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

doi:10.13305/j.cnki.jts.2023.02.001

摘要/Abstract

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。

关键词: QuEChERS, 茶, 草甘膦, 草铵膦, 氨甲基膦酸

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.

Key words: QuEChERS, tea, glyphosate, glufosinate, aminomethyl phosphonic acid

中图分类号:

S517.1
S482

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. doi: 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. doi: 10.13305/j.cnki.jts.2023.02.001.

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