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开发并验证了一种通过创新的提取/净化程序和 LC-MS/MS 分析方法定性筛选猪肌肉中兽药的方法。

Development and validation of a methodology to qualitatively screening veterinary drugs in porcine muscle via an innovative extraction/clean-up procedure and LC-MS/MS analysis.

机构信息

Departamento de Química, Universidade Federal de Minas Gerais, Belo Horizonte/MG, 31270-901, Brazil.

出版信息

Food Addit Contam Part A Chem Anal Control Expo Risk Assess. 2011 Dec;28(12):1667-76. doi: 10.1080/19440049.2011.609136. Epub 2011 Oct 19.

DOI:10.1080/19440049.2011.609136
PMID:22007798
Abstract

A qualitative multiresidue method that facilitates rapid monitoring of veterinary drugs in porcine muscle is described. The method comprises the application of an innovative extraction/clean-up procedure, namely liquid-liquid extraction with partition at very low temperature (LLE-FPVLT), and analysis by liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS). Besides the high selectivity, sensitivity and specificity, this high-throughput method proved to be quite general as 34 veterinary drugs (from six distinct classes: tetracyclines, sulfonamides, penicillins, quinolones, macrolides and benzimidazoles) could be successfully detected. The whole screening procedure was validated according to the directives from European Commission Decision 2002/657/EC and guidelines for the validation of screening methods. Acceptable values for the evaluation parameters were achieved for all analytes (except for ampicillin, clindamycin and erythromycin). Finally, these very promising results have strengthened the possibility of inclusion of such a methodology as an integral part of the National Residue Control Plan scope of the Ministry of Agriculture, Livestock and Food Supply of Brazil.

摘要

本文描述了一种可快速监测猪肌肉中兽药残留的多残留定性分析方法。该方法包括应用一种创新的提取/净化程序,即极低温度下的液-液萃取/分配(LLE-FPVLT),以及液相色谱-串联质谱(LC-MS/MS)分析。除了高选择性、灵敏度和特异性外,这种高通量方法还具有很强的通用性,可成功检测到 34 种兽药(来自 6 个不同类别:四环素类、磺胺类、青霉素类、喹诺酮类、大环内酯类和苯并咪唑类)。整个筛选过程符合欧洲委员会第 2002/657/EC 号决定和筛选方法验证指南的要求。所有分析物(氨苄西林、克林霉素和红霉素除外)的评估参数均达到可接受值。最后,这些非常有前景的结果增强了将这种方法纳入巴西农业、畜牧业和食品供应部国家残留控制计划范围的可能性。

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