分析测试学报2023，Vol.42Issue(12)：1537-1546,10.DOI:10.19969/j.fxcsxb.23080405
基于超高效液相色谱-四极杆/静电场轨道阱高分辨质谱筛查茶叶中166种农药残留方法研究
Screening of 166 Pesticide Residues in Tea Based on Ultra High Performance Liquid Chromatography-Quadrupole/Electrostatic Field Orbitrap High Resolution Mass Spectrometry
摘要
Abstract
An ultra high performance liquid chromatography-quadrupole/electrostatic field orbitrap high resolution mass spectrometric(UHPLC-Q-Exactive Orbitrap MS)method was established for the simultaneous determination of 166 pesticide residues in tea.The samples were pretreated by modified QuEChERS technology.In Full MS mode,the accurate molecular ion was employed as quantitative ion.The characteristic fragment ions and secondary mass spectrometry informations were used for qualitative analysis,and the external standard method was adopted for quantification.The accuracy and precision of the method were verified by taking green tea and black tea as sample matrices.Fif-teen pesticides in green tea had good linear relationships in the range of 4-200 μg/L,and the remain-ing 151 pesticides had good linear relationships in the range of 2-200 μg/L.All pesticides in black tea had good linear relationships in the range of 2-200 μg/L,and the correlation coefficients(r)were all greater than 0.99.Matrix effects of green tea and black tea were-56%-63%and-19%-110%,re-spectively.The recoveries of 116 pesticides in both green tea and black tea were all in the range of 70%-130%at four spiked levels.The relative standard deviations(RSDs)of 99%and 87%pesticides in green tea and black tea were both less than 20%.The limits of quantitation(LOQs)were 10-25 μg/kg.The method was applied to analyze the pesticide residues in 20 real tea samples(14 green teas and 6 black teas).Nine pesticides were detected in green tea and black tea samples,and the resi-dues were lower than the national standard maximum residue limits.This method provides a reference for high-throughput screening and detection of pesticide residues in tea.关键词
茶叶/超高效液相色谱-四极杆/静电场轨道阱高分辨质谱/农药残留/QuEChERS/筛查Key words
tea/UHPLC-Q-Exactive Orbitrap MS/pesticide residue/QuEChERS/screening分类
化学化工引用本文复制引用
方俊兰,张丹阳,伊岳星,刘颖颖,柴云峰,李祖光,陈红平..基于超高效液相色谱-四极杆/静电场轨道阱高分辨质谱筛查茶叶中166种农药残留方法研究[J].分析测试学报,2023,42(12):1537-1546,10.基金项目
现代农业产业技术岗位专家(CAS-19) （CAS-19）
中国农业科学院创新工程(CAAS ASTIP-2014-TRICAAS) （CAAS ASTIP-2014-TRICAAS）
国家自然科学基金项目(30500339) （30500339）
浙江省自然科学基金项目(Y407308) （Y407308）
