色谱

色谱 ›› 2015, Vol. 33 ›› Issue (3): 235-241.DOI: 10.3724/SP.J.1123.2014.11023

• 研究论文 • 上一篇    下一篇

QuEChERS-超高效液相色谱-串联质谱法测定蔬菜中41种农药残留

林涛1,2, 邵金良1, 刘兴勇1, 杨东顺1, 陈兴连1, 李彦刚1, 樊建麟1, 刘宏程1,2   

  1. 1. 云南省农业科学院质量标准与检测技术研究所, 云南 昆明 650223;
    2. 农业部农产品质量安全风险评估实验室(昆明), 云南 昆明 650223
  • 收稿日期:2014-11-17 修回日期:2014-12-25 出版日期:2015-03-08 发布日期:2015-02-12
  • 通讯作者: 刘宏程
  • 基金资助:

    2014年国家蔬菜产品质量安全风险评估项目(GJFP2014001);云南省社会发展科技计划项目(2012CA005).

Determination of 41 pesticide residues in vegetables by QuEChERS-ultra performance liquid chromatography- tandem mass spectrometry

LIN Tao1,2, SHAO Jinliang1, LIU Xingyong1, YANG Dongshun1, CHEN Xinglian1, LI Yangang1, FAN Jianlin1, LIU Hongcheng1,2   

  1. 1. Institute of Agriculture Quality Standards & Testing Technique, Yunnan Academy of Agricultural Science, Kunming 650223, China;
    2. Laboratory of Quality & Safety Risk Assessment for Agro-Products (Kunming), Ministry of Agriculture, Kunming 650223, China
  • Received:2014-11-17 Revised:2014-12-25 Online:2015-03-08 Published:2015-02-12

PDF

426

被引次数

93

摘要：

采用QuEChERS-超高效液相色谱-串联质谱技术,建立了蔬菜中常见的隐性农药、禁限用农药、植物生长调节剂等检出率较高的41种农药残留的测定方法。蔬菜样品用1%(v/v)乙酸-乙腈溶液提取,乙二胺-N-丙基硅烷(PSA)净化后直接进样分析,采用正、负离子多反应监测(MRM)模式,外标法定量。结果表明,在优化后的QuEChERS、色谱和质谱条件下,41种农药在1.0~100 μg/L范围内线性关系良好,相关系数(r2)大于0.999,检出限为0.003~1.00 μg/kg,不同基质中的平均回收率范围为74.1%~120.4%,相对标准偏差(RSD)范围为2.8%~11.9%。该方法快速简便、灵敏度高、净化效果好,可用于蔬菜中41种农药的快速测定,为蔬菜质量安全风险评估工作提供了有力保障。

关键词: QuEChERS, 残留, 超高效液相色谱-串联质谱, 农药, 蔬菜

Abstract:

A multiresidue analytical method for the rapid determination of 41 pesticide residues in vegetables was developed by using QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS), including recessive pesticides, banned pesticides and pesticides with restrict use, plant growth regulators and some other pesticides with high detection rates. The vegetable sample was extracted by 1% (v/v) acetic acid-acetonitrile, cleaned-up by primary secondary amine (PSA) and injected for analysis. The positive and negative ion modes and multiple reaction monitoring (MRM) mode were used in the analysis, and the analytes were quantified by the external standard method. Under the conditions of optimized QuEChERS, chromatography and mass spectrometry, the 41 pesticides showed good linearities in the range of 1.0 μg/L to 100 μg/L, with the correlation coefficients (r2) higher than 0.999. The limits of detection of the method were 0.003 μg/kg to 1.00 μg/kg. The average recoveries of the 41 pesticides in different matrices were in the range of 74.1%-120.4% with the relative standard deviations from 2.8% to 11. 9%. The method has the advantages of rapidity, simplicity, high sensitivity and better purification effect. It is suitable for the rapid determination of the common pesticides in vegetables, and it provides a strong guarantee for the risk assessment of the quality and safety of vegetables.

Key words: pesticides, QuEChERS, residues, ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS), vegetable

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