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TITLE:  A determinative and confirmatory method for ceftiofur metabolite desfuroylceftiofur cysteine disulfide in bovine kidney by LC-MS/MS
AUTHORS:  Feng S;Chattopadhaya C;Kijak P;Chiesa OA;Tall EA;
YEAR:  2012
JOURNAL ABBREV:  J Chromatogr B Analyt Technol Biomed Life Sci
JOURNAL FULL:  Journal of chromatography B, Analytical technologies in the biomedical and life sciences
VOLUME:  898
KEYWORDS:  Bacterial Infections;Calibration;Cattle;confirmation;control;drug;Food;INFECTION;INFECTIONS;Kidney;RESIDUE;residues;SINGLE;TISSUE;TISSUES;United States;UNITED-STATES;veterinary;Veterinary Medicine;
ABSTRACT:  Ceftiofur is a cephalosporin beta-lactam antibiotic widely used for treating certain bacterial infections in beef and dairy cattle. The regulatory HPLC-UV method for ceftiofur residues in animal tissues is time consuming and non-specific. Additionally, because the regulatory method involves chemical reactions to convert the metabolites into a single moiety, it is virtually impossible to incorporate the procedure into a multi-residue method. Ceftiofur residue violations in beef and dairy cattle have been frequently reported and therefore an improved method is needed. Herein we report a rapid and sensitive LC-MS/MS method for the determination and confirmation of ceftiofur metabolite, desfuroylceftiofur cysteine disulfide (DCCD), in bovine kidney tissue. The new method utilizes a simple extraction with phosphate buffer followed by SPE cleanup. A deuterated internal standard was synthesized and used for quantitation. The matrix-based calibration curve was linear from 25 to 2000ng/g. The average accuracy for control kidney samples from six different sources fortified at 50-1000ng/g was 97.7-100.2% with CV
AFFILIATIONS:  Center for Veterinary Medicine, U.S. Food and Drug Administration, 8401 Muirkirk Road, Laurel, MD 20708, United States