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中国农学通报 ›› 2017, Vol. 33 ›› Issue (36): 152-156.doi: 10.11924/j.issn.1000-6850.casb17070075

所属专题: 园艺

• 植物保护 农药 • 上一篇    下一篇

超高效液相色谱-串联质谱法测定甜菜中除草剂残留含量

周芹,吴玉梅   

  1. 黑龙江大学农作物研究院,黑龙江大学农作物研究院
  • 收稿日期:2017-07-16 修回日期:2017-11-15 接受日期:2017-11-17 出版日期:2017-12-29 发布日期:2017-12-29
  • 通讯作者: 吴玉梅
  • 基金资助:
    国家甜菜现代产业技术体系建设项目“质量安全与营养品质评价”(CARS-170503);国家农产品质量安全风险评估专项经费“糖料食用特 色农产品质量安全风险因子摸底排查与特质性营养品质评价”(GJFP201701002)。

Determination of Pesticide residues in Sugarbeet by ultra High Perfoemance Liquid Chromatography tandem mass spectrometry

  • Received:2017-07-16 Revised:2017-11-15 Accepted:2017-11-17 Online:2017-12-29 Published:2017-12-29

摘要: 为了建立甜菜中三种除草剂的定量分析方法,采用超高效液相色谱-电喷雾串联四极杆质谱仪, 在多反应监测正负离子扫描模式下对样品进行添加回收率试验。样品经甲醇配合快速溶剂萃取仪提取后配合固相萃取前处理小柱,甲醇、丙酮、二氯甲烷各2 mL为洗脱溶剂净化,外标法定量。结果表明:加标水平分别为50 μg/kg、20 μg/kg、10 μg/kg时,回收率为65.81%~100.36%,相对标准偏差(RSD)为1.4%~6.55%,方法的定量限在0.6 μg/kg~2.5 μg/kg之间,该方法具有快速、简便、灵敏度较高的特点,能同时满足甜菜中3种农药残留分析的要求。

Abstract: The paper aims to establish a quantitative analysis method for detecting three herbicides’residues in sugarbeet. The authors performed recovery tests by ultra high performance liquid chromatography-tandem mass spectrometry under multiple reaction monitoring mode. The sample was extracted with methanol by accelerated solvent extraction (ASE), and purified by solid phase extraction with methanol, acetone and dichloromethane, 2 mL each, and quantified by the external standard method. The results showed that: the recoveries at three spiked concentration levels of 50, 20, 10 μg/kg ranged from 65.81% to 100.36%, and RSD was between 1.4% and 6.55%, the limits of quantification of this method were in the range of 0.6-2.5 μg/kg. The method is not only fast and simple, but also high sensitive, can satisfy the detection requirement for the three herbicides’residues in sugarbeet simultaneously.