QuEChERS结合气相色谱串联质谱测定食用油中的200多种农药残留
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- 英文论文题名：Determination of over 200 pesticides in vegetable oils using QuEChERS sample preparation and GC-MS/MS analysis
- 论文作者：贺泽英 ; 王雯雯 ; 吕美玲 ; 刘潇威
- 英文论文作者：Zeying He ; Wenwen Wang ; Meiling lu ; Xiaowei Liu ; Agro-Environmental Protection Institute ; Ministry of Agriculture ; Agilent Technologies (China) Company ; Ltd.
- 年：2016
- 作者机构：农业部环境保护科研监测所;安捷伦科技(中国)有限公司;
- 论文关键词：QuEChERS ; EMR ; 食用油 ; GC-MS/MS ; 农药多残留
- 会议召开时间：2016-07-01
- 会议录名称：中国化学会第30届学术年会摘要集-第四十三分会：质谱分析
- 语种：中文
- 分类号：TS227;O657.63
- 学会代码：ZGHY
- 会议名称：中国化学会第30届学术年会-第四十三分会 ; 质谱分析
- 会议地点：中国辽宁大连
- 主办单位：中国化学会
- 学会名称：中国化学会
- 页数：1
- 文件大小：219k
- 原文格式：D
- 会议级别：全国
摘要
本研究开发了基于QuEChERS方法和EMR新型净化材料,应用气相色谱三重串联四极杆质谱联用仪(GC-MS/MS)同时测定食用油中200多种农药残留的简单、高通量分析方法。研究中对样品的提取和净化相关参数包括提取时间、溶剂与样品比、缓冲盐体系和净化材料的选择等进行了系统的对比和优化。为了更好的进行方法验证,共进行了7水平添加回收试验,分别是5、10、20、50、100、200和500μg kg~(-1)。方法的定量限在5~20μg kg~(-1)之间,大部分农药定量限为5μg kg~(-1),低于最大残留限量。七水平添加回收的回收率绝大部分在70~120%之间,相对标准偏差小于20%,研究表明,本方法具有很好的准确度。绝大部分农药在2.0-500μgL~(-1)的浓度范围之间线性良好,相关系数大于0.99。经验证,该多残留方法简单、灵敏、高效,能够用于食用油中大规模农药残留的筛查和定量分析。
In this study,a simple and high-throughput method for determination of over 200 pesticides in vegetable oils was developed based on QuEChERS(quick,easy,cheap,effective,rugged,and safe) sample preparation and a new EMR clean-up kit combined with gas chromatography-triple quadrupole mass spectrometry(GC-MS/MS).The extraction and clean-up procedures and parameters including extraction time,solvent/sample ratio,buffer system,and clean-up adsorbent selection were thoroughly investigated and optimized.For validation purpose,seven fortification levels were performed at 5,10,20,50,100,200 and 500 μg kg~(-1).The limits of quantification(LOQ)ranged between 5 and 20 μg kg~(-1),and for the majority of the pesticides,the LOQs were 5 μg kg~(-1),which were below the regulatory MRLs.This method was proved to be simple,sensitive and effective,which can be applied for large-scale pesticide screening and quantification in vegetable oils.
In this study,a simple and high-throughput method for determination of over 200 pesticides in vegetable oils was developed based on QuEChERS(quick,easy,cheap,effective,rugged,and safe) sample preparation and a new EMR clean-up kit combined with gas chromatography-triple quadrupole mass spectrometry(GC-MS/MS).The extraction and clean-up procedures and parameters including extraction time,solvent/sample ratio,buffer system,and clean-up adsorbent selection were thoroughly investigated and optimized.For validation purpose,seven fortification levels were performed at 5,10,20,50,100,200 and 500 μg kg~(-1).The limits of quantification(LOQ)ranged between 5 and 20 μg kg~(-1),and for the majority of the pesticides,the LOQs were 5 μg kg~(-1),which were below the regulatory MRLs.This method was proved to be simple,sensitive and effective,which can be applied for large-scale pesticide screening and quantification in vegetable oils.
引文
[1]Ma,F.;Rao Wu,R.;Li,P.;Yu,L.,Analytical approaches for measuring pesticides,mycotoxins and heavy metals in vegetable oils:A review.Eur.J.Lipid Sci.Tech.2015,118:339.
[2]Chamkasem,N.;Harmon,T.,Analysis of Pesticides in Olive Oil Using a Modified Qu ECh ERS Method with LC-MS/MS and GC-MS/MS[J].J.Regu.Sci.2015,3(1):16.
[2]Chamkasem,N.;Harmon,T.,Analysis of Pesticides in Olive Oil Using a Modified Qu ECh ERS Method with LC-MS/MS and GC-MS/MS[J].J.Regu.Sci.2015,3(1):16.
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