QuEChERS-气相色谱/串联质谱法同时测定杨桃中37种农药残留

建立了QuEChERS-气相色谱/三重四极杆串联质谱(GC-MS/MS)测定杨桃中37种农药残留量的方法.样品以1％乙酸乙腈为提取溶剂,采用QuEChERS净化,在质谱多反应监测(MRM)模式下进行定性,基质匹配标准曲线外标法定量.结果表明:在0.01～0.5 mg/L范围内,37种农药的线性关系良好,方法定量限均低于0.01 mg/kg;在低、中、高3个添加水平范围内平均回收率在72.9％～117％之间,相对标准偏差(RSD)≤9.6％.该方法简单、快速、溶剂用量少、灵敏度高,适用于分析杨桃样品中37种农药残留量的检测和确证.

Determination of 37 Pesticide Residues in Carambola Using QuEChERS and Gas Chromatography-Tandem Mass Spectrometry

A QuEChERS-gas chromatography-tandem mass spectrometry method was established for the determination of 37 pesticides residue in carambola.The samples were extracted with acetonitrile containing 1％ acetic acid,and then cleaned up by QuEChERS methods(150 mg PSA,150 mg C18,900 mg anhydrous MgSO4).The target compounds were determined by the mode of multiple reaction monitoring of GC-MS/MS and quantified by the matrix matching standard solution curve.The results showed that the linear range of the method between 0.01 mg/L and 0.5 mg/L was satisfying and the limit of quantitation of all pesticides were lower than 0.01 mg/kg.The average recoveries of all pesticides at the spiked levels from 0.01 to 0.5 mg/kg in carambola matrices were in the range from 72.9 ％ to 117％,and the relative standard deviations were less than 9.6 ％.This method was demonstrated to be simple,quick,accurate,less solvent and sensitive,and could be used for analysis of 37 pesticide residues in carambola.