加速溶剂萃取-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

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。

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.