加速溶剂提取-凝胶渗透色谱净化-气相色谱测定咸鱼中的敌敌畏

doi:10.7506/spkx1002-6630-201014061

食品科学 ›› 2010, Vol. 31 ›› Issue (14): 268-271.doi: 10.7506/spkx1002-6630-201014061

加速溶剂提取-凝胶渗透色谱净化-气相色谱测定咸鱼中的敌敌畏

王耀，胡浩光，谢翠美，卢伟华*

东莞市海洋与渔业环境监测站

收稿日期:2009-10-11 修回日期:2010-03-31 出版日期:2010-07-15 发布日期:2010-12-29
通讯作者: 王耀 E-mail:wyhf1@163.com；wangyao@dg.gov.cn
基金资助:
东莞市科技计划项目(K1000010701)

Determination of Dichlorvos Residue in Dried Salted Fish by Accelerated Solvent Extraction-Gel Permeation Chromatography Purification Followed by Gas Chromatography

WANG Yao，HU Hao-guang，XIE Cui-mei，LU Wei-hua*

(Dongguan Marine and Fishery Environment Monitoring Station, Dongguan 523079, China)

Received:2009-10-11 Revised:2010-03-31 Online:2010-07-15 Published:2010-12-29
Contact: WANG Yao E-mail:wyhf1@163.com；wangyao@dg.gov.cn

摘要/Abstract

摘要：

建立咸鱼中敌敌畏残留的气相色谱分析方法。采用加速溶剂萃取(ASE)提取咸鱼样品中的敌敌畏，经凝胶渗透色谱(GPC)净化，浓缩定容后用GC-FPD 检测分析，外标法定量。样品添加水平为2.5 × 10-2mg/kg 和10.0 ×10-2mg/kg 时，敌敌畏的回收率在74.4%～96.8% 之间，方法检出限为5.0 × 10-4mg/kg。本方法准确、自动化程度高、净化效果好，满足残留分析要求。

关键词: 加速溶剂提取, 凝胶渗透色谱, 气相色谱, 敌敌畏, 咸鱼

Abstract:

A novel method has been developed to determine dichlorvos residue in dried salted fish using capillary gas chromatography (GC). Samples were extracted by accelerated solvent extraction and cleaned up by gel permeation chromatography. The eluate was condensed and injected into a gas chromatograph equipped with a flame photometric detector (FPD) for the quantification of dichlorvos by external standard method. Recovery rates for dichlorvos in 9 varieties of blank dried salted fish samples spiked at 2.5 × 10-2 mg/kg and 10.0 × 10-2 mg/kg ranged from 74.4% to 96.8%. The limit of detection (LOD) of this method was 5.0×10-4 mg/kg. This method is accurate, highly automated and presents high cleanup effectiveness. It can meet the requirements of pesticide residue analysis.

Key words: accelerated solvent extraction, gel permeation chromatography, gas chromatography, dichlorvos, dried salted fish

中图分类号:

TS207.53

王耀，胡浩光，谢翠美，卢伟华*. 加速溶剂提取-凝胶渗透色谱净化-气相色谱测定咸鱼中的敌敌畏[J]. 食品科学, 2010, 31(14): 268-271.

WANG Yao，HU Hao-guang，XIE Cui-mei，LU Wei-hua*. Determination of Dichlorvos Residue in Dried Salted Fish by Accelerated Solvent Extraction-Gel Permeation Chromatography Purification Followed by Gas Chromatography[J]. FOOD SCIENCE, 2010, 31(14): 268-271.

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加速溶剂提取-凝胶渗透色谱净化-气相色谱测定咸鱼中的敌敌畏

Determination of Dichlorvos Residue in Dried Salted Fish by Accelerated Solvent Extraction-Gel Permeation Chromatography Purification Followed by Gas Chromatography

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