全自动固相萃取-超高效液相色谱串联质谱法测定茶叶中22种杀菌剂  

Simultaneous determination of 22 fungicide residues in tea using automatic solid phase extraction coupled with ultra-performance liquid chromatography-tandem mass spectrometry

作　　者：章剑[1] 李四生[1] 李建伟[1] 周浩丰[1] 李昌安[1] ZHANG Jian;LI Si-sheng;LI Jian-wei;ZHOU Hao-feng;LI Chang-an(Hefei Center for Disease Control and Prevention,Hefei,Anhui 230061,China)

机构地区：[1]合肥市疾病预防控制中心,安徽230061

出　　处：《现代预防医学》2021年第9期1672-1676,1686,共6页Modern Preventive Medicine

基　　金：合肥市卫生健康委应用医学研究重点项目(Hwk2020zd0018)。

摘　　要：目的建立茶叶中22种杀菌剂的全自动固相萃取-超高效液相色谱串联质谱联用(UPLC-MS/MS)测定法。方法样品用乙腈提取,经过TPT固相萃取柱净化,HSS T3色谱柱分离,串联质谱检测,空白基质匹配标准溶液外标法定量。结果22种杀菌剂在0.2~100μg/L范围内线性相关系数良好(r>0.999),检出限为0.10~1.0μg/kg,定量限为1.0~3.0μg/kg,回收率在55.3%~115.6%之间,相对标准偏差(RSD)在4.13%~15.44%之间。结论方法灵敏、准确、重现性好,适用于茶叶样品中多种杀菌剂残留量的快速筛查与日常检测。Objective To establish a method for simultaneous determination 22 fungicide residues in tea by automatic solid phase extraction coupled with ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)Methods The fungicides in tea were extracted with acetonitrile and cleaned up with TPT SPE cartridge and then separated on an HSS T3 chromatographic column,finally detected by tandem mass spectrometer.The quantifications were based on matrix-matched external standard curves method.Results The method showed good linearities in the range of 0.20-100μg/L,with the correlation coefficients(r)of above 0.999.The limits of detection and limits of quantification were 0.10-1.0μg/kg and 1.0-3.0μg/kg,respectively.The average recoveries ranged from 55.3%to 115.6%,and the relative standard deviations(RSDs)were 4.13%-15.44%.Conclusion The proposed method is sensitive,accurate,and reproducible,and it is suitable for rapid screening and daily detection of fungicide residues in tea samples.

关 键 词：超高效液相色谱-串联质谱法 全自动固相萃取 杀菌剂 茶叶 

分 类 号：R115[医药卫生—公共卫生与预防医学]