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

作　　者：黄优生[1] 熊华亮[1] 万偲 罗香[1] 肖庚鹏[1] 

机构地区：[1]江西省分析测试研究所,江西南昌330029 [2]南昌浩然生物医药有限公司,江西南昌330029

出　　处：《食品研究与开发》2014年第21期81-85,共5页Food Research and Development

基　　金：江西省科技支撑计划项目(20132BBG70102);南昌大学食品科学与技术国家重点实验室开放基金项目(SKLF-KF-201412)

摘　　要：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.

关 键 词：高效液相色谱-串联质谱法 QUECHERS 茶叶 农药残留 

分 类 号：TS272.7[农业科学—茶叶生产加工] O657.63[轻工技术与工程—农产品加工及贮藏工程]