色谱

色谱 ›› 2016, Vol. 34 ›› Issue (9): 835-849.DOI: 10.3724/SP.J.1123.2016.04004

• 研究论文 • 上一篇    下一篇

超高效液相色谱-串联质谱法快速检测蔬菜中248种农药残留

李凌云1, 许晓敏1, 林桓1, 赵文2, 叶融3, 黄晓冬1, 郑姝宁1, 刘新艳1, 刘肃1, 徐东辉1   

  1. 1. 中国农业科学院蔬菜花卉研究所, 农业部蔬菜产品质量安全风险评估实验室(北京), 农业部园艺作物生物学与种质创制重点实验室, 北京 100081;
    2. 中国农业科学院蜜蜂研究所, 北京 100093;
    3. 北京林业大学生物科学与技术学院, 北京 100083
  • 收稿日期:2016-04-05 出版日期:2016-09-08 发布日期:2016-08-26
  • 通讯作者: 徐东辉
  • 基金资助:

    国家蔬菜产品质量安全风险评估项目（GJFP2016002）.

Rapid detection of 248 pesticide residues in vegetables by ultra high performance liquid chromatography-tandem mass spectrometry

LI Lingyun1, XU Xiaomin1, LIN Huan1, ZHAO Wen2, YE Rong3, HUANG Xiaodong1, ZHENG Shuning1, LIU Xinyan1, LIU Su1, XU Donghui1   

  1. 1. Institute of Vegetables and Flowers, Chinese Academy of Agricultural Sciences, Ministry of Agriculture Laboratory of Quality & Safety Risk Assessment for Vegetable Products(Beijing), Key Laboratory of Biology and Genetic Improvement of Horticultural Crops, Ministry of Agriculture, Beijing 100081, China;
    2. Institute of Apicultural Research, Chinese Academy of Agricultural Sciences, Beijing 100093, China;
    3. College of Biological Sciences and Biotechnology, Beijing Forestry University, Beijing 100083, China
  • Received:2016-04-05 Online:2016-09-08 Published:2016-08-26
  • Supported by:

    National Vegetable Product Quality and Safety Risk Assessment Project (No. GJFP2016002).

PDF

227

摘要：

采用超高效液相色谱-串联质谱（UHPLC-MS/MS）技术建立了快速检测蔬菜中248种农药残留的分析方法。蔬菜样品采用乙腈提取，盐析后无需净化，缩短了样品前处理的时间。采用正负离子多反应监测（MRM）模式对蔬菜中248种农药残留进行定性和定量分析。245种农药在各自的线性范围内线性关系良好（r>0.99）。除丁硫克百威、灭蝇胺、苯磺隆和二氯喹啉酸4种农药外，其余244种农药在3个添加水平下的平均回收率范围为63.0%～126.4%，相对标准偏差（RSD）范围为0.5%～26.7%，方法的定量限为0.001～0.030 mg/kg。该方法具有简单、快速、灵敏度高、准确度高等优点，适合蔬菜样品中农药多残留的快速检测分析。

关键词: 超高效液相色谱-串联质谱, 农药残留, 蔬菜

Abstract:

A multiresidue analytical method for rapid detection of 248 pesticide residues in vegetables using an ultra high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) technique was successfully developed. The vegetable samples were extracted by acetonitrile. After salting out, the solvent extracts were analyzed by UHPLC-MS/MS directly. And further purification was not needed. The positive and negative ion modes and multiple reaction monitoring (MRM) mode were used to identify and quantify the 248 pesticide residues in vegetables. The results showed that 245 pesticides had good linearity within their respective linear ranges (r>0.99). Except four pesticides (carbosulfan, cyromazine, tribenuron-methyl, quinclorac), the average recoveries of the other 244 pesticides at three spiked levels ranged from 63.0% to 126.4% with the relative standard deviations (RSDs) from 0.5% to 26.7%. The limits of quantification of this method were in the range of 0.001-0.030 mg/kg. In comparison with other pretreatment methods for pesticide residues, this method not only shortened the time of sample pretreatment, but also enhanced significantly the recoveries of pesticides. The results in this study suggested that it is a simple, rapid, sensitive and accurate method for pesticide residue determination, and suitable for rapid screening of pesticide residues in vegetables.

Key words: pesticide residues, ultra high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS), vegetables

中图分类号: