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采用毛细管电泳激光诱导荧光检测法筛选和液相色谱-串联质谱法确认磺胺类残留:依据欧盟 2002/657/EC 进行验证。

Use of capillary electrophoresis with laser-induced fluorescence detection to screen and liquid chromatography-tandem mass spectrometry to confirm sulfonamide residues: validation according to European Union 2002/657/EC.

机构信息

Programa de Pós-Graduação em Biologia Celular e Molecular, Centro de Biotecnologia do Estado do Rio Grande do Sul, Universidade Federal do Rio Grande do Sul, Porto Alegre, RS, Brazil.

出版信息

J Chromatogr A. 2009 Nov 13;1216(46):8254-61. doi: 10.1016/j.chroma.2009.07.074. Epub 2009 Aug 12.

Abstract

A multiresidue method is described for determining six sulfonamides (SAs) (sulfadiazine, sulfathiazole, sulfamethazine, sulfamethoxazole, sulfaquinoxaline and sulfadimethoxine) in liver by a capillary electrophoresis screening method and a liquid chromatography coupled to tandem mass spectrometry confirmatory assay. Samples were prepared by homogenizing the tissue, with sodium hydroxide and acetonitrile. After evaporation, extracts were injected in the capillary electrophoresis system or mass spectrometry system for confirmatory analysis. The detection of analytes was achieved by laser-induced fluorescence in capillary electrophoresis. Procedures were validated according to the European Union regulation 2002/657/EC determining specificity, selectivity and detection capability for screening method and decision limit, detection capability, specificity, selectivity, trueness and precision for confirmation method. The results of validation process demonstrate that the method is suitable for application in Brazilian statutory veterinary drug residue surveillance programs. Capillary electrophoresis was proved to be a fast, robust method with low time and reagents consumption.

摘要

一种多残留方法被描述用于通过毛细管电泳筛选方法和液相色谱串联质谱确证测定肝中的六种磺胺类药物(SAs)(磺胺嘧啶、磺胺噻唑、磺胺甲恶唑、磺胺甲噁唑、磺胺喹噁啉和磺胺二甲氧嘧啶)。样品通过组织匀浆,用氢氧化钠和乙腈制备。蒸发后,提取物注入毛细管电泳系统或质谱系统进行确证分析。在毛细管电泳中通过激光诱导荧光检测分析物。程序根据欧盟法规 2002/657/EC 进行验证,确定筛选方法的特异性、选择性和检测能力以及决策限、检测能力、特异性、选择性、准确度和精密度的确认方法。验证过程的结果表明,该方法适用于巴西法定兽药残留监测计划的应用。毛细管电泳被证明是一种快速、稳健的方法,具有低时间和试剂消耗。

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