蔬果中三氯杀螨醇和拟除虫菊酯残留量的QuEChERS-气相色谱-串联质谱测定法

目的探索并建立测定蔬果中三氯杀螨醇和8种拟除虫菊酯残留量的QuEChERS-气相色谱-串联质谱(GC-MS/MS)测定法。方法2019年9-10月,对蔬果用乙腈超声提取15 min,经旋涡振荡,QuEChERS净化后进入GC-MS/MS分析。样品经DB-17MS(30 m×0.25μm,0.250 mm)分离,采用多反应监测模式(MRM)进行检测。以保留时间及特征离子对丰度比定性,定量离子峰面积定量。结果本试验条件下方法线性关系良好(r>0.9981),方法检出限为0.07~9.11μg/kg。平均回收率为77.2%~100.2%,相对标准偏差(RSD)为1.4%~9.4%。结论本方法操作简便快速、结果准确、精密度高,适用于同时检测蔬果中三氯杀螨醇和8种拟除虫菊酯残留量。

Determination of dicofol and pyrethroid residues in fruits and vegetables by QuEChERS-gas chromatography-tandem mass spectrometry

Objective To explore and establish a method for the determination of dicofol and eight pyrethroid residues in fruits and vegetables by QuEChERS-gas chromatography-tandem mass spectrometry.Methods From September to October 2019,fruits and vegetables were extracted with acetonitrile for 15 minutes,treated by vortex oscillation,urified by QuEChERS,and analyzed by GC-MS/MS.The samples were separated by DB-17 MS(30 m×0.25μm,0.250 mm)and detected under multiple reaction monitoring mode(MRM).Qualitative analysis was performed by retention time and characteristi c ion for abundance ratio,and quantitative analysis was performed by quantitative ion peak area.Results Under the experimental conditions,the linear relationship of the method was good(r>0.9981),and the detection limit of the method was 0.07-9.11μg/kg.The average recoveries were 77.2%-100.2%,and relative standard deviations(RSD)were 1.4%-9.4%.Conclusion The method is simple,rapid,accurate and precise.It is suitable for simultaneous determination of dicofol trichloride and eight pyrethroid residues in fruits and vegetables.