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固相萃取-气相色谱/三重四极杆质谱法同时分析蔬菜中的50种农药残留量
引用本文:曹慧,林珍珍,陈小珍,李祖光.固相萃取-气相色谱/三重四极杆质谱法同时分析蔬菜中的50种农药残留量[J].浙江工业大学学报,2012,40(3):279-283.
作者姓名:曹慧  林珍珍  陈小珍  李祖光
作者单位:1. 浙江省质量技术监督检测研究院 食品检测部,浙江杭州,310013
2. 浙江工业大学 化学工程与材料学院,浙江杭州,310032
摘    要:采用固相萃取-气相色谱/三重四极杆质谱(GC/MS/MS)法测定蔬菜中50种农药残留量.样品经乙腈提取、固相萃取小柱净化,用气相色谱-质谱/质谱法测定,外标法定量.50种农药在10~500 μg/L范围内线性关系良好,加标回收率在77.30%~116.91%之间,相对标准偏差均小于15%,定性检出限和定量检出限分别为0.1~5.0 μg/kg和0.3~16.7 μg/kg,可以满足欧盟、日本等国对蔬菜中农药残留量的限定要求.该方法具有简单快速,准确度和精密度高,适用于各种蔬菜中农药多残留量的检测和确证.

关 键 词:多农药残留  固相萃取  气相色谱/三重四极杆质谱  蔬菜

Determination of fifty pesticide residues in vegetables by using solid phase extraction-gas chromatography/tandem mass spectrometry
CAO Hui , LIN Zhen-zhen , CHEN Xiao-zhen , LI Zu-guang.Determination of fifty pesticide residues in vegetables by using solid phase extraction-gas chromatography/tandem mass spectrometry[J].Journal of Zhejiang University of Technology,2012,40(3):279-283.
Authors:CAO Hui  LIN Zhen-zhen  CHEN Xiao-zhen  LI Zu-guang
Affiliation:1.Zhejiang Test Academy of Quality and Technical Supervision,Hangzhou 310032,China; 2.College of Chemical Engineering and Materials Science,Zhejiang University of Technology,Hangzhou 310032,China)
Abstract:A method was developed for determination of 50 pesticide residues in vegetables by using gas chromatography-tandem mass spectrometry(GC/MS/MS).The samples were extracted with acetonitrile and cleaned up by solid phase extraction.The extracts were determined by GC/MS/MS using external standard method.The linearity of the method was good between 10 μg/L and 500 μg/L.The method was reliable and stable that the recoveries of 50 pesticides were in the range from 77.30% to 116.91% and the relative standard deviations were all not more than 15%.The limits of detection and the limits of quantitation were 0.1~5.0 μg/kg and 0.3~16.7 μg/kg respectively.The method was simple,accurate and sensitive,and was suitable for the simultaneous analysis of various pesticides residues in vegetables.It can satisfy the legislations on monitoring of pesticide residues in vegetables required by the European Union,Japan and other countries.
Keywords:multiple pesticide residues  solid phase extraction  gas chromatography-tandem mass spectrometry(GC/MS/MS)  vegetables
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