QuEChERS-超高效液相色谱-串联质谱法同时检测草莓中4种农药残留量  

Simultaneous Determination of 4 Pesticide Residues in Strawberry by QuEChERS and Ultra Performance Liquid Chromatography-Tandem Mass

作　　者：杜鑫 彭海燕 覃明丽 陈绍辉 易珊珊 蒋金芳 Du Xin;Peng Haiyan;Qin Mingli;Chen Shaohui;Yi Shanshan;Jiang Jinfang(Nanchong Monitoring and Test Center for Agricultural Products Quality,Nanchong Sichuan 637000,China)

机构地区：[1]南充农产品质量监测检验中心,四川南充637000

出　　处：《农药科学与管理》2022年第5期30-37,共8页Pesticide Science and Administration

摘　　要：应用QuEChERS结合超高效液相色谱—串联质谱法(UPLC-MS/MS)建立了同时检测草莓中噻螨酮、唑螨酯、噻嗪酮、阿维菌素等4种农药残留量的方法。样品经乙腈均质提取,N-丙基乙二胺(PSA)分散剂净化,用Waters XBridge C_(18)液相色谱柱分离,以甲醇、水(0.1%甲酸-5mmol/L乙酸铵)和乙腈为流动相进行梯度洗脱,采用电喷雾正离子模式(ESI^(+))和选择多反应监测模式(MRM)进行测定,基质匹配标准溶液外标法定量。结果表明:在0.005~0.20mg/L浓度范围内,4种农药均具有良好的线性相关性(r>0.9986),检出限为1.2~2.0μg/kg。空白样品加标量为0.010、0.050和0.10mg/kg 3个水平时,平均添加回收率为85.2%~108.2%,相对标准偏差(RSD)为2.8%~5.9%(n=6)。本方法简单、快速、重现性好,具有良好的抗基质干扰能力,适用于草莓样品中该4种农药残留的快速检测。A simple and rapid method by QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)was established for simultaneous determination of fexythiazox,fenpyroximate,buprofezin and abamectin in strawberry.The samples were firstly homogenized and extracted with acetonitrile,then cleaned up with dispersive method on primary-secondary amine(PSA)and separated by Waters XBridge C_(18) column using gradient elution with a mixture of water(0.1%formic acid-5 mmol/L ammonium acetate),acetonitrile and methanol as mobile phases.The residue of the tested pesticides was lastly quantified by matrix matching external standard method using UPLC-MS/MS in the multiple reactions monitoring(MRM)mode with positive electrospray ionization(ESI^(+)).The linear range of the method was in the range of 0.005~0.20 mg/L for all the analytes with correlation coefficients greater than 0.9986,and the detection quantitation limits were 1.2~2.0μg/kg.The average recoveries of blank samples spiked at 0.010,0.050,0.10 mg/kg were ranged from 85.2% to 108.2%,with the relative standard deviation(RSD)values of 2.8%~5.9%(n=6).This method proved to be accurate,reliable and good reproducibility,which can be used for simultaneous determination of 4 pesticide residues in strawberry.

关 键 词：QUECHERS 超高效液相色谱-串联质谱法 PSA 农药残留 草莓 

分 类 号：S482[农业科学—农药学] S481.8[农业科学—植物保护]