Determination of cephapirin and ceftiofur residues in bovine milk by liquid chromatography with ultraviolet detection

A method capable of quantitating cephapirin at a level fo 20 ng/mL and ceftiofur at a level of 50 ng/mL was developed for raw bovine milk. Raw bovine milk is deproteinated with acetonitrile. The supernatant is collected and then acetonitrile is removed under reduced pressure while warming in a water...

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Bibliographic Details
Published inJournal of AOAC International Vol. 81; no. 5; p. 973
Main Authors Schermerhorn, P G, Chu, P S, Ngoh, M A
Format Journal Article
LanguageEnglish
Published England 01.09.1998
Subjects
Animals
Cephalosporins - analysis
Cephapirin - analysis
Chromatography, Liquid
Drug Residues - analysis
Evaluation Studies as Topic
Food Contamination
Milk - chemistry
Spectrophotometry, Ultraviolet
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Summary:A method capable of quantitating cephapirin at a level fo 20 ng/mL and ceftiofur at a level of 50 ng/mL was developed for raw bovine milk. Raw bovine milk is deproteinated with acetonitrile. The supernatant is collected and then acetonitrile is removed under reduced pressure while warming in a water bath at 40 degrees-50 degrees C. The extract is mixed with water and loaded onto a conditioned C18 solid-phase extraction column. Analytes are eluted with acetonitrile, which is removed completely under a stream of nitrogen gas. Analytes are separated from coextractives by gradient elution with an ion-pair mobile phase on a reversed-phase column and are detected by ultraviolet absorbance at 290 nm. Mean recoveries from fortified milk samples ranged from 79 to 87% for cephapirin and from 76 to 86% for ceftiofur, with intralaboratory coefficients of variation ranging of 6-10% and 7-14%, respectively.
ISSN:1060-3271
DOI:10.1093/jaoac/81.5.973