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

李自强; 杨梅; 张新忠; 罗逢健; 楼正云; 梁爽

doi:10.13305/j.cnki.jts.2023.02.001

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茶叶科学 ›› 2023, Vol. 43 ›› Issue (2) : 263-274. DOI: 10.13305/j.cnki.jts.2023.02.001

研究报告

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

李自强¹, 杨梅², 张新忠², 罗逢健², 楼正云², 梁爽^1,*

作者信息 +

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

LI Ziqiang¹, YANG Mei², ZHANG Xinzhong², LUO Fengjian², LOU Zhengyun², LIANG Shuang^1,*

Author information +

文章历史 +

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（R²）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。

Abstract

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 (R²) ranging from 0.999 3 to 1.000 0 in black and green tea. The limits of detection ( LOD ) of the method were 0.005 0, 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.

导出引用

李自强, 杨梅, 张新忠, 罗逢健, 楼正云, 梁爽. 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[J]. 茶叶科学. 2023, 43(2): 263-274 https://doi.org/10.13305/j.cnki.jts.2023.02.001

LI Ziqiang, YANG Mei, ZHANG Xinzhong, LUO Fengjian, LOU Zhengyun, LIANG Shuang. Simultaneous Determination of Glyphosate, Glufosinate and Aminomethyl Phosphonic Acid Residues in Tea by Modified QuEChERS Method Coupled with UPLC-MS/MS[J]. Journal of Tea Science. 2023, 43(2): 263-274 https://doi.org/10.13305/j.cnki.jts.2023.02.001

中图分类号： S517.1 S482

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