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A determinative and confirmatory method for ceftiofur metabolite desfuroylceftiofur cysteine disulfide in bovine kidney by LC-MS/MS
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Feng S;Chattopadhaya C;Kijak P;Chiesa OA;Tall EA;
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2012
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J Chromatogr B Analyt Technol Biomed Life Sci
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Jun
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JOUR
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627
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Journal of chromatography B, Analytical technologies in the biomedical and life sciences
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898
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62
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68
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Bacterial Infections;Calibration;Cattle;confirmation;control;drug;Food;INFECTION;INFECTIONS;Kidney;RESIDUE;residues;SINGLE;TISSUE;TISSUES;United States;UNITED-STATES;veterinary;Veterinary Medicine;
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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=10.1%. The limit of confirmation was 50ng/g
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Center for Veterinary Medicine, U.S. Food and Drug Administration, 8401 Muirkirk Road, Laurel, MD 20708, United States
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