色谱

色谱

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超高效液相色谱-串联质谱法快速测定农产品中残留的种衣剂农药

陈跃1,王金花2,卢晓宇2,汪万春2,黄梅2,徐超一2   

  1. 1.School of Science, Beijing University of Chemical Technology, Beijing 100029, China; 2.Technology Center, Beijing Entry-Exit Inspection and Quarantine Bureau, Beijing 100026, China
  • 收稿日期:2008-04-07 修回日期:2008-07-07 出版日期:2008-11-30 发布日期:1983-06-25
  • 通讯作者: 王金花
  • 基金资助:
    国家质检总局科技计划项目(2006IK220)

Determination of pesticide residues from seed coating reagent in agricultural products using ultra performance liquid chromatography-tandem mass spectrometry

CHEN Yue1, WANG Jinhua2, LU Xiaoyu2, WANG Wanchun2, HUANG Mei2, XU Chaoyi2   

  1. 1.School of Science, Beijing University of Chemical Technology, Beijing 100029, China; 2.Technology Center, Beijing Entry-Exit Inspection and Quarantine Bureau, Beijing 100026, China
  • Received:2008-04-07 Revised:2008-07-07 Online:2008-11-30 Published:1983-06-25
  • Contact: WANG Jinhua

PDF

946

被引次数

24

摘要： 应用超高效液相色谱-串联质谱(UPLC-MS/MS)联用技术,建立了高灵敏、快速地同时检测农产品中8种种衣剂农药残留量的方法。样品经甲醇-水(体积比为1∶1)提取后,无需经过任何净化过程;以梯度流动相洗脱、经Acquity UPLC C18超高效液相色谱柱分离;电喷雾正离子(ESI+)采集模式、多反应监测模式(MRM)对定量离子和定性离子进行MS/MS测定。8种种衣剂农药在0.001～0.20 mg/L范围内线性关系良好(r≥0.997)。添加浓度为0.006～1.2 mg/kg时,回收率为60%～110%,相对标准偏差小于10%;方法的检出限为0.0005～0.002 mg/kg。该方法仅需约2 min的检测时间,而且灵敏、准确,适合于水果、蔬菜、粮谷等农产品中种衣剂农药残留量的快速、高灵敏地检测分析。

关键词: 超高效液相色谱-串联质谱, 农产品 , 农药残留, 种衣剂

Abstract: An ultra performance liquid chromatography-tandem mass spectrometric method (UPLC-MS/MS) has been developed for the simultaneous determination of eight pesticide residues from seed coating in fruits, vegetable and grain. The sample was extracted by methanol-water (1∶1, v/v) and determined by ultra performance liquid chromatography-electrospray ionization tandem mass spectrometry in positive mode (ESI+) and multiple reaction monitoring (MRM) mode. The UPLC analyses were performed on an Acquity UPLC C18 column with gradient eluation. The utility of the method was demonstrated by the analysis of crude extracts, with no sample clean up, from soybean. The linear range was 1-200 μg/L. The correlation coefficients (r) were under 0.997. The average recoveries of eight pesticides in samples (from 0.006 to 1.2 mg/kg) ranged from 60% to 110%, and the relative standard deviations (RSDs) were less than 10%. The results indicate that the method is easier, faster, more sensitive, and suitable for the qualitative and quantitative confirmation of pesticide residues from seed coating reagent in fruit, vegetable and grain samples.

Key words: agricultural products , pesticide residue, seed coating reagent, ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)