinephrine, nortriptyline, noscapine, nylidrin, oxazepam, oxycodone, oxymorphone,

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    oxyphenbutazone, oxytetracycline, papaverine, pargyline, pemoline, pentazocine, pento-barbital, persantine, phenacetin, phenazocine, phenazopyridine, phencyclidine, phendi-metrazine, phenelzine, pheniramine, phenobarbital, phenothiazine, phensuximide, phen-termine, phenylbutazone, phenylephrine, phenylpropanolamine, piperocaine, prazepam,prednisolone, primidone, probenecid, progesterone, propiomazine, propranolol, propyl-paraben, pseudoephedrine, puromycin, pyrilamine, pyrithyldione, quazepam, quinaldicacid, quinidine, quinine, ranitidine, recinnamine, reserpine, resorcinol, saccharin, albu-terol, salicylamide, salicylic acid, scopolamine, scopoletin, secobarbital, strychnine, sul-facetamide, sufadiazine, sulfadimethoxine, sulfaethidole, sulfamerazine, sulfamethazine,sulfamethoxizole, sulfanilam ide, sulfapy ridine, sulfasoxizole, sulinda c, tamox ifen, tema -zepam, testosterone, tetracaine, tetracycline, dronabinol, tetramisole, thebaine, theobro-mine, theophylline, thiabendazole, thiamine, thiamylal, thiobarbituric acid, thioridazine,thiosalicylic acid, thiothixen e, thymol, tolazamide, tolazoline, tobu tam ide, tolm etin, tr an -ylcypromine, triamcinolone, tribenzylamine, trichloromethiazide, trifluoperazine, tri-hexyphenidyl, trimethoprim, tripelennamine, triproilidine, tropacocaine, tyramine, vera-pamil, vincamine, warfarin, yohimbine, zoxazolamine

    REFERENCEHill, D.W.; Kind, A. J. Reversed-phase solvent gradie nt HPLC reten tion indexes of drug s. J.Anal.ToxicoL,1994, 18, 233-242SAMPLEMatrix: solutionsSample preparat ion: Prepare a 10 jjig/mL solution in MeOH, inject a 20 JULL aliquot.HPLCVARIABLESColumn: 125 X 4.9 Spherisorb S5W silicaMobile phase: MeOH containing 10 mM ammonium perchlorate and 1 mL/L 100 mMNaOH in MeOH, pH 6.7Flow rate: 2Injection volume: 20Detector: E, LeCarbone, V25 glassy carbon electrode, + 1.2 VCHROMATOGRAMRetent ion t ime: 1.76OTHER SUBSTANCESAlso analyzed: acebutolol, acepromazine, acetophenazine, N-acetylprocainamide, alpreno-lol, amethocaine, amiodarone, amitriptyline, antazoline, atenolol, azacyclonal, bame-thane, benactyzine, benperidol, benzethidine, benzocaine, benzoctamine, benzphetamine,benzquinamide, bromhexine, bromodiphenhydramine, bromperidol, brompheniramine,brompromazine, buclizine, bufotenine, bupivacaine, buprenorphine, butacaine, butetha-mate, chlorcyclizine, chlorpheniramine, chlorphenoxamine, chlorprenaline, chlorproma-zine, chlorprothixene, cimetidine, cinchonidine, cinnarizine, clemastine, clomipramine,clonidine, cocaine, cyclazocine, cyclizine, cyclopentam ine, cyp rohe ptadin e, de serp idine , de-sipramine, dextromoramide, dextropropoxyphene, dicyclomine, diethylcarbamazine, die-

    thylpropion, diethy lthiambuten e, dihydroergotamine, dimethindene, dimethothiazine, di-phenhydramine, diphenoxylate, dipipanone, diprenorphine, dipyridamole, disopyramide,dothiepin, doxapram, doxepin, doxylamine, droperidol, ephedrine, ergocornine, ergocris-tine, ergocristinine, ergocryptine, ergom etrine, ergosine, ergosinine, ergotamine, ethopro-pazine, etorphine, etoxeridine, fenethazine, fenfluramine, fenoterol, fentanyl, flavoxate,fluopromazine, flupenthixol, fluphenazine, flurazepam , haloperido l, hydro xyzine, hyo-scine, ibogaine, imipramine, indapamine, iprindole, isothipendyl, isoxsuprine, ketanserin,laudanosine, lidocaine, lofepramine, loxapine, maprotiline, mecamylamine, meclophen-oxate, meclozine, medazepam, mephentermine, mepivacaine, meptazinol, mepyramine,mesoridazine, metaraminol, methadone, methamphetamine, methapyrilene, methdila-zene, methotrimeprazine, methoxamine, methoxyphenamine, methoxypromazine, meth-

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    ylephedrine, methylergonovine, methysergide, metoclopramide, metopimazine, metopro-lol, 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, phendimetra-zine, phenelzine, phenglutarimide, phenindamine, pheniramine, phenmetrazine, pheno-morphan, phenoperidine, phenothiazine, phenoxybenzamine, phentolamine, phenyle-phrine, phenyltoloxamine, physostigmine, piminodine, pimozide, pindolol, pipamazine,pipazethate, piperacetazine, piperidolate, pipradol, pirenzepine, piritramide, pizotifen,practolol, pramoxine, prazosin, prenylamine, prilocaine, primaquine, proadifen, procain-amide, procaine, prochlorperazine, procyclidine, proheptazine, prolintane, promazine, pro-methazine, pronethalol, properidine, propiomazine, propranolol, prothipendyl, protripty-line, proxymetacaine, pseudoephedrine, pyrimethamine, quinidine, quinine, ranitidine,rescinnamine, sotalol, tacrine, terazosin, terbutaline, terfenadine, thenyldiamine, theoph-ylline, thiethylperazine, thiopropazate, thioproperazine, thioridazine, thiothixene, thon-zylamine, timolol, tocainide, tolpropamine, tolycaine, tranylcypromine, trazodone, trifluo-perazine, trifluperidol, trimeperidine, trimeprazine, trimethobenzamide, trimethbprim,trimipramine, tripelennamine, triprolidine, tryptamine, verapamil, xylometazoline

    REFERENCEJane , L;McKinnon, A.;Flanagan, R.J. High-performance liquid chromatographic analysis ofbasic drugson silica columns using non-aqueous ionic eluents. II. Application of UV, fluorescence and electro-chemical oxidation detection. J.Chromatogr., 1985,323, 191-225 ANNOTATED BIBLIOGRAPHYTsai, CE.; Kondo, F. Liquid chromatographic determination of salbutamol and clenbuterol residues inswine serum and muscle. Microbios, 1994,80, 251-258Malkki, L.;Tammilehto, S. Optimization of the separation of salbutamol and its decomposition productsby liquid chromatography with diode-array detection. J.Pharm.Biomed.AnaL, 1993,11, 7 9 - 8 4Nasr, M.M. Single-puff particle-size analysis of albuterol metered-dose inhalers (MDIs) by high-pressureliquid chromatography with electrochemical detection (HPLC-EC). Pharm.Res., 1993 ,10 ,1381-1384Sagar, K.A.; Kelly, M.T.; Smyth, M.R. Simultaneous determination of salbutamol and terbutaline atoverdose levels in human plasma by high performance liquid chromatography with electrochemicaldetection. Biomed.Chromatogr., 1993,7, 2 9 - 3 3Degroodt, J.M.;Wyhowski de Bukanski, B.; Srebrnik, S. Immunoaffinity-chromatography purificationof salbutamol in liver and HPLC-fluorometric detection at trace residue level. Z.Lebensm.Unters.Forsch., 1992,195, 566-568Tamisier-Karolak, L.; Delhotal-Landes, B.; Jolliet-Riant, P.;Milliez, J.; Janne t , D.;Barre, J.; Flouvat,B. Plasma assay of salbutamol by means of high-performance liquid chromatography with ampero-metric determination using a loop column for injection of plasma extracts. Application to the eval-uation of subcutaneous administration of salbutamol. Ther.Drug M onit., 1992,14,243248Meyer, H.H.;Rinke, L.; Dursch, I. Residue screening for the beta-agonists clenbuterol, salbutam ol andcimaterol in urine using enzyme immunoassay and high-performance liquid chromatography.J.Chromatogr., 1991,564, 551-556 [extracted cimaterol, clenbuterol; urine; cow; SPE; enzyme im-mun oassay detection; UVdetection]Wu, Y.Q.; Shi, R.; Williams, R.L.; Lin, E.T. High-performance liquid chromatographic assay for basicamine drugs in human plasma with a silica gel column and an aqueous m obile phase. IV.Albuterol.J.Liq.Chromatogr., 1991,14, 253-264 [plasma; fluorescence detection; LOD 0.2 ng/mL; metaproter-enol (IS)]Beaulieu, N.; Cyr, T.D.;Lovering, E.G. Liquid chromatographic methods for the determination of albu-terol (salbutamol), albuterol sulphate and related compounds in drug raw materials , tablets andinhalers. J.Pharm.Biomed.AnaL, 1990,8, 583-589Bland, R.E.;Tanner, R.J.; Chern, WH.;Lang, J.R.; Powell, J.R. Determination of albuterol concentra-tions in human plasma using solid-phase extraction and high-performance liquid chromatography

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