UHPLC-MS/MS和GC-MS/MS测定甜菜中523种农药及代谢物的残留量  

Simultaneous determination of 523 pesticides and metabolites in beet using UHPLC-MS/MS and GC-MS/MS

作　　者：原海越 史小萌 李备 王雯雯[3] 刘潇威 贺泽英 YUAN Haiyue;SHI Xiaomeng;LI Bei;WANG Wenwen;LIU Xiaowei;HE Zeying(Hainan Institute for Food Control,Key Laboratory of Tropical Fruits and Vegetables Quality and Safety for State Market Regulation,Haikou 570311,China;Agro-Environmental Protection Institute,Ministry of Agriculture and Rural Affairs,Tianjin 300191,China;Agilent Technologies Limited,Beijing 100102,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),海口570311 [2]农业农村部环境保护科研监测所,天津300191 [3]安捷伦科技有限公司,北京100102

出　　处：《农业环境科学学报》2023年第7期1666-1674,共9页Journal of Agro-Environment Science

基　　金：国家市场监管重点实验室(热带果蔬质量与安全)基础应用研究课题(KF-2022009)。

摘　　要：建立同时检测甜菜中523种农药及代谢物的QuEChERS提取结合超高效液相色谱串联质谱法和气相色谱串联质谱分析方法。采用QuEChERS前处理方法提取,MgSO4和乙二胺-N-丙基硅烷化硅胶(PSA)净化,采用UHPLC-MS/MS和GC-MS/MS检测。PSA的用量会影响40种农药的回收率,用量为0或5 mg·mL^(-1)时,回收率在60%~120%之间。523种农药在2~200μg·kg^(-1)添加浓度水平回收率在65.1%~116.4%之间,RSD值小于24.1%。方法定量为2μg·kg^(-1)或5μg·kg^(-1),线性相关系数均大于0.99,采用基质标准曲线定量分析。针对142种农药适用于两种仪器的检测结果无明显差异。实际样品检测出的农药残留物浓度均低于我国规定相应的最大残留限量,但根据欧盟标准的规定,部分样品中毒死蜱、溴氰菊酯和氰戊菊酯存在超标现象。该方法样品前处理简单快速,方法的准确度、精密度和灵敏度均满足农药残留在农作物中检测分析要求,适用于523种农药及代谢物在甜菜中的多残留检测。This study aimed to develop a multiresidue method for simultaneous detection of 523 pesticides and metabolites in beet using QuEChERS extraction combined with UHPLC-MS/MS and GC-MS/MS.The samples were extracted by the QuEChERS pretreatment method,purified by d-SPE with MgSO4 and PSA,and determined using UHPLC-MS/MS and GC-MS/MS.The dosage of PSA affected the recoveries of 40 pesticides,which were between 60%and 120%when PSA was used 0 mg·mL^(-1) or 5 mg·mL^(-1).The recoveries of 523 pesticides and metabolites at 2-200μg·kg^(-1) ranged from 65.1%to 116.4%with RSDs<24.1%.The limits of quantification(LOQs)were 2μg·kg^(-1) or 5μg·kg^(-1).The linear correlation coefficients were>0.99.There was no significant difference in the detection results of the two instruments for 142 pesticides.The concentrations of pesticide residues detected in real samples were all below the corresponding national maximum residue limits(MRL).However,according to the European Union standard,residual concentrations of chlorpyrifos,deltamethrin,and fenvalerate exceeded the MRLs in some samples.This analytical method is simple and rapid,and its accuracy,precision,and sensitivity all meet the requirements of pesticide residues analysis.Therefore,this method can be applied in analysis of 523 pesticides and metabolites in beet.

关 键 词：甜菜 农药多残留分析 超高效液相色谱串联质谱 气相色谱串联质谱 

分 类 号：S481.8[农业科学—农药学]