自动QuEChERS结合液相色谱-质谱联用法测定饲料中172种农药及其代谢物残留量  

Automatic QuEChERS combined with liquid chromatography-mass spectrometry for determination of 172 pesticides and their metabolite residues in feed

作　　者：张嘉楠 武侠均 周伟帅 侯铭源 刘怡菲 张洋 ZHANG Jianan;WU Xiajun;ZHOU Weishuai;HOU Mingyuan;LIU Yifei;ZHANG Yang

机构地区：[1]秦皇岛市农产品质量安全检验监测中心,河北秦皇岛066000 [2]河北省兽药饲料工作总站,河北石家庄050035 [3]秦皇岛益尔动物科技有限公司,河北秦皇岛066000

出　　处：《饲料研究》2025年第4期124-132,共9页Feed Research

基　　金：河北省三期现代农业产业技术体系肉牛创新团队兽药残留减量控制综合试验推广站建设项目(项目编号:HBCT2024240408、HBCT2024250406);河北省重点研发计划项目(项目编号:22327304D)。

摘　　要：试验旨在探究自动QuEChERS结合液相色谱-质谱联用法(LC-MS/MS)测定饲料中172种农药及其代谢物残留量。饲料样品粉碎后加水浸泡,经乙腈提取、N-丙基乙二胺(PSA)和C18净化,通过自动QuEChERS样品制备系统进行一站式的前处理,在电喷雾离子源正负离子模式下,采用基质匹配外标法定量。结果显示,172种农药及其代谢物在0.002~0.100 mg/L的范围内相关系数(r)均>0.99,定量限达到0.01 mg/kg,在0.01、0.02、0.10 mg/kg的加标水平下的平均回收率(相对标准偏差)分别为63.3%~104.0%(1.02%~12.30%)、66.5%~104.0%(0.34%~10.20%)、80.1%~108.0%(0.37%~12.30%)。研究表明,采用自动QuEChERS技术对饲料样品进行提取和净化,外标基质匹配标准曲线法定量,建立检测饲料中172种农药及其代谢物残留量的液相色谱-质谱联用检测方法,具有操作简便、快速、自动化程度高的特点,适用于饲料中多种农药残留的快速分析。The experiment aimed to explore the determination of residues of 172 pesticides and their metabolites in feed using automatic QuEChERS combined with liquid chromatography-tandem mass spectrometry(LC-MS/MS).Feed samples were crushed and soaked in water,then extracted with acetonitrile and purified with N-propyl ethylene diamine(PSA)and C18.The one-stop pretreatment was carried out by the automatic QuEChERS sample preparation system.Quantification was performed using the matrix-matched external standard method under the positive and negative ion modes of electrospray ionization.The results showed that the correlation coefficients(r)of the 172 pesticides and their metabolites were all>0.99 in the range of 0.002~0.100 mg/L,and the limit of quantification reached 0.01 mg/kg.The average recoveries(relative standard deviations)at the spiked levels of 0.01,0.02 and 0.10 mg/kg were 63.3%~104.0%(1.02%~12.30%),66.5%~104.0%(0.34%~10.20%)and 80.1%~108.0%(0.37%~12.30%),respectively.The study indicates that the LC-MS/MS method for detecting the residues of 172 pesticides and their metabolites in feed,which uses automatic QuEChERS technology for extraction and purification and the external standard matrix-matched standard curve method for quantification,has the characteristics of simple operation,rapidity,and high degree of automation,and is suitable for the rapid analysis of multiple pesticide residues in feed.

关 键 词：饲料 农药多残留 自动QuEChERS 液相色谱-质谱联用法 

分 类 号：S816.17[农业科学—饲料科学]