QuEChERS-高效液相色谱/串联质谱法同时测定茶油中21种农药残留

Simultaneous determination of 21 kinds of pesticide residues in camellia oil by QuEChERS-high performance liquid chromatography-tandem mass spectrometry

采用QuEChERS结合液相色谱/串联质谱法建立了茶油中21种农药残留的快速分析方法。样品用乙腈均质提取,PSA和C18净化。对色谱、质谱条件和样品前处理进行了优化。在多反应监测(MRM)模式下进行质谱分析,外标法定量。21种农药在5.0~200μg/L范围内具有良好的线性关系,相关系数均大于0.995。在50,100,200μg/kg水平的平均加标回收率为63.1%~128.6%,RSD为1.6%~15%。21种农药的定量限为0.12~6.93μg/kg。方法适用于茶油中21种农药的定量与定性分析。

A method for the simultaneous determination of 21 pesticide residues in camellia oil was developed based on QuEChERS with liquid chromatography-tandem mass spectrometry. The samples were extracted with acetonitrile,then cleaned up by primary secondary amine( PSA) and C18 and analyzed by HPLC-MS/MS with multiple reaction monitoring( MRM) mode. The external standard method was applied to quantify the pesticides.The conditions of chromatography,mass spectrometry and sample pretreatment were optimized. The results showed that the methods for all the 21 pesticides detection had good linearity in certain ranges with the correlation coefficients( r) higher than 0. 995. The recoveries at the levels of 50,100,200 μg/kg in camellia oil ranged from 63. 1% to 128. 6% with the relative standard deviations of 1. 6%-15%. The limits of quantification were0. 12-6. 93 μg/kg. The method is suitable for the determination of the 21 pesticide residues in camellia oil.