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一种双验证方法,用于检测牛肝中延长浓度范围内的驱虫药残留。

A dual validation approach to detect anthelmintic residues in bovine liver over an extended concentration range.

机构信息

Teagasc, Ashtown Food Research Centre, Ashtown, Dublin 15, Ireland.

出版信息

Talanta. 2010 Nov 15;83(1):14-24. doi: 10.1016/j.talanta.2010.08.025. Epub 2010 Aug 21.

DOI:10.1016/j.talanta.2010.08.025
PMID:21035637
Abstract

This paper describes a method for the detection and quantification of 38 residues of the most widely used anthelmintics (including 26 veterinary drugs belonging to the benzimidazole, macrocyclic lactone and flukicide classes) in bovine liver using two different protocols for MRL and non-MRL levels. A dual validation approach was adopted to reliably quantify anthelmintic residues over an extended concentration range (1-3000 μg kg(-1)). Sample extraction and purification was carried out using a modified QuEChERS method. A concentration step was included when analysing in the low μg kg(-1) range. Rapid analysis was carried out by ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS), which was capable of detecting residues to <2 μg kg(-1). The method has been single-laboratory validated according to the 2002/657/EC guidelines and met acceptability criteria in all but a few cases. The inclusion of 19 internal standards, including 14 isotopically labelled internal standards, improved accuracy, precision, decision limit (CCα) and detection capability (CCβ).

摘要

本文描述了一种使用两种不同的 MRL 和非 MRL 水平方案,检测和定量分析牛肝中 38 种最广泛使用的驱虫药(包括属于苯并咪唑类、大环内酯类和杀吸虫类的 26 种兽药)残留的方法。采用双重验证方法,可在较宽的浓度范围内(1-3000μgkg(-1))可靠地定量分析驱虫药残留。采用改良的 QuEChERS 方法进行样品提取和净化。当分析低μgkg(-1)范围时,包括浓缩步骤。采用超高效液相色谱-串联质谱法(UHPLC-MS/MS)进行快速分析,能够检测到<2μgkg(-1)的残留。该方法已按照 2002/657/EC 准则进行了单实验室验证,但在少数情况下不符合可接受标准。包括 19 种内标物,包括 14 种同位素标记的内标物,提高了准确度、精密度、决策限(CCα)和检测能力(CCβ)。

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