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Cefadroxil

Molecular formula: C16H17N3O5S Molecular weight: 363.4 CAS Registry No.: 66592-87-8

SAMPLE Matrix: blood Sample preparation: 100 |xL Plasma + 8 mL dichloromethane, shake for 20 min, centrifuge at 2500 rpm for 20 min. Remove 7 mL of the organic layer and evaporate it to dryness under nitrogen or at 60. Dissolve residue in 200 |xL mobile phase, inject a 20 \iL aliquot. HPLCVARIABLES Column: 150 X 6 Shimpack CLS-ODS (Shimadzu) Mobile phase: MeCN: 0.5 mM phosphoric acid 12:88 Column temperature: 40 Flow rate: 1.5 Injection volume: 20 Detector: UV 254 CHROMATOGRAM Internal standard: cefadroxil OTHER SUBSTANCES Simultaneous: antipyrine KEYWORDS plasma; rat; cefadroxil is IS REFERENCE
Lee, C.K.; Uchida, T.; Kitagawa, K.; Yagi, A.; Kim, N.-S.; Goto, S. Skin permeability of various drugs with different lipophilicity. J.Pharm.Sci., 1994, 83, 562-565

SAMPLE Matrix: blood Sample preparation: 100 |xL Serum + 1 mL MeCN, vortex, centrifuge at 2000 g for 10 min. Remove the aqueous phase and add it to 2.5 mL dichloromethane, vortex, centrifuge, inject a 25 JJIL aliquot of the upper aqueous layer. HPLCVARIABLES Column: 150 x 3.9 5 jxm C18 (Waters) Mobile phase: MeCN: 150 mM ammonium acetate 0.7:99.3, pH 7.0 Flow rate: 1.1 Injection volume: 25 Detector: UV 254 CHROMATOGRAM Internal standard: cefadroxil OTHER SUBSTANCES Extracted: ceftibuten

KEYWORDS serum; mouse; cefadroxil is IS REFERENCE


Onyeji, CO.; Nicolau, D.P.; Nightingale, CH.; Quintiliani, R. Optimal times above MICs of ceftibuten and cefaclor in experimental intra-abdominal infections. Antimicrob.Agents Chemother., 1994, 38, 1112-1117

SAMPLE Matrix: blood Sample preparation: 500 jxL Plasma + 100 u,L 100 |xg/mL cefadroxil + 300 JJLL 5% trichloroacetic acid + 500 |xL MeCN + 1.5 mL dichloromethane, vortex for 10 s, centrifuge at 500-600 g at 5 for 10 min, inject a 25 |JLL aliquot of the aqueous supernatant. HPLCVARIABLES Guard column: 23 X 4 37-50 |xm Corasil C18 Column: 150 X 4 Nova-Pak Mobile phase: MeCN: 5 mM 1-octanesulfonic acid 12:88 Flow rate: 1 Injection volume: 25 Detector: UV 280 CHROMATOGRAM Retention time: 10 Internal standard: cefadroxil OTHER SUBSTANCES Extracted: cefepime KEYWORDS plasma; rat; cefadroxil is IS REFERENCE
Barbhaiya, R.H.; Forgue, S.T.; Shyu, W.C; Papp, E.A.; Pittman, K.A. High-pressure liquid chromatographic analysis of BMY-28142 in plasma and urine. Antimicrob.Agents Chemother., 1987, 31, 55 59

SAMPLE Matrix: blood Sample preparation: 100 u-L Serum + 10 |xL 200 |xg/mL cephradine in water + 100 |xL 6% trichloroacetic acid, vortex, centrifuge at 9000 g for 10 min, inject 25 |xL supernatant. HPLCVARIABLES Guard column: Waters Guard-Pak C18 Column: 200 X 4.6 5 ^m Nucleosil SA Mobile phase: 20 mM Ammonium dihydrogen phosphate to final concentration of 20 mM in water:MeOH:MeCN 30:35:35. The pH was adjusted to 3.0 with concentrated phosphoric acid. Flow rate: 1.5 Injection volume: 25 Detector: UV 240 CHROMATOGRAM Retention time: 7.7 Internal standard: cephradine Limit of quantitation: 1 \xgJmL

KEYWORDS

serum
REFERENCE
Lindgren, K. Determination of cefadroxil in serum by high-performance liquid chromatography with cephradine as internal standard. J.Chromatogr., 1987, 413, 347-350

SAMPLE

Matrix: blood Sample preparation: 100 |xL Serum + 10 |xL 5 jx^mL cefixime in MeOH + 100 \xL MeCN, vortex for 15 s, centrifuge at 14000 g for 2 min. Remove the supernatant and evaporate it under a stream of nitrogen, reconstitute in 100 |xL mobile phase, inject a 50-80 jxL aliquot.
HPLCVARIABLES

Guard column: RCSS Silica Guard Pak (Waters) Column: 150 X 4.6 5|xm Ultrasphere Octyl C8 Mobile phase: MeOH: 12.5 mM pH 2.6 NaH2PO4 (pH adjusted with concentrated phosphoric acid) 20:80 Flow rate: 2 Injection volume: 50-80 Detector: UV 240
CHROMATOGRAM

Retention time: 3 Internal standard: cefixime (11) Limit of detection: 1 \g/ mL OTHER SUBSTANCES Extracted: cefaclor, cephalexin, cephradine Noninterfering: acetaminophen, cimetidine, diazepam, digoxin, ibuprofen, phenytoin, propranolol, salicylic acid, warfarin
KEYWORDS

serum
REFERENCE
McAteer, J.A.; Hiltke, M.R; Silber, B.M.; Faulkner, R.D. Liquid-chromatographic determination of five orally active cephalosporins- cefixime, cefaclor, cefadroxil, cephalexin, and cephradine-in human serum. Clin.Chem., 1987, 33, 1788-1790

SAMPLE

Matrix: blood Sample preparation: 1 mL Plasma + 1 mL MeCN, shake 30 s, centrifuge 5 min. Transfer upper layer phase, add 6 mL dichloromethane, shake 5 min, centrifuge 5 min, inject 10100 |JLL upper aqueous phase.
HPLCVARIABLES

Column: 300 X 3.9 /xBondapak C18 Mobile phase: MeOH: 10 mM pH 4.8 buffer 5:95 Flow rate: 1.5 Injection volume: 10-100 Detector: UV 240
CHROMATOGRAM

Retention time: 6.4 Limit of detection: 150 ng/mL

KEYWORDS plasma REFERENCE


Brisson, A.M.; Fourtillan, J.B. Pharmacokinetic study of cefadroxil following single and repeated doses. J.Antimicrob.Chemother., 1982, 10 Suppl B, 11-15

SAMPLE Matrix: blood, middle ear fluid Sample preparation: Condition a 2.8 mL 500 mg Bond Elut C18 SPE cartridge with 4 mL MeOH and 1 mL 50 mM pH 6.8 phosphate buffer. 200 |xL Plasma or 50 (xL middle ear fluid + 1 mL 50 mM pH 6.8 phosphate buffer, vortex, add to the SPE cartridge, wash with 1 mL 50 mM pH 6.8 phosphate buffer, wash with 1 mL buffer, dry under vacuum, elute with 1 mL MeOH: water 40:60. Evaporate the eluate to dryness under a stream of nitrogen at 40, reconstitute with 35 JJLL MeOH: water 5:95, inject a 25 |xL aliquot. HPLCVARIABLES Guard column: 10 x 2 5 \xm MOS Hypersil C8 Column: 150 X 2 5 |jim MOS Hypersil C8 Mobile phase: MeCN: 5 mM phosphate buffer containing 5 mM tetrabutylammonium 6: 94, adjusted to pH 6.5 (After 14 min wash column with MeCN: buffer 25:75 for 2 min, re-equilibrate for 4 min.) Column temperature: 40 Flow rate: 0.35 Injection volume: 25 Detector: UV 210 CHROMATOGRAM Retention time: 12.30 Internal standard: cefadroxil OTHER SUBSTANCES Extracted: amoxicillin KEYWORDS plasma; SPE; cefadroxil is IS REFERENCE
Yuan, Z.; Russlie, H.Q.; Canafax, D.M. Sensitive assay for measuring amoxicillin in human plasma and middle ear fluid using solid-phase extraction and reversed-phase high-performance liquid chromatography. J.Chromatogr.B, 1995, 674, 93-99

SAMPLE Matrix: blood, urine Sample preparation: Plasma. 150 |xL Plasma + 150 |xL MeCN, vortex, rotate at 20 rpm for 10 min; centrifuge at 1000 g for 10 min. Transfer supernatant to another tube and add 7 volumes dichloromethane, equilibrate for 10 min; rotate at 20 rpm for 10 min; centrifuge at 1000 g for 10 min, inject an aliquot of the upper aqueous layer (J.Chromatogr. 1987, 413, 109). Urine. Dilute with water, inject an aliquot. HPLCVARIABLES Guard column: C18 Column: 150 X 1.6 Spherisorb S5-ODS2 C18 Mobile phase: MeOH: 100 mM pH 3 acetate buffer 13:87 Flow rate: 1 Detector: UV 254

CHROMATOGRAM

Limit of detection: 300 ng/mL


KEYWORDS

plasma; rat; pharmacokinetics


REFERENCE
Gimeno, M.J.; Martinez, M.; Granero, L.; Torres-Molina, R; Peris, J.-E. Influence of probenecid on the renal excretion mechanisms of cefadroxil. Drug Metab.Dispos., 1996, 24, 270-272

SAMPLE

Matrix: blood, urine Sample preparation: 1 mL Plasma + 1 mL 6% trichloroacetic acid, mix, centrifuge at 4000 rpm for 10 min, inject an aliquot of the supernatant. Inject an aliquot of urine directly.
HPLCVARIABLES

Guard column: 10x 47 jim Lichrosorb RP 18 Column: 250 X 4 7 |xm Lichrosorb RP 18 Mobile phase: MeCN: 25 mM pH 7 phosphate buffer 5:95 Flow rate: 1 Injection volume: 10 Detector: F ex 385 em 485 following post-column reaction. The column effluent mixed with 200 |xg/mL fluorescamine in MeCN pumped at 0.25 mL/min and the mixture flowed through a 4.5 m X 0.25 mm ID coil of PTFE tubing to the detector.; UV 260
CHROMATOGRAM

Limit of detection: 0.3 ng/mL (F); 0.6 ng/mL (UV)


OTHER SUBSTANCES

Noninterfering: amidopyrin, aspirin, barbital, caffeine, cefmenoxime, cefotaxime, ceftizoxime, ceftriaxone, cetazidime, diazepam, dibekacin, gentamycin, kanamycin, lidocaine, netilmicin, tetracaine, theophylline, tobramycin
KEYWORDS

post-column reaction; plasma; F detection may be less susceptible to interferences


REFERENCE
Blanchine, M.D.; Fabre, H.; Mandrou, B. Fluorescamine post-column derivatization for the HPLC determination of cephalosporins in plasma and urine. J.Liq.Chromatogr., 1988, 11, 2993-3010

SAMPLE

Matrix: bulk, formulations Sample preparation: Homogenize sample, weigh out sample equivalent to 50 mg cefadroxil, make up to 50 mL with 100 mM pH 4.5 phosphate buffer. Take 5 mL of this solution, add 0.5 mL 30 mg/mL dimethyl phthalate in MeCN: water 1:1, make up to 50 mL with 100 mM pH 4.5 phosphate buffer.
HPLCVARIABLES

Column: 300 X 3.9 10 ^m ^Bondapak C18 Mobile phase: MeCN: 10 mM pH 4.5 phosphate buffer 60:40 Flow rate: 1 Injection volume: 10 Detector: UV 254

CHROMATOGRAM

Retention time: 2 Internal standard: dimethyl phthalate Limit of quantitation: 20 [xg/mL


KEYWORDS

capsules; powders
REFERENCE
Hsu, M.-C; Chang, Y-W.; Lee, Y.-T. Column liquid chromatography and microbiological assay compared for determination of cefadroxil preparations. J.Chromatogr., 1992, 609, 181-186

SAMPLE

Matrix: bulk, formulations Sample preparation: Dissolve in water to a concentration of 40 |xg/mL, inject a 20 (JLL aliquot.
HPLCVARIABLES

Column: 300 X 3.9 10 |xm ixBondapak C18 Mobile phase: MeOH: water: acetic acid 30:70:0.1 Flow rate: 1 Injection volume: 20 Detector: UV 254
CHROMATOGRAM

Retention time: 5 Limit of quantitation: 1.8 jxg/mL


OTHER SUBSTANCES

Simultaneous: impurities, cefaclor, cefamandole, cefamandole nafate, cefazolin, cefoperazone, cefotaxime, cefoxitin, ceftizoxime, cephalexin, cephalothin, cephapirin, cephradine
REFERENCE
Ting, S. Reverse-phase liquid chromatographic analysis of cephalosporins. J.Assoc.Off.Anal.Chem., 1988, 71, 1123-1130

SAMPLE

Matrix: milk Sample preparation: Condition a Bond Elut C8 SPE cartridge with 5 mL MeOH and 5 mL water. 20 mL Milk + 1 mL 1 M oxalic acid, heat at 60 for 10 min, centrifuge for 10 min, remove the supernatant and add it to 20 mL water and 400 (xL tributylamine, shake well, add to the SPE cartridge, wash with two 2.5 mL portions of water, elute with 2.5 mL MeOH. Evaporate the eluate to dryness under a stream of nitrogen, extract the residue with three 100 |xL portions of 50 mM pH 6.0 potassium phosphate buffer, filter (0.2 ixm), inject an aliquot of the filtrate. (Buffer was 545 mL 100 mM citric acid, 455 mL 200 mM Na2HPO4, and 74.4 g EDTA, adjust to pH 4.5 with ammonium hydroxide, make up to 2 L with water.)
HPLCVARIABLES

Column: 250 X 4.6 10 |xm Lichrosorb RP-8 Mobile phase: MeOH: 50 mM pH 6.0 potassium phosphate buffer 35:65 Flow rate: 1 Injection volume: 200 Detector: UV 210; Charm II assay

OTHER SUBSTANCES

Extracted: amoxicillin, ticarcillin Simultaneous: ampicillin, ceftiofur, cephapirin, cloxacillin, dicloxacillin, nafcillin, oxacillin, penicillin G
KEYWORDS

SPE
REFERENCE
Zomer, E.; Quintana, J.; Saul, S.; Charm, S.E. LC-Receptograms: A method for identification and quantitation of (J-lactams in milk by liquid chromatography with microbial receptor assay. J.AOAC Int., 1995, 78, 1165-1172

SAMPLE

Matrix: perfusate
HPLCVARIABLES

Guard column: 40 |xm C18 (Teknochroma) Column: 150 X 3.9 4 |xm Novapak C18 (Teknochroma) Mobile phase: MeCN:buffer 16:84, adjusted to pH 3.9 with dilute NaOH (Buffer was 5.8 mL glacial acetic acid and 2.456 g sodium laurylsulfate in 1 L water.) Flow rate: 1 Detector: UV 280
KEYWORDS

rat
REFERENCE
Sancho-Chust, V.; Fabra-Campos, S.; Gomez-Meseguer, V.; Bengochea, M.; Martin-Villodre, A. Experimental studies on the influence of surfactants on intestinal absorption of drugs. Cefadroxil as model drug and sodium lauryl sulfate as model surfactant: Studies in rat colon. Arzneimittelforschung, 1995, 45, 595-601

SAMPLE

Matrix: solutions
HPLCVARIABLES

Column: 250 X 4 OmniPac PCX-500 (Dionex) Mobile phase: Gradient. A was MeCN: 90 mM perchloric acid 13.5:86.5. B was MeCN: 300 mM perchloric acid 45:55. A:B from 100:0 to 0:100 over 7 min, maintain at 0:100. Flow rate: 1 Detector: UV 254
CHROMATOGRAM

Retention time: 6.5


OTHER SUBSTANCES

Simultaneous: 7-aminocephalosproranic acid, cefazolin, cefotaxime, cephalexin, cephaloridine, cephalosporin C, cephalothin, cephapirin, D-hydroxyphenylglycine
REFERENCE
Slingsby, R.W.; Rey, M. Determination of Pharmaceuticals by multi-phase chromatography: Combined reversed phase and ion exchange in one column. J.Liq.Chromatogr., 1990, 13, 107-134

SAMPLE

Matrix: surface wipes Sample preparation: Swab 100 X 100 mm surface with water (total volume 10 mL), remove excess liquid with a second swab, vortex swabs for 45 s, filter (0.45 jxm polycarbonate), inject a 50 |xL aliquot.
HPLCVARIABLES

Column: 150 X 4.6 5 |xm Nucleosil C18 Mobile phase: MeCN: 70 mM KH2PO4 4:96 Flow rate: 1 Injection volume: 50 Detector: UV 254
CHROMATOGRAM

Retention time: 5.6 Limit of quantitation: 100 ng/mL


REFERENCE
Gorski, R.J.; Plasz, A.C.; Elrod, L.J.; Yoder, J.; White, L.B. Determination of cefsulodin, cefmenoxime, and cefadroxil as residues on surfaces. Pharm.Res., 1991, 8, 15251527

SAMPLE

Matrix: tissue Sample preparation: Homogenize muscle with three volumes phosphate-buffered saline (Polytron, level 3) for 2 min, centrifuge at 1300 g for 10 min. 125 |xL Supernatant + 100 JJLL water + 800 JJLL MeCN, vortex for 30 s, centrifuge at 1600 g for 5 min. Remove the supernatant and evaporate it to dryness under a stream of nitrogen, reconstitute the residue in 125 \L mobile phase, inject a 50 |xL aliquot.
HPLCVARIABLES

Column: 4 jxm Novapak C18 Mobile phase: MeCN: 5 mm sodium heptanesulfonic acid 9:91, adjust pH to 3.33 with glacial acetic acid Flow rate: 2 Injection volume: 50 Detector: UV 280
CHROMATOGRAM

Retention time: 6.7 Internal standard: cefadroxil OTHER SUBSTANCES Extracted: cefepime
KEYWORDS

mouse; muscle; cefadroxil is IS


REFERENCE
Darouiche, R.; Musher, D.; Hamill, R.; Ou, C; Rognerud, C. Cephalosporin penetration into soft tissue of paralyzed limbs. Antimicrob.Agents Chemother., 1989, 33, 1326-1328

ANNOTATED BIBLIOGRAPHY

Changqin, H.; Shaohong, S.; Kaimin, W. The chromatographic behavior of cephalosporins in gel filtration chromatography, a novel method to separate high molecular weight impurities. J.Pharm.

Biomed.AnaL, 1994, 12, 533-541 [also cefamandole, cefmenoxime, cefoperazone, cefotaxime, ceftazidime, ceftriaxone, cephalexin, cephaloridine, cephalothin, cephradine] Muranushi, N.; Horie, K.; Masuda, K.; Hirano, K. Characteristics of ceftibuten uptake into Caco-2 cells. Pharm.Res., 1994, 11, 1761-1765 [also cefaclor, cefazolin, ceftibuten, cephalexin, cephradine, cyclacillin, latamoxef] Snippe, N.; Van de Merbel, N.C.; Ruiter, RRM.; Steijer, O.M.; Lingeman, H.; Brinkman, U.A.T. Automated column liquid chromatographic determination of amoxicillin and cefadroxil in bovine serum and muscle tissue using on-line dialysis for sample preparation. J.Chromatogr.B, 1994, 662, 61-70 [extracted amoxicillin; cow; serum; muscle; on-line dialysis; SPE; post-column reaction; LOD 50 ng/mL; LOD 200 ng/g] Nahata, M.C; Jackson, D.S. Liquid chromatographic method for the determination of cefadroxil in its suspension and in serum. J.Liq.Chromatogr., 1990, 13, 1651-1656 [suspensions; serum; cefaclor (IS)]

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