QuEChERS结合UPLC-MS/MS法测定海南豇豆中倍硫磷及其Ⅰ型代谢物农药残留  

Determination of fenthion and its typeⅠmetabolites in cowpea in Hainan by UPLC-MS/MS combined with QuEChERS

作　　者：李萍萍[1,2,3] 徐志 张振山[1,2,3] 李春丽[1,2,3] 张群 刘春华[1,2,3] LI Pingping;XU Zhi;HANG Zhenshan;LI Chunli;HANG Qun;LIU Chunhua(Chinese Academy of Tropical Agricultural Sciences,Analysis and Test Center,Haikou 571101,China;Chinese Academy of Tropical Agricultural Sciences,Hainan Provincial Key Laboratory of Quality and Safety for Tropical Fruits and Vegetables,Haikou 571101,China;Chinese Academy of Tropical Agricultural Sciences,Key Laboratory of Quality and Safety Control of Subtropical Fruits and Vegetables,Ministry of Agriculture and Rural Affairs,Haikou 571101,China;Chinese Academy of Tropical Agricultural Sciences,Key Laboratory of Nutritional Quality and Health Benefits of Tropical Agricultural Products of Haikou City,Haikou 571101,China)

机构地区：[1]中国热带农业科学院分析测试中心,海口571101 [2]中国热带农业科学院海南省热带果蔬产品质量安全重点实验室,海口571101 [3]中国热带农业科学院农业农村部亚热带果品蔬菜质量安全控制重点实验室,海口571101 [4]中国热带农业科学院海口市热带农产品营养品质与健康功效重点实验室,海口571101

出　　处：《农药》2024年第8期580-585,591,共7页Agrochemicals

基　　金：海南省科技专项资助(ZDYF2022XDNY232);海南省热带果蔬产品质量安全重点实验室的开放课题资助(KFKT2023004);2023年生态科技特派员项目(WZSKTPXM202214)。

摘　　要：[目的]建立QuEChERS结合UPLC-MS/MS法测定海南豇豆中倍硫磷及其Ⅰ型代谢物的分析方法。[方法]样品经乙腈提取,氯化钠盐析,石墨化炭黑(GCB)和N-丙基乙二胺(PSA)分散固相萃取净化,以Agilent ZORBAX Eclipse Plus C18柱为分离色谱柱,多反应监测(MRM)模式下检测倍硫磷及其Ⅰ型代谢物,定量分析采用溶剂标准曲线法(外标法)。[结果]倍硫磷及其Ⅰ型代谢物在2.0~100.0μg/L质量浓度范围内线性关系良好,相关系数(r)大于0.999;以海南豇豆阴性样品为基质,在2、5、10、50μg/kg 4个质量分数加标水平下,倍硫磷及其Ⅰ型代谢物的平均加标回收率为89.3%~99.3%,相对标准偏差(RSD)为1.2%~7.3%,方法定量限均为2μg/kg。[结论]方法具有简便、高效、准确、廉价等特点,适用于豇豆中倍硫磷及其Ⅰ型代谢物的同时测定。方法的建立可为相关监管部门对豇豆中倍硫磷及其Ⅰ型代谢物农药污染的有效监测提供技术支撑。[Aims]A method was established for analysis of fenthion and its typeⅠmetabolites in cowpea in Hainan by using QuEChERS purification combined with UPLC-MS/MS for determination.[Methods]The samples were extracted by acetonitrile,salted out with sodium chloride,purified with graphitized carbon black(GCB)and N-propylethylenediamine(PSA).The pesticides were separated with Agilent ZORBAX Eclipse Plus C18.Fenthion and its typeⅠmetabolites were analyzed by UPLC-MS/MS with multiple reaction monitoring(MRM)mode.The solvent standard calibration curve was used for quantitative analysis with external standard method.[Results]The results showed that the good linear relationships were obtained for fenthion and its typeⅠmetabolites in the concentration range from 2 to 100μg/L.The correlation coefficients(r)were greater than 0.999.The average spiked recoveries for blank cowpea at 4 levels of 2,5,10,50μg/kg were in the range of 89.3%to 99.3%,with relative standard deviations(RSD)in the range of 1.2%to 7.3%.The LOQs of the method were all 2.0μg/kg.[Conclusions]The method is simple and cheap with high efficiency and accuracy,which is suitable to analyze fenthion and its typeⅠmetabolites in cowpea in Hainan.This method will supply an effective technical support to supervise fenthion and its typeⅠmetabolites in cowpea.

关 键 词：倍硫磷 Ⅰ型代谢物 QUECHERS UPLC-MS/MS 豇豆 

分 类 号：TQ450.2[化学工程—农药化工]