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根据欧盟法规2002/657/EC对肌肉中磺胺类药物确证方法的验证。

Validation of a confirmatory method for the determination of sulphonamides in muscle according to the European Union regulation 2002/657/EC.

作者信息

Pecorelli Ivan, Bibi Rita, Fioroni Laura, Galarini Roberta

机构信息

Istituto Zooprofilattico Sperimentale dell'Umbria e delle Marche, via Salvemini, Perugia 1-06126, Italy.

出版信息

J Chromatogr A. 2004 Apr 2;1032(1-2):23-9. doi: 10.1016/j.chroma.2003.11.010.

Abstract

A simple multiresidue method is described for assaying 10 sulphonamides (SAs) (sulfadiazine, sulfathiazole, sulfapyridine, sulfamerazine, sulfamethazine, sulfamonomethoxine, sulfachlorpyridazine, sulfamethoxazole, sulfaquinoxaline and sulfadimethoxine) in muscle samples. Samples were prepared by homogenizing the tissue, extracting with ethyl acetate and cleaning up with a cation-exchange solid-phase extraction (SPE) column. The detection of analytes was achieved by HPLC-diode array detection (DAD) at 270 nm. The procedure was validated according to the European Union regulation 2002/657/EC determining specificity, decision limit, detection capability, trueness and precision. The results of validation process demonstrate that the method is suitable for application in European Union statutory veterinary drug residue surveillance programmes.

摘要

本文描述了一种简单的多残留方法,用于测定肌肉样品中的10种磺胺类药物(SAs)(磺胺嘧啶、磺胺噻唑、磺胺吡啶、磺胺甲基嘧啶、磺胺二甲嘧啶、磺胺间甲氧嘧啶、磺胺氯哒嗪、磺胺甲恶唑、磺胺喹恶啉和磺胺二甲氧嘧啶)。样品制备方法为将组织匀浆,用乙酸乙酯萃取,并用阳离子交换固相萃取(SPE)柱净化。通过在270nm波长下进行高效液相色谱-二极管阵列检测(HPLC-DAD)来检测分析物。该方法根据欧盟法规2002/657/EC进行了验证,确定了特异性、决策限、检测能力、准确性和精密度。验证过程的结果表明,该方法适用于欧盟法定兽药残留监测计划。

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