快速滤过型净化结合超高效液相色谱-串联质谱法同时测定鸡蛋中38种杀菌剂类农药残留  

Simultaneous Detection of 38 Fungicides Residues in Eggs by Multi-Plug Filtration Cleanup with Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：万娜 潘永波 梁晓涵 王丹 陈秋宇 邹冬梅[2] WAN Na;PAN Yongbo;LIANG Xiaohan;WANG Dan;CHEN Qiuyu;ZOU Dongmei(Hainan Institute for Food Control,Key Laboratory of Tropical Fruits and Vegetables Quality and Safety for State Market Regulation,Haikou 570314,China;Hainan Provincial Key Laboratory of Quality and Safety for Tropical Fruits and Vegetables Analysis and Testing Center,Chinese Academy of Tropical Agricultural Sciences,Haikou 571101,China)

机构地区：[1]海南省食品检验检测中心国家市场监管重点实验室(热带果蔬质量与安全),海南海口570314 [2]中国热带农业科学院分析测试中心海南省热带果蔬产品质量安全重点实验室,海南海口571101

出　　处：《食品工业科技》2023年第17期324-333,共10页Science and Technology of Food Industry

基　　金：国家市场监管重点实验室(热带果蔬质量与安全)自主研究课题(No.ZZ-2022006);国家市场监管重点实验室(热带果蔬质量与安全)自主研究课题(No.ZZ-2023024);农业农村部农业国际交流与合作项目(No.SYZ2017-06)。

摘　　要：采用快速滤过型净化法(m-PFC)结合超高效液相色谱-串联质谱(UPLC-MS/MS),建立了鸡蛋中38种杀菌剂类农药残留同时检测的分析方法。样品加水混匀后经过乙酸乙腈提取,Qu ECh ERS盐包分层,取上层提取液经m-PFC柱净化,液相色谱-质谱联用测定,采用多反应监测模式(MRM)进行分析,基质外标法定量。结果表明:该方法的检出限(LOD)为0.01~0.2μg/kg,定量限(LOQ)为0.02~0.7μg/kg,其定量限满足国家标准GB2763-2021中规定的最大残留限量要求,38种杀菌剂类农药在0.001~0.50μg/m L浓度范围线性关系良好,决定系数(R2)均高于0.9912。在10、50、200μg/kg三种浓度水平下添加回收率在72.7%~113.5%之间,相对标准偏差为0.40%~10%(n=6)。该方法快速、准确,为监测鸡蛋中农药残留提供了检测方法,也为鸡蛋中农药最大残留限量的制定提供了参考。This research demonstrated a method for simultaneous determination of 38 fungicides residues in eggs based on multi-plug filtration cleanup(m-PFC)method combined with ultra-performance liquid chromatoid-tandem mass spectrometry(UPLC-MS/MS).After mixing with water,samples were extracted with acetonitrile(acetic acid).QuEChERS salt packs were used to separate the organic and aqueous phases of the sample.The upper fraction was purified on an m-PFC column before analysis by LC-MS/MS,the samples were then analyzed using multi-reaction monitoring(MRM)method and quantified using the matrix-matched external standard method.The results showed a limit of detection(LOD)of 0.01~0.2μg/kg and the limit of quantification(LOQ)of 0.02~0.7μg/kg,meeting the maximum residue limit requirements specified in the national standard GB 2763-2021.The correlation coefficient(R2)of 38 fungicides was higher than 0.9912 in the concentration range of 0.001~0.50μg/mL.The recoveries at three concentration levels(10,50 and 200μg/kg)were in the range of 72.7%~113.5%,with the relative standard deviation(RSD,n=6)of 0.40%~10%.Thus,the method is proved to be rapid and accurate for monitoring pesticide residues in eggs,which also provides a reference for the formulation of maximum residue limits of pesticides in eggs.

关 键 词：鸡蛋 快速滤过型净化 超高效液相色谱-串联质谱 杀菌剂类农药 

分 类 号：O657.63[理学—分析化学] TS253.7[理学—化学]