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高效液相色谱-飞行时间质谱法同时测定猪肉中 141 种兽药及其代谢物

Untargeted multi-residue method for the simultaneous determination of 141 veterinary drugs and their metabolites in pork by high-performance liquid chromatography time-of-flight mass spectrometry.

机构信息

Shanghai Institute for Food and Drug Control, Shanghai 201203, China.

Shanghai Institute for Food and Drug Control, Shanghai 201203, China.

出版信息

J Chromatogr A. 2020 Dec 20;1634:461671. doi: 10.1016/j.chroma.2020.461671. Epub 2020 Nov 2.

Abstract

A rapid, simple and generic analytical method has been developed for the analysis of veterinary drugs in pork by a quadrupole time-of-flight mass spectrometry (Q-TOF MS). This method allows for the simultaneous identification, screening and quantitation of 141 veterinary drug residues and metabolites from eighteen different classes. After extraction with acetonitrile/water and clean-up with C cartridges, the samples were analyzed by HPLC-Q-TOF MS. Validation of this method consisted of confirmation of identity, selectivity, linearity, limit of detection (LOD), lowest limit of quantification (LLOQ), matrix effect, recovery, precision and applicability of the method. Identification of the analytes was based on accurate mass measurements. The characteristic fragments were obtained by collisional experiments for a more reliable identification. The procedure was then applied to real pork samples. Sulfamethazine was detected in one sample and its metabolites were successfully found in one single run. This approach proved to be satisfactory for routine analysis.

摘要

一种快速、简单和通用的分析方法已经被开发出来,用于通过四极杆飞行时间质谱(Q-TOF MS)分析猪肉中的兽药。该方法允许同时鉴定、筛选和定量来自十八个不同类别的 141 种兽药残留和代谢物。在乙腈/水提取和 C 柱净化后,样品通过 HPLC-Q-TOF MS 进行分析。该方法的验证包括确证、选择性、线性、检测限(LOD)、最低定量限(LLOQ)、基质效应、回收率、精密度和方法适用性。分析物的鉴定基于准确的质量测量。通过碰撞实验获得特征碎片,以进行更可靠的鉴定。然后将该程序应用于实际的猪肉样品。在一个样品中检测到磺胺甲噁唑,并且在单次运行中成功地发现了其代谢物。该方法被证明可用于常规分析。

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