改良QuEChERS方法与UPLC-MS/MS联用测定茶叶中草甘膦、草铵膦及氨甲基膦酸  

Simultaneous Determination of Glyphosate,Glufosinate and Aminomethyl Phosphonic Acid Residues in Tea by Modified QuEChERS Method Coupled with UPLC-MS/MS

作　　者：李自强 杨梅 张新忠[2] 罗逢健[2] 楼正云[2] 梁爽 LI Ziqiang;YANG Mei;ZHANG Xinzhong;LUO Fengjian;LOU Zhengyun;LIANG Shuang(College of Plant Protection,Jilin Agricultural University,Changchun 130118,China;Research Center of Quality Safety for Agricultural Products,Tea Research Institute,Chinese Academy of Agricultural Sciences,Hangzhou 310008,China)

机构地区：[1]吉林农业大学植物保护学院,吉林长春130118 [2]中国农业科学院茶叶研究所农产品质量安全研究中心,浙江杭州310008

出　　处：《茶叶科学》2023年第2期263-274,共12页Journal of Tea Science

基　　金：吉林省科技发展计划项目(20230202025NC);国家自然科学基金青年项目(42007354)。

摘　　要：建立了改良QuEChERS-超高液相色谱-串联质谱法(UPLC-MS/MS)快速检测红茶和绿茶中草甘膦、草铵膦及氨甲基膦酸残留的分析方法。样品经纯净水提取2次,提取液采用MWCNT、C18、PVPP和CNT-OH吸附剂分散固相萃取净化,质谱以多反应监测模式(MRM)进行测定,外标法定量。结果表明,红茶和绿茶基质中,草甘膦、草铵膦和氨甲基膦酸在一定浓度范围内线性良好,相关系数(R^(2))为0.999 3~1.000 0,方法的检出限(LOD)分别为0.005 0、0.030、0.030 mg·kg^(-1),定量限(LOQ)分别为0.050、0.10、0.10 mg·kg^(-1),平均加标回收率在81.6%~120.0%,相对标准偏差(RSD)在0.6%~13.6%。该方法前处理简单、成本低、重复性好、灵敏度高,适用于红茶和绿茶中草甘膦、草铵膦及氨甲基膦酸的检测。An analytical method was developed for the simultaneous determination of glyphosate,glufosinate and aminomethyl phosphonic acid residues in black and green tea by ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)coupled with a modified QuEChERS method.The samples were extracted twice with pure water,and the extraction solutions were purified by dispersive solid phase extraction with MWCNT,C18,PVPP and CNT-OH adsorbents.The mass spectrometry was performed in multiple reaction monitoring(MRM)mode and quantified by external standard method.The results show that glyphosate,glufosinate and aminomethyl phosphonic acid had a good linear relationship within a certain concentration range with correlation coefficients(R^(2))ranging from 0.9993 to 1.0000 in black and green tea.The limits of detection(LOD)of the method were 0.0050,0.030 mg·kg^(-1) and 0.030 mg·kg^(-1),respectively.The limits of quantitation(LOQ)were 0.050,0.10 mg·kg^(-1) and 0.10 mg·kg^(-1),respectively.The average spiked recovery rates and the relative standard deviations(RSD)of pesticides were in the range of 81.6%-120.0%and 0.6%-13.6%,respectively.The method is simple,inexpensive,reproducible,sensitive and suitable for the determination of glyphosate,glufosinate and aminomethyl phosphonic acid in black and green tea.

关 键 词：QUECHERS 茶 草甘膦 草铵膦 氨甲基膦酸 

分 类 号：S517.1[农业科学—作物学] S482