加速溶剂萃取凝胶渗透色谱/固相萃取净化气相色谱质谱法测定咸鱼中有机磷农药残留

Determination of Organophosphate Pesticide Residues in Salt Fish Using Accelerated Solvent Extraction and Gel Permeation Chromatography/Solid Phase Extraction with Gas Chromatography-Mass Spectrometry

建立了咸鱼中有机磷农药残留的分析方法。乙腈为溶剂,样品经ASE萃取,提取液用凝胶渗透色谱除去脂类、蛋白质和大部分的色素,再经Carb/PSA小柱净化。采用GC-MS定性分析,GC-FPD定量分析。加标水平为0.05～0.20mg/kg时,农药的回收率为64.5%～98.6%,相对标准偏差2.7%～14.7%。方法的检出限为0.6～9.0μg/kg(以3倍性噪比计)。本方法具有提取效率高,净化效果好,回收率高,准确灵敏等优点,适用于咸鱼中农药残留检测实际工作的需要。

A novel method for the determination organophosphrous pesticides residues in salt fish was established.The target anslytes were extracted by accelerated solvent extraction（ASE） using acetonitrile as the extraction solvent.The gel permeation chromatography was used to remove the grease,protein and pigment and then,the small molecule compounds in the extracted solution were purified by the Carb/PSA solid phase extraction.The qualitative analysis were performed by using mass spectrometric detection GC-MSD（SIM） and quantitative analysis by GC-flame photometry detector（FPD） method.The average recoveries of organophosphrous pesticides were 64.5%-98.6%,spiked at 0.05-0.20mg/kg levels.The relative standard deviations for all the compounds were 2.7%-14.7%.The detection limit of the method varied between 0.0006 0.0090 mg/kg.The method is rapid,precise,sensitive,high efficient.It can be applied to the routine analysis for organophosphrous pesicide resdues in salt fish.