UPLC-MS/MS法同时检测番茄与黄瓜中的24种杀虫剂

Simultaneous Determination of 24 Insecticides in Cucumber and Tomato by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

建立了超高效液相色谱-串联质谱检测番茄和黄瓜中24种杀虫剂残留的分析方法。样品用乙腈提取,经QuEChERS方法净化,高速离心,过滤膜后以超高效液相色谱-串联质谱(UPLC-MS/MS)检测。结果表明:在0.1~50μg/L质量浓度范围内,24种杀虫剂线性良好,相关系数(r2)大于0.99;在0.002、0.01、0.1、1.0 mg/kg 4个加标水平下,24种杀虫剂在番茄和黄瓜中的平均回收率为70.3%~110%,相对标准偏差(RSD)小于15%;方法的定量下限(LOQ)为0.05~5μg/kg,检出限(LOD)为0.01~1.82μg/kg。方法的定量下限和检出限均符合检测要求。该方法具有高灵敏度、高准确度和高效率的优点,适用于番茄和黄瓜中24种杀虫剂的同时检测。

An analytical method was developed for the simultaneous determination of 24 insecticide residues in cucumber and tomato by ultra performance liquid chromatography-tandem mass spectrometry（UPLC-MS/MS）.The samples were firstly extracted with acetonitrile,then purified by QuEChERS method and centrifuged at a high speed,finally filtered with a 0.22 μm membrane filter before UPLC-MS/MS determination.The results indicated that there were good linear relationships for 24 kinds of insecticides in the concentration range of 0.1-50 μg/L with the linear correlation coefficients（r2） more than 0.99.The average recoveries for the target compounds at four spiked levels of 0.002,0.01,0.1,1.0 mg/kg were in the range of 70.3%-110% with the relative standard deviations less than 15%.The limits of quantitation（LOQs） and the limits of detection（LODs） of the method were in the ranges of 0.05-5 μg/kg and 0.01-1.82 μg/kg,respectively,which could meet the detection requirements.This method is suitable for the simultaneous detection on 24 insecticides in cucumber and tomato with the advantages of high sensitivity,accuracy and efficiency.