色谱

色谱 ›› 2010, Vol. 28 ›› Issue (08): 743-748.DOI: 10.3724/SP.J.1123.2010.00743

• 研究论文 • 上一篇    下一篇

液相色谱-串联质谱法测定稻米中的草甘膦和氨甲基膦酸残留

曹赵云, 牟仁祥, 陈铭学*   

  1. 中国水稻研究所, 农业部稻米及制品质量监督检验测试中心, 浙江 杭州 310006
  • 收稿日期:2010-04-19 修回日期:2010-06-28 出版日期:2010-08-28 发布日期:2010-08-28
  • 通讯作者: 研究员. Tel: (0571)63370275.
  • 基金资助:

    基金项目：浙江省科学仪器设备协作共用平台科研计划资助项目(No.2008F70020)

Determination of glyphosate and aminomethylphosphonic acid in rice by liquid chromatography-tandem mass spectrometry

CAO Zhaoyun, MOU Renxiang, CHEN Mingxue*   

  1. Rice Product Quality Inspection and Supervision Center of Ministry of Agriculture, China National Rice Research Institute, Hangzhou 310006, China
  • Received:2010-04-19 Revised:2010-06-28 Online:2010-08-28 Published:2010-08-28

PDF

705

被引次数

59

摘要： 采用液相色谱-串联质谱建立了稻米中草甘膦及氨甲基膦酸残留量的测定方法。试样经水提取和C18固相萃取柱净化后,在硼酸缓冲液中与9-芴甲基氯甲酸酯(FMOC-Cl)进行衍生反应。以5 mmol/L乙酸铵溶液(pH 9)和乙腈为流动相,草甘膦和氨甲基膦酸的衍生产物在C18柱进行液相色谱分离;质谱检测采用电喷雾负离子化模式和多反应监测模式。结果表明,草甘膦和氨甲基膦酸在0.00050～1.0 mg/L范围内线性良好,线性相关系数(r)分别为0.9997和0.9999。通过对空白大米样品进行3个加标水平的添加回收实验(n=5),草甘膦和氨甲基膦酸的平均回收率和相对标准偏差(RSD)分别为72.5%～113.6%和3.8%～16.2%,方法的检出限分别为2.0 μg/kg和3.0 μg/kg。该方法快速、灵敏,适用于稻米中草甘膦和氨甲基膦酸的同时分析。

关键词: 氨甲基膦酸, 草甘膦, 稻米, 液相色谱-串联质谱, 柱前衍生化

Abstract: A method was developed for the determination of glyphosate (GLY) and amino-methylphosphonic acid (AMPA) in rice using liquid chromatography tandem mass spectrometry (LC-MS/MS). The sample was extracted with water followed by a simple cleanup with a C18 solid phase extraction (SPE) cartridge, and then GLY and AMPA were derivatized using 9-fluorenylmethoxycarbonyl (FMOC-Cl) in borate buffer. The derivatives of GLY and AMPA were separated on a C18 column with gradient elution with the mobile phase of acetonitrile and 5 mmol/L ammonium acetate (pH 9), and finally detected with negative ion electrospray ionization-mass spectrometry (ESI-MS) in multiple reaction monitoring (MRM) mode. The results showed that the linearities of GLY and AMPA were in the concentration range of 0.00050 to 1.0 mg/L with the correlation coefficients of 0.9997 and 0.9999, respectively. The mean spiked recoveries of GLY and AMPA at 3 spiked levels ranged from 72.5% to 113.6% with the relative standard deviations (RSD, n=5) of 3.8%-16.2%. The limits of detection were 2.0 and 3.0 μg/kg for GLY and AMPA, respectively. This method is rapid, sensitive, and suitable for simultaneous determination of GLY and AMPA in rice.

Key words: aminomethylphosphonic acid, glyphosate, liquid chromatography-tandem mass spectrometry (LC-MS/MS), pre-column derivatization, rice