注射器内分散固相萃取-超高效液相色谱-串联质谱法快速测定茶叶中24种农药残留  

Rapid Determination of 24 Pesticide Residues in Tea by in-Syringe Dispersive Solid Phase Extraction-Ultra High Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：马佳丽 王晨[1,3,4] 陈红平 柴云峰[1,3,4] 诸力 刘新[1,3,4] MA Jiali;WANG Chen;CHEN Hongping;CHAI Yunfeng;ZHU Li;LIU Xin(Tea Research Institute,Chinese Academy of Agriculture Sciences,Hangzhou 310008,China;Graduate School,Chinese Academy of Agriculture Sciences,Beijing 100081,China;Key Laboratory of Tea Quality and Safety Control,Ministry of Agriculture and Rural Affairs,Hangzhou 310008,China;Laboratory of Quality and Safety Risk Assessment for Tea Products(Hangzhou),Ministry of Agriculture and Rural Affairs,Hangzhou 310008,China)

机构地区：[1]中国农业科学院茶叶研究所,浙江杭州310008 [2]中国农业科学院研究生院,北京100081 [3]农业农村部茶叶质量安全控制重点实验室,浙江杭州310008 [4]农业农村部茶叶产品质量安全风险评估实验室(杭州),浙江杭州310008

出　　处：《茶叶科学》2021年第5期717-730,共14页Journal of Tea Science

基　　金：财政部和农业农村部:国家现代农业产业技术体系(CARS-19);中国农业科学院创新团队(CAAS-ASTIP-2014-TRICAAS-06);国家农产品质量安全风险评估项目(GJFP2020001)。

摘　　要：基于茶叶基质特点,开发了注射器内分散固相萃取快速前处理技术,建立了茶叶中24种农药残留超高效液相色谱-串联质谱检测方法。茶叶样品经乙腈提取,无水MgSO4盐析,在设计的注射器装置内以N-丙基乙二胺键合硅胶和石墨化炭黑作为分散吸附剂进行净化,超高效液相色谱-串联质谱法进行检测。在3个添加水平(0.01、0.05、0.5 mg·kg^(-1))下,红茶和绿茶中24种农药的平均回收率为61.7%~98.8%,相对标准偏差为0.4%~5.5%,准确度和精密度良好。24种农药的红茶和绿茶基质标准工作液线性关系良好,相关系数(R2)均大于0.995,检出限(LOD)和定量限(LOQ)分别为0.05~5.36μg·kg^(-1)和0.18~17.86μg·kg^(-1),该方法具有良好的灵敏度。本方法具有简便快捷、所需仪器少、省时等优势,适用于茶叶中多农药残留的定量检测。Based on the characteristics of tea matrix,a rapid pretreatment technology of in-syringe dispersive solid phase extraction(dSPE)was developed,and an analytical method based on ultra high performance liquid chromatography-tandem mass spectrometry was established for the detection of 24 pesticide residues in tea.Tea samples were extracted using acetonitrile,salted-out with MgSO4,purified with primary secondary amine and graphitized carbon black as dispersive adsorbents in designed syringe devices,and detected by UPLC-MS/MS.Recoveries of 24 pesticides in black and green teas were 61.7%-98.8%at three spiked levels(0.01 mg·kg^(-1),0.05 mg·kg^(-1) and 0.5 mg·kg^(-1)),which indicated high accuracy with the relative standard deviations of 0.4%-5.5%.The calibration curves of 24 pesticides in black and green teas showed good linearity with correlation coefficients(R2)higher than 0.995.The limits of detection(LOD)and the limits of quantitation(LOQ)were 0.05-5.36μg·kg^(-1) and 0.18-17.86μg·kg^(-1),respectively,which show high sensitivity of this method.Being simple,fast,less instrument required and time-saving,this method is suitable for quantification of multiple pesticide residues in tea.

关 键 词：茶叶 超高效液相色谱-串联质谱 农药残留 注射器内分散固相萃取 

分 类 号：S571.1[农业科学—茶叶生产加工] TS207.3[农业科学—作物学]