色谱

色谱 ›› 2019, Vol. 37 ›› Issue (1): 93-99.DOI: 10.3724/SP.J.1123.2018.08002

• 研究论文 • 上一篇    下一篇

基于高效液相色谱-三重四极杆质谱技术测定荔枝和香蕉中的草铵膦及3种代谢物

王思威1, 曾广丰2, 刘艳萍1, 王潇楠1, 孙海滨1   

  1. 1. 广东省农业科学院植物保护研究所, 广东省植物保护新技术重点实验室, 广东 广州 510640;
    2. 广东省出入境检疫检验局检验检疫技术中心, 广东 广州 510623
  • 收稿日期:2018-08-02 出版日期:2019-01-08 发布日期:2014-11-29
  • 通讯作者: 孙海滨E-mail:sunhb@gdppri.cn.
  • 基金资助:

    国家重点研发计划项目（2016YFD0200206-Y）；国家荔枝龙眼产业技术体系（CARS-32-16）.

Determination of glufosinate-ammonium and its three metabolites in litchi and banana by high performance liquid chromatography coupled with triple quadrupole mass spectrometry

WANG Siwei1, ZENG Guangfeng2, LIU Yanping1, WANG Xiaonan1, SUN Haibin1   

  1. 1. Guangdong Provincial Key Laboratory of High Technology for Plant Protection, Institute of Plant Protection, Guangdong Academy of Agricultural Sciences, Guangzhou 510640, China;
    2. Guangdong Inspection and Quarantine Technology Center, Guangzhou 510623, China
  • Received:2018-08-02 Online:2019-01-08 Published:2014-11-29
  • Supported by:

    National Key Research and Development Plan Project (No. 2016YFD0200206-Y); China Litchi and Longan Research System (No. CARS-32-16).

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摘要：

采用高效液相色谱-三重四极杆质谱技术，建立了荔枝和香蕉中草铵膦及3种代谢物的检测分析方法。样品加水超声提取，离心沉淀后进样分析，分析物经Extend-C18色谱柱分离，以0.1%氨水-甲醇（9：1，v/v）作为流动相等度洗脱，在电喷雾负离子扫描、多反应监测模式下，外标法定量分析，同时探讨了前处理和仪器分析条件对草铵膦及代谢物的影响效果。结果表明，草铵膦及3种代谢物在1~1000 μg/L范围内，峰面积与质量浓度的线性关系良好；当添加浓度水平在50、100、1000 μg/kg时，草铵膦及代谢物在荔枝和香蕉中的平均回收率为82.9%~98.6%，相对标准偏差（RSD）为2.6%~6.3%，检出限（LOD）为5~10 μg/kg。本方法简化了样品前处理步骤，具有良好的可靠性和灵敏度，适于荔枝和香蕉中草铵膦及其代谢物的快速分析。

关键词: 草铵膦, 代谢物, 高效液相色谱, 荔枝, 三重四极杆质谱, 香蕉

Abstract:

A method was developed for the determination of glufosinate-ammonium and its metabolites in litchi and banana by high performance liquid chromatography coupled with triple quadrupole mass spectrometry. The samples were ultrasound extracted by water, centrifuged to precipitate, and filtered through a 0.22 μm Millipore membrane. The sample extract was separated by an Extend-C18 column with 0.1% ammonia-methanol (9:1, v/v) as mobile phase with an isocratic elution, identified by electrospray ionization in negative and multiple reaction monitoring modes, and quantified with external standard method. Moreover, the pretreatment and mass spectrometry conditions were discussed. The method showed good linear relationship in the range of 1-1000 μg/L for glufosinate-ammonium and its metabolites. The average recoveries ranged from 82.9% to 98.6% with the relative standard deviations of 2.6%-6.3% when the litchi and banana samples were spiked at 50, 100, 1000 μg/kg. The limits of detection were 5-10 μg/kg. The method has rapid analysis speed as well as high reliability and sensitivity, which are suitable for the fast determination of glufosinate-ammonium and its metabolites in litchi and banana samples.

Key words: banana, glufosinate-ammonium, high performance liquid chromatography (HPLC), litchi, metabolites, triple quadrupole mass spectrometry (MS/MS)

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