食品科学 ›› 2017, Vol. 38 ›› Issue (20): 235-241.doi: 10.7506/spkx1002-6630-201720034

• 安全检测 • 上一篇    下一篇

QuEChERS法-液相色谱-串联质谱法测定蔬菜中7 种农药及其代谢物的残留量

王建华,葛敏敏,张慧丽,林洪,汤志旭,李立   

  1. (1.山东出入境检验检疫局检验检疫技术中心,山东?青岛 266002;2.中国海洋大学食品科学与工程学院,山东?青岛 266100;3.中国检验检疫科学研究院,北京 100176)
  • 出版日期:2017-10-25 发布日期:2017-09-29
  • 基金资助:
    公益性行业(质检)科研专项(201410177;201210012)

Determination of 7 Pesticide and Metabolite Residues in Vegetables Using QuEChERS and Liquid Chromatography-Tandem Mass Spectrometry

WANG Jianhua, GE Minmin, ZHANG Huili, LIN Hong, TANG Zhixu, LI Li   

  1. (1. Inspection and Quarantine Technical Center, Shandong Entry-Exit Inspection and Quarantine Bureau, Qingdao 266002, China; 2. College of Food Science and Engineering, Ocean University of China, Qingdao 266100, China; 3. Chinese Academy of Inspection and Quarantine, Beijing 100176, China)
  • Online:2017-10-25 Published:2017-09-29

摘要: 样品经乙腈提取,C18吸附剂和石墨化碳黑分散固相萃取净化,液相色谱-三重四极杆串联质谱在动态多反应监测模式下检测,基质匹配标准曲线外标法进行定量,建立了蔬菜中7?种农药及其代谢物的多残留分析方法。在10、20?μg/kg?7种农药及其添加物添加水平下,农药及其代谢物的平均回收率为71.9%~117.8%,相对标准偏差为0.8%~9.6%,定量限为0.2~10?μg/kg。该方法简便、快速、灵敏,适用于蔬菜中多种农药及其代谢物的同时检测。

关键词: 液相色谱-串联质谱, 蔬菜, 农药及其代谢物?

Abstract: A method was developed for the simultaneous determination of 7 pesticide and metabolite residues in vegetables by employing quick, easy, cheap, effective, rugged and safe (QuEChERS) extraction coupled with liquid chromatography triple quadrupole mass spectrometry (LC-MS/MS). Samples were extracted with acetonitrile, and then the extract was purified by dispersive solid phase extraction (SPE) using graphite carbon black (GCB) and C18 sorbent. The analytes were monitored by liquid chromatography-tandem triple quadrupole mass spectrometry in the dynamic multiple reaction monitoring (DMRM) mode, and quantification was carried out by the external standard method with matrix-match standard solution. The recoveries at spiked levels of 10 and 20 μg/kg were in the range from 71.9% to 117.8% and the precision, expressed as relative standard deviation (RSD, n=3), ranged from 0.8% to 9.6% under the selected conditions. The limits of quantification (LOQs) were in the range of 0.2–10 μg/kg. The method proved to be simple, fast, sensitive and useful for the analysis of the 7 pesticides and their metabolite residues in vegetables.

Key words: liquid chromatography-tandem mass spectrometry (LC-MS/MS), vegetables, pesticides and metabolites

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