湖北农业科学 ›› 2019, Vol. 58 ›› Issue (21): 163-166.doi: 10.14088/j.cnki.issn0439-8114.2019.21.035

• 检测分析 • 上一篇    下一篇

液质联用法测定果蔬中氨基甲酸酯类农药残留

褚乾梅, 黄大明, 朱梦洁, 王雪, 张姝娟, 董菁, 王盾   

  1. 襄阳市农业科学院,湖北 襄阳 441057
  • 收稿日期:2019-05-08 出版日期:2019-11-10 发布日期:2019-11-27
  • 通讯作者: 王 盾,男,副研究员,博士,主要从事农产品质量安全检测研究,(电子信箱)113093208@qq.com
  • 作者简介:褚乾梅(1989-),女,湖北襄阳人,助理研究员,硕士,主要从事农产品质量安全检测研究,(电话)0710-3085381(电子信箱)529193146@qq.com
  • 基金资助:
    襄阳市青年科技英才开发计划项目

Determination of carbamate pesticides in vegetables and fruits by high performance liquid chromatography-tandem mass spectrometry

CHU Qian-mei, HUANG Da-ming, ZHU Meng-jie, WANG Xue, ZHANG Shu-juan, DONG Jing, WANG Dun   

  1. Xiangyang Academy of Agriculutral Sciences,Xiangyang 441057,Hubei,China
  • Received:2019-05-08 Online:2019-11-10 Published:2019-11-27

摘要: 建立果蔬中多菌灵、啶虫脒、甲萘威等12种氨基甲酸酯类农药的QuEchERs结合高效液相色谱-串联质谱的检测方法。样品经乙腈提取,应用QuEchERs技术净化,经0.22 μm微孔滤膜过滤,以乙腈-5 mmol/L醋酸铵溶液(含0.1%甲酸)为流动相梯度洗脱,并在ZOBRAX EclipseXDB-C18柱上实现12种农药的基线分离。该方法采用多反应监测(MRM)正离子模式扫描,标准曲线外标法定量。结果表明,12种待测物在各自的浓度范围内线性关系良好,相关系数均不小于0.996 6,检出限为0.1 μg/L。在三个不同添加水平下的平均回收率为80%~127%,相对标准偏差为1.1%~10.2%。该方法操作简单,净化效果好,灵敏度高,可用于果蔬中12种氨基甲酸酯类农药残留的快速分析。

关键词: 高效液相色谱-串联质谱, 果蔬, QuEchERs, 氨基甲酸酯类农药, 检测

Abstract: A high performance liquid chromatography-tandem mass spectrometric method with modified QuEchERs method for sample preparation was developed for the simultaneous determination of 12 carbamate pesticides in vegetables and fruits. The samples were extracted with acetonitrile,purified with QuEchERs method and filtrated by 0.22 μm microporous filters. The separation was carried on an ZOBRAX EclipseXDB-C18 Colum(150 mm×4.6 mm,5 μm) by a gradient elution using methanol -5 mmol/L ammonium acetate solution(contain 0.1% formic acid aqueous)as mobile phase. The analytes were detected by tandem mass spectrometry under multiple reaction monitoring(MRM) mode with positive electrospray ionization(ESI+) and quantified by external standard calibration method. The correlation coefficients of the standard calibration curves for the 12 analytes were all above 0.996 6. The limits of detection was 0.1 μg/L. The blank samples were fortified at three leves,and the average recoveries ranged from 80.0% to 127.0% with the RSDs from 1.1% to 10.2%. The method developed was easy to operate,sensitive,and had good purification effect. It could be applied for the rapid determination of 12 carbamate pesticides in vegetables and fruits.

Key words: high performance liquid chromatography-tandem mass spectrometry, vegetables and fruits, QuEchERs, carbamate pesticides, detection

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