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采用QuEChERS萃取法结合液相色谱-质谱检测(LC-MS)测定牛肉中农药多残留的方法。

Multiresidue method for detection of pesticides in beef meat using liquid chromatography coupled to mass spectrometry detection (LC-MS) after QuEChERS extraction.

作者信息

Oliveira Fabiano Aurélio da Silva, Pereira Elba Nathália Corrêa, Gobbi Jennifer Mattedi, Soto-Blanco Benito, Melo Marília Martins

机构信息

a Laboratório de Pesticidas , Laboratório Nacional Agropecuário em Minas Gerais (LANAGRO-MG) , Pedro Leopoldo , Brazil.

b Laboratório de Toxicologia, Departamento de Clínica e Cirurgia Veterinárias, Escola de Veterinária , Universidade Federal de Minas Gerais (UFMG) , Belo Horizonte , Brazil.

出版信息

Food Addit Contam Part A Chem Anal Control Expo Risk Assess. 2018 Jan;35(1):94-109. doi: 10.1080/19440049.2017.1395519. Epub 2017 Nov 3.

Abstract

Beef meat is an important food that can be contaminated by pesticides. This study aimed to optimize a multiresidue method for identification and quantification of pesticides in beef meat by liquid chromatography coupled to mass spectrometry detection (LC-MS). The extraction and clean-up procedures were adapted from the QuECHERS method. From the 188 analytes tested, the method was validated as qualitative method for 19 compounds and as quantitative method for 152 compounds. The results were satisfactory, yielding coefficients of variation of less than 20% and recoveries ranging from 70% to 120% and expanded uncertainty of less than 50%. The quantification limit was typically 10 µg kg (but 25 µg kg for 12 of the compounds) and the detection limit was 5.0 µg kg. Thirty-two real samples of commercialized beef meat were analyzed without any residual pesticide being found. Thus, the results showed that the multiresidue method for detecting 171 pesticides, using adapted QuECHERS for extraction and LC-MS for detection, is suitable for analyzing beef meat.

摘要

牛肉是一种重要的食物,但可能会受到农药污染。本研究旨在优化一种多残留方法,用于通过液相色谱-质谱检测(LC-MS)鉴定和定量牛肉中的农药。提取和净化程序改编自QuECHERS方法。在测试的188种分析物中,该方法被验证为19种化合物的定性方法和152种化合物的定量方法。结果令人满意,变异系数小于20%,回收率在70%至120%之间,扩展不确定度小于50%。定量限通常为10 μg/kg(但其中12种化合物为25 μg/kg),检测限为5.0 μg/kg。对32个商业化牛肉的实际样品进行分析,未发现任何残留农药。因此,结果表明,采用改良的QuECHERS进行提取、LC-MS进行检测的171种农药多残留检测方法适用于牛肉分析。

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