A determinative and confirmatory method for ceftiofur metabolite desfuroylceftiofur cysteine disulfide in bovine kidney by LC-MS/MS
- 作者：Shixia Feng ; shixiafeng@fda.hhs.gov ; Chaitali Chattopadhaya ; Philip Kijak ; Oscar A. Chiesa ; Elizabeth A. Tall
- 关键词：Ceftiofur ; Desfuroylceftiofur cysteine disulfide ; Bovine kidney ; LC&ndash ; MS/MS
- 刊名：Journal of Chromatography B ; Analytical Technologies in the Biomedical and Life Sciences
- 出版年：2012
- 期刊代码：124_15700232
- 类别：ch
- 出版时间：1 June, 2012
- 卷：898
- 期：Complete
- 页码：62-68
- 文件大小：383 K
摘要
Ceftiofur is a cephalosporin 尾-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 2000 ng/g. The average accuracy for control kidney samples from six different sources fortified at 50-1000 ng/g was 97.7-100.2%with CV 鈮?#xA0;10.1%. The limit of confirmation was 50 ng/g.