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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 • 上一篇    下一篇

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,*   

  1. 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
  • 收稿日期:2023-01-13 修回日期:2023-03-10 出版日期:2023-04-15 发布日期:2023-05-05
  • 通讯作者: *liangshuang@jlau.edu.cn
  • 作者简介:李自强,男,硕士研究生,主要从事农药快速检测方面的研究,lzq_99@126.com。
  • 基金资助:
    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)

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 Shuang1,*   

  1. 1. College of Plant Protection, Jilin Agricultural University, Changchun 130118, China;
    2. Research Center of Quality Safety for Agricultural Products, Tea Research Institute, Chinese Academy of Agricultural Sciences, Hangzhou 310008, China
  • Received:2023-01-13 Revised:2023-03-10 Online:2023-04-15 Published:2023-05-05

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

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