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中国农学通报

中国农学通报 ›› 2020, Vol. 36 ›› Issue (25): 129-136.doi: 10.11924/j.issn.1000-6850.casb20190900621

所属专题： 园艺

• 植物保护·农药 • 上一篇    下一篇

超高效液相-串联质谱法测定茶叶中草甘膦、草铵膦、氨甲基膦酸残留

刘文静(), 林晶, 傅建炜(), 吴建鸿   

  1. 福建省农业科学院农业质量标准与检测技术研究所/福建省农产品质量安全重点实验室,福州 350003
  • 收稿日期:2019-09-10 修回日期:2020-01-08 出版日期:2020-09-05 发布日期:2020-08-18
  • 通讯作者: 傅建炜
  • 作者简介:刘文静,女,1982年出生,山东寿光人,助理研究员,硕士,研究方向：农产品质量安全与检测技术研究。通信地址：350003 福建省农业科学院农业质量标准与检测技术研究所,E-mail：411935637@qq.com。
  • 基金资助:
    福建省公益类项目“福建陈年老茶卫生安全与功能成分分析”(207R1018-1);福建省院青项目“茶叶中真菌毒素的检测与隐患排查分析”(YC2018-11);福建省农科院科技创新团队资助项目“农产品质量安全创新团队”(STIT2017-1-12)

Determination of Glyphosate, Ammonium Phosphate and Ammonia in Tea by UHPLC-MS

Liu Wenjing(), Lin Jing, Fu Jianwei(), Wu Jianhong   

  1. Institute of Agricultural Quality Standards and Testing Technology Research, Fujian Academy of Agricultural Sciences/Fujian Key Laboratory of Agro-products Quality & Safety, Fuzhou 350003
  • Received:2019-09-10 Revised:2020-01-08 Online:2020-09-05 Published:2020-08-18
  • Contact: Fu Jianwei

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摘要：

探讨一种超高效液相-串联质谱法测定茶叶中草甘膦、草铵膦、氨甲基膦酸残留的测定方法,以期为建立茶叶中草铵膦、草甘膦及其代谢产物等农残检测方法的国家标准提供参考。茶样经超纯水、二氯甲烷提取和CAX萃取柱净化后,在硼酸盐缓冲液中与9-芴基甲基三氯甲烷(FMOC-Cl)进行衍生反应,衍生后产物在Waters HSS T3色谱柱上进行超高效液相色谱分离,质谱检测采用电喷雾正离子源、多反应离子监测模式。在0~100 ng/mL范围内,草铵膦、草甘膦和氨甲基膦酸均有良好的线性关系(R2>0.999);方法检出限为0.7 μg/kg;在不同茶类（乌龙茶、花茶、白茶）中添加浓度为2.0、4.0、10.0 μg/kg时,草甘膦的平均回收率为86.3%~100.2%,草铵膦的平均回收率为85.7%~101.5%,氨甲基膦酸的平均回收率为88.1%~98.4%;相对标准偏差(RSD)在1.1%~5.0%之间。该方法样品前处理简单,分析时间短,回收率和精密度等符合农药多残留检测技术的要求,适用于茶叶中草铵膦、草甘膦和氨甲基膦酸残留的同时检测。

关键词: 超高效液相-串联质谱, 草甘膦, 草铵膦, 氨甲基膦酸, 茶叶

Abstract:

A method is developed for the determination of glufosinate-ammonium (GLUF), glyphosate (PMG) and aminomethylphosphonic acid (AMPA) in tea using ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The sample is extracted with ultrapure water and dichloromethane under ultrasonication, followed by a simple cleanup with a C18 solid phase extraction (SPE) cartridge, and then GLUF, PMG and AMPA are derivatized using 9-fluorenylmethoxycarbonyl (FMOC-Cl) in borate buffer. The derivatives of GLUF, PMG and AMPA are separated on a Waters HSS T3 column in a gradient elution mode, and finally detected with positive electrospray ionization-mass spectrometry (ESI-MS/MS) in multiple reaction monitoring (MRM) mode. The quantification analysis is performed by external standard method. The method shows a good linearity (R2>0.999) in the range of 0-100 ng/mL. The limit of detection (LODs) of GLUF, PMG and AMPA is 0.7 g/kg. At the spiked level of 2.0, 4.0和10.0 μg/kg, the recovery of GLUF, PMG and AMPA is 86.3%-100.2%,85.7%-101.5%, and 88.1%-98.4%, respectively, and the relative standard deviation (RSDs) (n=6) of GLUF, PMG and AMPA is 1.1%-5.0% respectively. This method is simple, rapid and characterized with acceptable sensitivity and accuracy to meet the requirements for the analysis of GLUF, PMG and AMPA simultaneously in tea.

Key words: UHPLC-MS, glyphosate, glufosinate-ammonium, aminomethylphosphonic acid, tea

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