色谱

色谱

• 研究论文 • 上一篇    下一篇

高效液相色谱-串联质谱法检测食品中的草甘膦及其主要代谢物氨甲基膦酸残留

李波1,邓晓军1,郭德华1,金淑萍2   

  1. 1.Shanghai Entry-Exit Inspection and Quarantine Bureau, Shanghai 200135, China;
    2.East China University of Science and Technology, Shanghai 200237, China
  • 收稿日期:2006-12-25 修回日期:2007-04-12 出版日期:2007-07-30 发布日期:1985-06-25
  • 通讯作者: 李波

Determination of Glyphosate and Aminomethylphosphonic Acid Residues in Foods Using High Performance Liquid chromatography-Mass Spectrometry/Mass Spectrometry

LI Bo1, DENG Xiaojun1, GUO Dehua1, JIN Shuping2   

  1. 1.Shanghai Entry-Exit Inspection and Quarantine Bureau, Shanghai 200135, China;
    2.East China University of Science and Technology, Shanghai 200237, China
  • Received:2006-12-25 Revised:2007-04-12 Online:2007-07-30 Published:1985-06-25

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摘要：

建立了高效液相色谱-串联质谱测定植物产品(大豆、大米、小麦、蔬菜、水果、茶叶等)、动物肉类产品、水产品、板栗、蜂蜜等产品中草甘膦(PMG)及其主要代谢物氨甲基膦酸(AMPA)残留量的方法。样品经水提取后用二氯甲烷除去其中的脂肪,再经阳离子交换柱(CAX)净化，用 9-芴基甲基氯仿(FMOC-Cl)衍生化,采用多反应监测技术所确定的定性离子对其进行定性，同位素内标法定量。方法的定量检测低限为0.05 mg/kg,线性范围为0.20～10 μg/L,各种基质下PMG和AMPA的平均加标回收率为80.0%～104%,相对标准偏差为6.7%～18.2%。

关键词: 氨甲基膦酸, 草甘膦, 高效液相色谱-串联质谱, 食品 , 同位素内标

Abstract:

A method for the determination of glyphosate (PMG) and aminomethylphosphonic acid (AMPA) residues in plant products, such as rice, wheat, vegetables, fruits and tea, pig and chicken muscles, aquatic products, chestnut, honey, etc., was developed using high performance liquid chromatography coupled to tandem mass spectrometry (HPLC-MS/MS). In this method, PMG and AMPA were extracted with water from samples, defatted using an extraction step with dichloromethane, and purified using a cation-exchange (CAX) solid phase extraction cartridge. Then, these were derived using fluorenylmethylchloroformate (FMOC-Cl) in borate buffer for subsequent HPLC-MS/MS analysis. Isotope-labeled PMG 1,2-13C15N was used as the internal standard for the quantitative analysis of two residues. For all samples, the recoveries ranged from 80.0% to 104% and the relative standard deviations (RSDs) ranged from 6.7% to 18.2%. The limit of quantification (LOQ) was determined to be 0.05 mg/kg with a linear range of 0.20-10 μg/L. It is demonstrated that this method is reliable and sensitive for the analysis of PMG and APMA with low concentrations in foods.

Key words: aminomethylphosphonic acid, foods , glyphosate, labelled glyphosate 1,2-13C15N as internal standard, high performance liquid chromatography-mass spectrometry/mass spectrometry （HPLC-MS/MS）