液相色谱串联质谱法同时检测茶叶中23种农药残留

Simultaneous Determination of 23 Pesticides in Tea by High Performance Liquid Chromatography-Tandem Mass Spectrometry

建立了Qu ECh ERS样品前处理-液相色谱串联质谱法同时检测茶叶中23种农药残留的分析方法。样品经Qu ECh ERS方法进行前处理,采用液相色谱分离、多反应监测(MRM)模式进行检测,基质曲线外标法定量。23种农药的定量限(LOQ)为0.09μg/kg^10μg/kg,多菌灵和杀螟硫磷线性范围为5.0 ng/m L^80 ng/m L,其他农药线性范围为2.0 ng/m L^40 ng/m L,线性相关系数均大于0.992 5。多菌灵和杀螟硫磷在20、40、80μg/kg 3个添加水平、其他21种农药在10、20、40μg/kg 3个添加水平范围内的回收率为67%~115%,相对标准偏差(RSD)为1.3%~14.8%。该方法操作简便、灵敏度高,适合于茶叶中23种农药残留的定量及确证分析。

An analytical method was developed for the simultaneous determination of 23 pesticides in Tea based on QuEChERS extraction followed by high performance liquid chromatography-tandem mass spectrometry （HPLC-MS/MS）. The samples were extracted using the QuEChERS method. The target analytes were separated on a RP-HPLC column and analyzed in multiple reaction monitoring （MRM） mode. Sample matrix-matched calibration was used to determine the residue contents by external standard. The results showed that the calibration curves were linear in the range of 5.0 ng/mL-80 ng/mL for carbendazim and fenitrothion, and 2.0 ng/mL-40 ng/mL for other pesticides, with correlation coefficients larger than 0.992 5. The limits of quantitation （LOQ） were of 23 pesticides 0.09μg/kg-10μg/kg. The recoveries of carbendazim and fenitrothion with the concentration levels at 20,40,80μg/kg and other pesticides with the concentration levels at 10,20,40μg/kg were range of 67%-115%, which relative standard deviations （RSD） were 1.3%-14.8%. This method was simple, effective and sensitive for qualification analysis of 23 pesticides in Tea.