农药2024,Vol.63Issue(8) :580-585,591.DOI:10.16820/j.nyzz.2024.0807

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 type Ⅰ metabolites in cowpea in Hainan by UPLC-MS/MS combined with QuEChERS

李萍萍 徐志 张振山 李春丽 张群 刘春华
农药2024,Vol.63Issue(8) :580-585,591.DOI:10.16820/j.nyzz.2024.0807

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 type Ⅰ metabolites in cowpea in Hainan by UPLC-MS/MS combined with QuEChERS

李萍萍 1徐志 1张振山 1李春丽 1张群 2刘春华1
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作者信息

  • 1. 中国热带农业科学院分析测试中心,海口 571101;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;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
  • 2. 中国热带农业科学院分析测试中心,海口 571101;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;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;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
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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 PlusC18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2.0~100.0 μg/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/kg4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2 μg/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.

Abstract

[Aims]A method was established for analysis of fenthion and its type Ⅰ metabolites 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 type Ⅰ metabolites 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 type Ⅰ metabolites in the concentration range from 2 to 100 pg/L.The correlation coefficients(r)were greater than 0.999.The average spiked recoveries for blank cowpea at 4 levels of 2,5,10,50 pg/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 2.0 pg/kg.[Conclusions]The method is simple and cheap with high efficiency and accuracy,which is suitable to analyze fenthion and its type Ⅰmetabolites in cowpea in Hainan.This method will supply an effective technical support to supervise fenthion and its type Ⅰ metabolites in cowpea.

关键词

倍硫磷/Ⅰ型代谢物/QuEChERS/UPLC-MS/MS/豇豆

Key words

fenthion/type Ⅰ metabolite/QuEChERS/UPLC-MS/MS/cowpea

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基金项目

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开放课题资助(KFKT2023004)

2023年生态科技特派员项目(WZSKTPXM202214)

出版年

2024
农药
沈阳化工研究院有限公司

农药

CSTPCDCSCD北大核心
影响因子:0.665
ISSN:1006-0413
参考文献量29
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