QuEChERS-UPLC-MS/MS法同时检测李子中29种农药残留  

Simultaneous determination of 29 pesticides residues in plums byQuEChERS-UPLC-MS/MS

作　　者：朱峰 龙育鋆 宋邦燕 张海艳 廖国会[1] 陈明贵[1] 陈湘燕[1] 秦立新[1] 马玉华[2] ZHU Feng;LONG Yujun;SONG Bangyan;ZHANG Haiyan;LIAO Guohui;CHEN Minggui;CHEN Xiangyan;QIN Lixin;MA Yuhua(Institute of Plant Protection,Guizhou Academy of Agricultural Sciences(Pesticide Risk Monitoring Center of Guizhou Province),Guiyang 550006,China;Guizhou Academy of Agricultural Sciences,Guiyang 550006,China)

机构地区：[1]贵州省农业科学院植物保护研究所(贵州省农药风险监测中心),贵阳550006 [2]贵州省农业科学院,贵阳550006

出　　处：《植物保护》2025年第1期181-189,共9页Plant Protection

基　　金：贵州省优秀青年科技人才计划(黔科合平台人才(YQK[2023]026));贵州省农业科学院博士基金(黔农科博士基金[2024]07号)。

摘　　要：本研究建立了基于QuEChERS前处理方法同时检测李子果实中29种农药残留的超高效液相色谱串联质谱(UPLC-MS/MS)分析方法。样品经1%乙酸乙腈提取,50 mg PSA和30 mg GCB净化后采用UPLC-MS/MS检测,以0.5 mmol/L乙酸铵-0.1%甲酸水为水相,乙腈为有机相进行梯度洗脱,基质外标法定量。29种农药在0.001~0.1 mg/kg范围内呈良好的线性关系,决定系数(R 2)大于0.990;在0.001、0.01、0.1 mg/kg 3个添加水平下,29种农药在李子中的平均添加回收率为70.6%~114.0%,相对标准偏差为1.0%~9.7%(n=5)。29种农药的定量限为0.001 mg/kg。采用所建立的方法对贵州省10批李子样品进行残留检测,结果显示,李子中共检出18种农药,残留量均小于0.1047 mg/kg。该方法的精密度和灵敏度均满足农药残留检测分析要求,能简单、快速地同时检测李子中29种农药残留。This study established a method for the simultaneous analysis of 29 pesticides residues in plums using QuEChERS-based ultra performance liquid chromatography-tandem mass spectrometry(QuEChERS-UPLC-MS/MS).The samples were extracted with acetonitrile containing 1%acetic acid,purified with 50 mg PSA and 30 mg GCB,and detected by UPLC-MS/MS.Gradient elution was performed using 0.5 mmol/L ammonium acetate and 0.1%formic acid in water as the aqueous phase,and acetonitrile as the organic phase,with external matrix standard quantification.The 29 pesticides showed a good linear relationship in the range of 0.001-0.1 mg/kg,with determination coefficients(R 2)greater than 0.990.The average recoveries of the 29 pesticides ranged from 70.6%to 114.0%,with relative standard deviation(RSD)of 1.0%-9.7%(n=5)at spiking levels of 0.001 mg/kg,0.01 mg/kg,and 0.1 mg/kg.The limits of quantification(LOQ)for the 29 pesticides were 0.001 mg/kg.Residue analysis of 10 batches of plum samples from Guizhou province showed that a total of 18 pesticides were detected,with the residue level lower than 0.1047 mg/kg.The precision and sensitivity of this method meet the requirements for pesticide residue detection,providing a simple and rapid approach for simultaneous detection of 29 pesticide residues in plums.

关 键 词：农药 残留 李子 QUECHERS 超高效液相色谱串联质谱 

分 类 号：R155.54[医药卫生—营养与食品卫生学]