Fa Moti Dine

7/28/2019 Fa Moti Dine

1/6

SAMPLEMatrix: bloodSample preparat ion: Condition an SPE cartridge with 1 mL MeOH an d 1 mL water. Add1 mL plasma to the SPE cartridge, wash with 5 mL water, elute with 2 mL MeCN.Evaporate the eluate, reconstitute in acetic acid/phosphate buffer, centrifuge, inject analiquot.HPLC VARIABLESGuard co lumn: Newguard RP-8 (Applied Biosystems)Column: Spherisorb C8Mobile phase: MeC N: 30 mM p H 2.6 N aH 2PO 4 7:93 containing 7.2 mM triethylamineFlow rate: 1D etec tor: UV 267CHROMATOGRAMRetent ion t ime: 9 .6Limit of quant i tat ion: 2 ng/mLKEYWORDSplasma; SPE; pharmacokineticsREFERENCESch wa rtz, J.I. ; Yeh, K.C.; Berger, M.L.; Tomasko, L.; Hoover, M .E.; Ebel, D.L.; Stauffer, L.A.; H an , R.;Bjornsson, T.D. Novel oral medication delivery system for famotidine. J. CUn.Pharmacol., 1995, 35,362-367SAMPLEMatrix: bloodSample preparat ion: 1.5 mL Plasma + 100 |xL 4 M HCl, shake, add 8 mL diethyl ether,shake for 15 min, centrifuge at 1000 g at 4 for 5 min, discard ether layer. Add 0.5 mLsaturated Na2CO 3 solution, 0.5 mL saturated NaHCO 3 solution, 100 JJLL 5 |xg/mL clopam-ide in water, and 7 mL ethyl acetate to aqueous layer, shake 15 min, centrifuge at 2000g at 4 for 5 min, rep eat extraction, combine organic layers a nd ev apora te them to dryn essun der a stre am of nitrogen at 37. Re constitute w ith 150 jxL M eCN : w ater 12:8 8, vortex,inject 90 |xL aliquot.HPLCVARIABLESColumn: 100 X 2 5 |xm ODS Hypersil C18Mobile pha se: MeC N: wa ter 12:88 containing 20 mM N a2HPO 4 and 50 mM sodium dodecylsulfate adjusted to pH 3 with orthophosphoric acidFlow rate: 0.5Inject ion volume: 90Detector: UV 267CHROMATOGRAMRetention time: 13Internal s tandard: clopamide (9)Limit of detection: 5 ng/mL

FamotidineMolecular formu la: C8H15N7O2S3Molecular weight: 337.4CAS Registry No.: 76824-35-6


2/6

OTHER SUBSTANCESNoninterfer ing: acetaminophen, amiloride, aspirin, atenolol, chlorothiazide, cimetidine,cyclopenthiazide, diazepam, furosemide, indapamide, labetalol, lorazepam, metoprolol,phenytoin, propranolol, ran itidin e, salicylic acid, theophylline

KEYWORDSplasma; microboreREFERENCEWanwimolruk, S.; Zoest, A.R.; Wanwimolruk, S.Z.; Hung, CT. Sensitive high-performance liquid chromatographic determination of famotidine in plasma. Application to pharmacokinetic study.J.Chromatogr., 1991, 572, 227-238SAMPLEMatrix: bloodSample preparat ion: 1 mL Plasma + 1 mL satu rated potassium carbonate + 5 mL ethylacetate, mix, centrifuge. Remove the organic layer and add it to 1 mL sa tu rat ed NaC lsolution and 1 mL 1 M HCl, centrifuge. Remove the aqueous phase and add it to 1 mLsaturated potassium carbonate solution and 3 mL ethyl acetate, extract. Remove a 2.5mL aliquot of the organic layer and evaporate it to dryness under reduced pressure,reconstitute the residue with 400 jxL 250 JJIM phenanthrenequinone in MeOH, evaporateto dryness u nd er reduced pre ssu re, rec ons titute with 40 (xL DM F and 40 uX. 2 M N aOH ,he at at 60 for 15 m in, cool on ice, neu tra lize w ith 5 M acetic acid, inject a 20 |xL aliquot.

HPLC VAR IABLESColumn: reversed phaseMobile phase: M eCN : 10 mM pH 4 citrate buffer 40 :50Flow rate: 1Inject ion volum e: 20Detector: F ex 296 em 411CHROMATOGRAMLimit of detect ion: 5 ng/mLKEYWORDSplasma; pharmacokinetics; derivatizationREFERENCEEchizen, H.; Shoda, R.; Umeda, N.; Ishizaki, T. Plasma famotidine concentration versus intragastric pHin patients w ith upper gastrointestina l bleeding and in healthy subjects. CUn.Pharmacol.Then, 1988,44, 690-698SAMPLEMatrix: blood, urineSample preparat ion: 50 JJLL Plasma or urine + 350 |xL 0.2 jxg/mL 3-butylxanthine inMeOH, centrifuge at 6000 g for 5 min. Evaporate supernatant under a stream of nitrogenat 40, reconstitute in 250 JULL mobile phase, inject an aliquot.HPLCVARIABLESColumn: 250 X 4.2 Cosmosil 5C18Mobile phase: M eCN : 30 mM pH 7.0 pho sph ate buffer 10:90F low rate: 1.5D etecto r: UV 267


3/6

CHROMATOGRAMInterna l s tandard: 3-butylxanthineLimit of quantitation: 100 ng/mLKEYWORDSplasmaREFERENCEHasegaw a, T.; Nada i, M.; Wang, L.; Takaya ma , Y.-L; Kato, K.; Nabesh ima, T.; Kato, N. Renal excretionof famotidine and role of adenosine in renal failure induced by bacterial lipopolysaccharide in rats.DrugMetab.Dispos., 1994, 22, 8 - 1 3SAMPLEMatrix: formulationsSample preparat ion: Inject a 20 JJLL aliquot.HPLCVARIABLESColumn: Nova Pak C18Mobile phase: MeCN:0.1% acetic acid: 10 mM pH 7.8 (NH4)H 2PO4 10:23:74Flow rate: 1Inject ion volum e: 20Detector: UV 300CHROMATOGRAMRetention t ime: 13.9OTHER SUBSTANCESSimul taneous: cefmetazoleNoninterfer ing: degradation productsKEYWORDSstability-indicating; injections; 5% dextroseREFERENCELee, D.K.T.; Wong, C-Y; Wang, D.-R; Chang, L.-C; Wu, K.-H. Stability of cefmetazole sodium andfamotidine. Am.J.Health-Syst.Pharm., 1996, 53, 432-442SAMPLEMatrix: formulationsSample preparat ion: Dilute with 5% dextrose (if necessary), inject a 20 jxL aliquot.HPLCVARIABLESColumn: Nova Pak C18Mobile phase: M eOH: 100 mM (NH4)2HPO 4 20:80, pH 7.80Flow rate: 1Inject ion volum e: 20Detector: UV 322CHROMATOGRAMRetent ion t ime: 4 .6OTHER SUBSTANCESSimul taneous: cefazolin


4/6

KEYWORDSinjections; 5% dextrose; stability-indicatingREFERENCEWang, D.-P.; Chang, L.-C; Wong, C-Y; Lee, D.K.T. Stability of cefazolin sodium-famotidine admixture.Am.J.Hosp.Pharm., 1994, 51, 2205-2209SAMPLEMatrix: formulationsSa mple p re p ara ti on : Shake, remove 2 mL of oral suspension, dilute to 40 mL with water,vortex 1 min, centrifuge at 2000 rpm for 10 min. Dilute a 100 |xL aliquot of supernatantwith 100 |xL of 100 |xg/mL theophylline and add 800 |xL water, inject 20 |JLL aliquot.HPLCVARIABLESColumn: 300 mm 10 |xm Waters reversed-phase C18Mobile phase : MeCN: 50 mM sodium acetate buffer 8:92, adjusted to pH 6.5Flow rate: 1.5Injection volume: 20D etec tor: UV 254C H R O M A T O G R A MRetention time: 5.6Internal standard: theophylline (4.3)KEYWORDSstability-indicatingREFERENCEQuercia, R.A.; Jay, G.T.; Fan, C ; Chow, M.S. Stability of famotidine in an extemp oraneously prep aredoral liquid. Am.J.Hosp.Pharm., 1993, 50, 6 9 1 - 6 9 3SAMPLEMatrix: solutionsHPLC VARIABLESColum n: 250 X 4.6 5 ixm octadecylsilane (Beckman)Mobile phase : MeOH:MeCN:glacial acetic acid: 10 mM KH2PO4 12:3:0.1:84.9, pH 5.0Flow rate: 1D etecto r: UV 266REFERENCEJunnarkar, G.H.; Stavchansky, S. Isothermal and nonisothermal decomposition of famotidine in aqueoussolution. Pharm.Res., 1995, 12, 599-604SAMPLEMatrix: solutionsHPLCVARIABLESColumn: 150 X 4.6 12 |xm l-m3o-istoyl-2-[(13-carboxyl)-tridecoyl]-sn-3-glycerophosphocho-line chemically bonded to silica (Regis)M obile phase : MeCN: 100 mM pH 7.0 phosphate buffer 20:80Flow rate: 1D etec tor: UV 254


5/6

CHROMATOGRAMRetention t ime: k/ 0 .54OTHER SUBSTANCESAlso analyzed: acebutolol, alprenolol, antaz oline , ateno lol, betaxolol, bisoprolol, bopindolol,bupranolol, carteolol, celiprolol, chloropyramine, chlorpheniramine, cicloprolol, cimeti-dine, cinnarizine, cirazoline, clonidine, dilevalol, dimethindene, diphenhydramine, doxa-zosin, esmolol, isothipendyl, ketotifen, metiamide, metoprolol, moxonidine, nadolol, na-phazoline, nifenalol, nizatidine, oxprenolol, pheniramine, phentolamine, pindolol,pizotyline (pizotifen), practolol, prazosin, promethazine, propranolol, pyrilamine (mepyr-amine), ranitidine, roxatidine, sotalol, tiamenidine, timolol, tramazoline, tripelennamine,triprolidine, tymazoline, UK-14,304REFERENCEKaliszan, R.; Nasal, A.; Turowski, M. Binding site for basic drugs on c^-acid glycoprotein as revealed bychemometric analysis of biochromatographic data. Biomed.Chromatogr., 1995, 9, 211-215SAMPLEMatrix: solutionsHPLC VARIABLESColumn: 250 X 4.6 Zorbax RXMobile phase: Gra dient. A was 10 mL concen trated orthophosph oric 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, make u p to 1 L with M eCN. A:B from 100:0 to 0:100 over

30 min, maintain at 0:100 for 5 min.Column temperature: 30Flow rate: 2D etec tor: UV 210OTHER SUBSTANCESAlso analyzed: acepromazine, acetaminophen, acetophenazine, albuterol, aminophylline,amitriptyline, amobarbital, amoxapine, amphetamine, amylocaine, antipyrine, aprobar-bital, asp irin, atenolol, atropin e, averme ctin, barb ital, benzocaine, benzoic acid, benzotro-pine, benzphetamine, berberine, bibucaine, bromazepan, brompheniramine, buprenor-phine, buspirone, butabarbital, butacaine, butethal, caffeine, carbamazepine, carbromal,chloramphenicol, chlordiazepoxide, chloroquine, chlorothiazide, chloroxylenol, chlorphe-nesin, chlorpheniramine, chlorpromazine, chlorpropamide, chlortetracycline, cimetidine,cinchonidine, cinchonine, clenbuterol, clonazepam, clonixin, clorazepate, cocaine, codeine,colchicine, cortisone, coumarin, cyclazocine, cyclobenzaprine, cyclothiazide, cyheptamide,cymarin, danazol, danthron, dapsone, debrisoquine, desipramine, dexamethasone, dex-tromethorphan, dextropropoxyphene, diamorphine, diazepam, diclofenac, diethylpropion,diethylstilbestrol, diflunisal, digitoxin, digoxin, diltiazem, diphenhydramine, diphenoxy-late, diprenorphine, dipyrone, disulfiram, dopamine, doxapram, doxepin, dronabinol,ephedrine, epinephrine, epinine, estradiol, estriol, estrone, ethacrynic acid, ethosuximide,etonitazene, etorphine, eugenol, fenbendazole, fencamfamine, fenoprofen, fenproporex,

fentanyl, flubendazole, flufenamic acid, flunitrazepam, 5-fluorouracil, fluoxymesterone,fluphenazine, furosemide, gentisic acid, gitoxigenin, glipizide, glunixin, glutethimide, gly-benclamide, guaiacol, halazepam, haloperidol, hydrochlorothiazide, hydrocodone, hydro-cortisone, hydromorphone, hydroxyquinoline, ibogaine, ibuprofen, iminostilbene, imipra-mine, indomethacin, isocarbostyril, isocarboxazid, isoniazid, isoproterenol, isoxsuprine,ivermectin, k etam ine, ketoprofen, kynu renic acid, levorphanol, lidocaine, lorazepam , lor-me tazepam , loxapine, mazindol, mebendazole, meclizine, meclofenamic acid, med azepam ,mefenamic acid, megestrol, mepacrine, meperidine, mephentermine, mephenytoin, me-phesin, mephobarbital, mepivacaine, mescaline, mesoridazine, methadone, methamphet-amine, methapyrilene, methaqualone, methazolamide, methocarbamol, methoxamine,methsuximide, methyl salicylate, methyldopa, methyldopamine, methylphenidate, meth-


6/6

ylprednisolone, me thyltesto steron e, methyp rylon, mei prolol, mibolerone, m orphine , na-dolol, nalorphine, naloxone, naltrexone, naphazoline, naproxen, nefopam, niacinamide,nicotine, nicotinic acid, nifedipine, niflumic acid, nitrazepam, norepinephrine, nortripty-line, noscapine, nylidrin, oxazepam, oxycodone, oxymorphone, oxyphenbutazone, oxytet-racycline, papaverine, pargyline, pemoline, pentazocine, pentobarbital, persantine, phe-nacetin, phenazocine, phenazopyridine, phencyclidine, phendimetrazine, phenelzine,pheniramine, phenobarbital, phenothiazine, phensuximide, phentermine, phenylbuta-zone, phenylephrine, phenylpropanolamine, piperocaine, prazepam , prednisolone, primi-done, probenecid, progesterone, propiomazine, propranolol, propylparaben, pseudoephed-r ine, puromycin, pyrilamine, pyrithyldione, quazepam, quinaldic acid, quinidine, quinine,ranitidine, recinnamine, reserpine, resorcinol, saccharin, albuterol, salicylamide, salicylicacid, scopolamine, scopoletin, secobarbital, strychnine, sulfacetamide, sufadiazine, sulfad-imethoxine, sulfaethidole, sulfamerazine, sulfamethazine, sulfamethoxizole, sulfanila-mide, sulfapyridine, sulfasoxizole, sulindac, tamoxifen, temazepam, testosterone, tetra-caine, tetracycline, tetramisole, thebaine, theobromine, theophylline, thiabendazole,thiamine, thiamylal, thiobarbituric acid, thioridazine, thiosalicylic acid, thiothixene, thy-mol, tolazamide, tolazoline, tobutamide, tolmetin, tranylcypromine, triamcinolone, triben-zylamine, trichloromethiazide, trifluoperazine, trihexyphenidyl, trimethoprim, tripelen-nam ine, triproilidine, tropacocaine, tyram ine, verapam il, vincamine, warfarin, yohimbine,zoxazolamine

REFERENCEHill, D.W.; Kind , A. J. Reversed-phase solvent gradient HPLC retention indexes of drugs. J. Anal.Toxicol.,1994, 18, 233-242 ANNOTATED BIBLIOGRAPHYQin, X.Z.; Ip, D.P.; Chan g, K.H.; Drad ransky , P.M.; Brooks, M.A.; Sa kum a, T. Pha rm aceu tical applicationof LC-M S. 1-Characterization of a famotidine degradate in a package screening study by LC-APCIMS. J.Pharm.Biomed.AnaL, 1994, 12, 221-233Kamath, B.V.; Shivram, K.; Newalkar, B.L.; Shah, A.C. Liquid chromatographic analysis and degrada-tion kinetics of famotidine. J.Liq.Chromatogr., 1993, 16, 1007 -1014 [tablets; stability indicating]Imai, Y.; Kobayashi, S. A simple metho d for the quantification of famotidine in hu m an p lasm a an d u rin eby paired-ion high performance liquid chromatography. Biomed.Chromatogr., 1992, 6, 2 2 2 - 2 2 3Cvitkovic, L.; Zupancic-Kralj, L.; Marsel, J. Determination of famotidine in human plasma and urineby high-performance liquid chromatography. J.Pharm.Biomed.AnaL, 1991, 9, 207-210Guo, P.; Ye, L.M.; Lu, B.; He, Y. J.; Li, Z.W. [Direct injection of pla sm a to de term ine fam otidine in p lasm ausing HPLC column switching technique]. Yao Hsueh Hsueh Pao, 1990, 25, 6 2 2 - 6 2 5Bullock, L.; Fitzgerald, J.R; Glick, M.R. Stability of famotidine 20 and 50 mg/L in total nutrient ad-mixtures . Am.J.Hosp.Pharm., 1989, 46, 2326-2329 [theophylline (IS)]Bullock, L.; Fitzgerald, J.F.; Glick, M.R.; Parks, R.B.; Schnabel, J.G.; Hancock, B.G. Stability of famo-tidine 20 and 40 mg/L and amino acids in total parenteral nutrient solutions. Am.J.Hosp.Pharm.,1989, 46, 2321-2325 [stability-mdicating; theophylline (IS)]DiStefano, J.E.; Mitrano, F.P.; Baptista, R.J.; Der, M.M.; Silvestri, A.P.; Palombo, J.D.; Bistrian, B.R.Long-term stability of famotidine 20 mg/L in a total pa ren tera l nu trie nt solution. Am.J.Hosp.Pharm.,1989, 46, 2333-2335 [non-interfering degradation products]

Fa Moti Dine

Documents