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园艺学报 ›› 2017, Vol. 44 ›› Issue (3): 566-574.doi: 10.16420/j.issn.0513-353x.2016-0425

• 新方法 • 上一篇    下一篇

桃果实叶片和土壤草甘膦和氨甲基膦酸残留的HPLC-MS/MS检测方法

乔成奎,王  超,黄玉南,谢汉忠*,罗  静,庞  涛,方金豹   

  1. 中国农业科学院郑州果树研究所,农业部果品质量安全风险评估实验室(郑州),农业部果品及苗木质量监督检验测试中心(郑州),郑州 450009
  • 出版日期:2017-03-25 发布日期:2017-03-25

Determination of Glyphosate and Aminomethylphosphonic Acid Residues in Peach Fruit,Leaf and Soil by High Performance Liquid Chromatography–Tandem Mass Spectrometry

QIAO Chengkui,WANG Chao,HUANG Yunan,XIE Hanzhong*,LUO Jing,PANG Tao,and FANG Jinbao   

  1. Zhengzhou Fruit Research Institute,Chinese Academy of Agricultural Sciences;Laboratory of Quality and Safety Risk Assessment for Fruit(Zhengzhou),Ministry of Agriculture;Fruit and Nursery Stock Quality Supervision and Testing Center(Zhengzhou),the Ministry of Agriculture,Zhengzhou 450009,China
  • Online:2017-03-25 Published:2017-03-25

摘要:

建立了桃果实、叶片和土壤中草甘膦(PMG)及其代谢物氨甲基膦酸(AMPA)的高效液相色谱—串联质谱(HPLC-MS/MS)的检测方法。样品经碳酸氢钠水溶液和二氯甲烷共同提取,以9–芴基甲基三氯甲烷为衍生剂室温下衍生3 h,多反应监测(MRM)模式检测。草甘膦及其代谢物氨甲基膦酸在1 ~ 2 000 μg · L-1的质量浓度范围内线性关系良好,相关系数均大于0.999;在0.01 ~ 1.0 mg · kg-1添加水平下平均回收率为76.7% ~ 93.0%,相对标准偏差(RSD)为2.2% ~ 8.7%;方法定量限(LOQ)均为0.01 mg · kg-1;适用于桃果实和叶片及土壤中草甘膦及其代谢物氨甲基膦酸残留的快速检测。

关键词: 桃;果实;叶片;土壤;草甘膦;氨甲基膦酸;高效液相色谱&mdash, 串联质谱

Abstract:

An analytical method for the determination of glyphosate(PMG)and aminomethyl- phosphonic acid(AMPA)in peach fruit,leaf and soil was established using high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS). The samples were extracted with NaHCO3 water solution and dichloromethane,derived with 9-fluorenylmethyl chloroformate(FMOC-Cl)at room temperature for 3 h,and analyzed in multiple reaction monitoring(MRM)mode. The results indicated good linearity with correlation coefficients greater than 0.999 in the concentration range of 1–2 000 μg · L-1. The average recoveries of PMG and AMPA in each matrixes were found between 76.7% and 93.0% at 0.01–1.0 mg · kg-1,with relative standard deviations(RSD)of 2.2%–8.7%. The limits of  quantification(LOQ)were 0.01 mg · kg-1. The method was suitable for rapid determination of PMG and AMPA residues in fruit and leaf of peach and soil.

Key words: peach, fruit, leaf, soil, glyphosate, aminonethylphosphonic acid, HPLC-MS/MS