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Cefixime

Molecular formula: C16H15N5O7S2 Molecular weight: 453.4 CAS Registry No.: 79350-37-1

SAMPLE Matrix: bile, blood Sample preparation: Plasma. 25 |xL Plasma + 25 |xL buffer + 450 |xL 5% trichloroacetic acid, mix, centrifuge, inject a 10 |xL aliquot of the supernatant. Bile. 100 |xL Bile + 900 J L J L L buffer, mix, centrifuge at 2000 rpm for 5 min, inject a 10 J U L L aliquot of the supernatant. (Buffer was 2.54% NaH2PO4.2H2O and 4.41% Na2HPO4.12H2O, pH 7.4.) HPLCVARIABLES Column: 150 X 4.6 Chemcosorb 7C18 (Chemco) Mobile phase: MeCN: buffer 11:89 (plasma) or 13:87 (bile) (Buffer was 20 mM (NH4)H2PO4 adjusted to pH 3.2 with phosphoric acid.) Column temperature: 40 Flow rate: 2 (plasma), 1 (bile) Injection volume: 10 Detector: UV 290 KEYWORDS rat; plasma REFERENCE
Yasui, H.; Yamaoka, K.; Nakagawa, T. Alternative continuous infusion method for analysis of enterohepatic circulation and biliary excretion of cefixime in the rat. J.Pharm.ScL, 1994, 83, 819-823

SAMPLE Matrix: blood Sample preparation: 100 |xL Serum + 10 jxL 5 |xg/mL cephalexin 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 5080 |xL 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: 11 Internal standard: cephalexin (15) Limit of detection: 100 ng/mL OTHER SUBSTANCES Extracted: cefaclor, cefadroxil, 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 cephalosporinscefixime, cefaclor, cefadroxil, cephalexin, and cephradinein human serum. Clin.Chem., 1987, 33, 1788-1790

SAMPLE Matrix: blood, CSF Sample preparation: 150 |xL Serum or CSF + 150 |xL 6% trichloroacetic acid, centrifuge for 3 min, inject 75 |xL supernatant. HPLCVARIABLES Column: 150 X 4.6 3 |xm Techsphere C18 Mobile phase: 170 mL MeCN + 1.36 g NaH2PO4 + 2 mL phosphoric acid + 828 mL water adjusted to pH 2.7 Flow rate: 2 Injection volume: 75 Detector: UV 313 KEYWORDS serum; method has advantages over that of Falkowski et al. (J. Chromatogr. 1987; 422; 145152) REFERENCE
White, L.O.; Reeves, D.S.; Lovering, A.M.; MacGowan, A.P. HPLC assay of cefixime in serum and CSF. J.Antimicrob.Chemother., 1993, 31, 450-451

SAMPLE Matrix: blood, tissue, urine Sample preparation: Serum, plasma. Dilute serum or plasma 1:2 to 1:10 with buffer, centrifuge, inject a 20 |xL aliquot of supernatant. Urine. Dilute urine 1:10 to 1:100 with buffer, centrifuge, inject a 20 |JLL aliquot of supernatant. Tissue (lung, gut). Cut tissue with a scalpel, homogenize with 1-3 mL buffer, centrifuge at 9600 g for 5 min three times, inject a 20 |xL aliquot. Tissue (chondral). Cut tissue with a scalpel, homogenize with 3-6 mL buffer in an ice bath for 2-3 min, centrifuge at 9600 g for 5 min four or five times, inject a 100 |xL aliquot. Pleural. Dilute human pleural samples with buffer, centrifuge, inject a 20 |xL aliquot. (Buffer was 66.6 mM K2HPO4 adjusted to pH 7.40 with KH2PO4.) HPLCVARIABLES Column: 200 X 4 5 |xm Nucleosil C18 Mobile phase: MeOH: buffer 15:85, adjusted to pH 5.2 with phosphoric acid (Buffer was 57.4 mM K2HPO4 adjusted to pH 5.2 with phosphoric acid.) Flow rate: 1 Injection volume: 20-100 Detector: UV 230 CHROMATOGRAM Retention time: 9 Limit of detection: 100 ng/mL

KEYWORDS serum; plasma; lung; gut; pleural; chondral REFERENCE


Knoller, J.; Kdnig, W.; Schonfeld, W.; Bremm, K.D.; Roller, M. Application of high-performance liquid chromatography of some antibiotics in clinical microbiology. J.Chromatogr., 1988, 427, 257-267

SAMPLE Matrix: blood, urine Sample preparation: Serum. 250 JULL Serum + 250 |xL 4 |xg/inL IS in 6% trichloroacetic acid in water, vortex at high speed for 15 s, centrifuge at 30000 g for 2 min, inject a 75 |xL aliquot of the supernatant. Urine. 100 |xL Urine + 2 mL 0.25 |xg/mL IS in 6% trichloroacetic acid in water, vortex at high speed for 15 s, centrifuge at 30000 g for 2 min, inject a 75 |xL aliquot of the supernatant. HPLCVARIABLES Column: 100 X 8 5 |xm Nova-Pak C18 RCM-100 Mobile phase: MeCN.water:85% phosphoric acid 17:82.8:0.2 containing 1.36 g/L KH2PO4, pH 2.7 (serum) or MeCN: water: 85% phosphoric acid 20:79.8:0.2 containing 1.36 g/L KH2PO4, pH 2.7 (urine) Flow rate: 2 Injection volume: 75 Detector: UV 280 (serum); UV 313 (urine) CHROMATOGRAM Retention time: 3.5 (serum), 4 (urine) Internal standard: 7-hydroxycoumarin (5.6 (serum), 6.8 (urine)) Limit of quantitation: 50 ng/mL (serum); 1000 ng/mL (urine) OTHER SUBSTANCES Noninterfering: acetaminophen, caffeine, salicylic acid, theophylline KEYWORDS serum; human; rat; dog; monkey REFERENCE
Falkowski, A.J.; Look, Z.M.; Noguchi, H.; Silber, B.M. Determination of cefixime in biological samples by reversed- phase high-performance liquid chromatography. J.Chromatogr., 1987, 422, 145-152

SAMPLE Matrix: blood, urine Sample preparation: Dilute serum 1:10 with buffer, dilute urine 1:10-100 with buffer, centrifuge at 9300 g for 4 min, inject 20 jxL of supernatant. (Buffer was 60 mmol K2HPO4 adjusted to pH 7.40 with 50 mmol KH2PO4 (Soerensen buffer).) HPLCVARIABLES Column: 200 X 4 Nucleosil 5 C18 Mobile phase: MeOH: 43 mM K2HPO4 15:85 adjusted to pH 5.20 with phosphoric acid Flow rate: 1 Injection volume: 20 Detector: UV 230 CHROMATOGRAM Retention time: 12 Limit of detection: 100 ng/mL

KEYWORDS serum REFERENCE


Knoller, J.; Schonfeld, W.; Bremm, K.D.; Konig, W. In vitro stability of cefixime (FK-027) in serum, urine and buffer. J.Chromatogr., 1987, 389, 312-316

ANNOTATED BIBLIOGRAPHY

Liu, G.L.; Sha, R.G.; Gao, S.; Shen, Y.X.; Wang, S.X. [Determination of cefixime in human plasma and urine using high performance liquid chromatography column switching technique]. Yao Hsueh Hsueh Poo, 1993, 28, 216-221 Nahata, M.C. Measurement of cefixime in serum and cerebrospinal fluid by high-performance liquid chromatography. J.Liq.Chromatogr., 1991, 14, 3755-3759 [serum; CSF; 7-hydroxycoumarin (IS); LOD 30 ng/mL]

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