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超快速液相色谱-串联质谱法快速筛查蔬菜中176种农药残留

[Rapid screening of 176 pesticide residues in vegetables by ultra fast liquid chromatography-tandem mass spectrometry].

作者信息

Zheng Shuning, Li Lingyun, Lin Huan, Zhao Wen, Zhang Yanguo, Yao Zhoulin, Liu Su

机构信息

Institute of Vegetables and Flowers, Chinese Academy of Agricultural Sciences, Supervision and Testing Center for Vegetable Quality, Ministry of Agriculture, Beijing 100081, China.

出版信息

Se Pu. 2013 Jan;31(1):71-8. doi: 10.3724/sp.j.1123.2012.07033.

DOI:10.3724/sp.j.1123.2012.07033
PMID:23667993
Abstract

A multiresidue analytical method for rapid screening of 176 pesticide residues in vegetables was developed by using ultra fast liquid chromatography-tandem mass spectrometry (UFLC-MS/MS). The vegetable samples were extracted by acetonitrile. It is not necessary for the extract to make a further purification after salting out. Multiple reaction monitoring with information-dependent acquisition of enhanced product ion (MRM-IDA-EPI) was used for the analysis. Based on EPI spectra and chromatographic peak area, identification and quantification of the 176 pesticide residues in vegetables were carried out by using library search technique. All the pesticides had the good linearity within their respective linear ranges (r > 0.99). The average recoveries of the 174 pesticides except for carbosulfan and cyromazine were in the range of 72.4% to 126.4% with the relative standard deviations (RSDs) from 1.0% to 18.7%. The limits of detection and quantification of the method were 0.005 - 2.0 microg/kg and 0.1 - 10 microg/kg, respectively. The results demonstrated that the method has distinct advantages of rapid speed, high sensitivity and good accuracy. Therefore, this method is suitable for the rapid screening of pesticide residues in vegetables.

摘要

采用超快速液相色谱-串联质谱法(UFLC-MS/MS)建立了一种用于快速筛查蔬菜中176种农药残留的多残留分析方法。蔬菜样品用乙腈提取。提取液经盐析后无需进一步净化。采用多反应监测-信息依赖采集增强产物离子(MRM-IDA-EPI)进行分析。基于EPI光谱和色谱峰面积,利用库检索技术对蔬菜中的176种农药残留进行定性和定量分析。所有农药在各自线性范围内均具有良好的线性关系(r>0.99)。除丁硫克百威和环丙氨嗪外,174种农药的平均回收率在72.4%至126.4%之间,相对标准偏差(RSD)为1.0%至18.7%。该方法的检出限和定量限分别为0.005 - 2.0μg/kg和0.1 - 10μg/kg。结果表明,该方法具有速度快、灵敏度高、准确性好等明显优点。因此,该方法适用于蔬菜中农药残留的快速筛查。

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