加速溶剂萃取-凝胶渗透色谱净化-气相色谱快速分析动物源性食品中残留的多种有机磷农药

建立了动物源性食品猪肉、牛肉、鸡肉及鱼肉中36种有机磷农药残留的快速分析方法。以乙腈作为溶剂,对试样采用加速溶剂萃取仪萃取,自动凝胶渗透色谱仪净化预处理,N-丙基乙二胺(PSA)填料再净化,毛细管气相色谱法分离,火焰光度检测器(磷型)检测,内标法定量。该方法分离效果良好,重现性好,灵敏度、精密度高,杂质干扰少。36种有机磷农药的检测限(LOD)为0.0012 mg/kg(乙拌磷)～0.014 mg/kg(吡唑硫磷),定量限(LOQ)为0.004 mg/kg(乙拌磷)～0.047 mg/kg(吡唑硫磷)。当试样中有机磷农药的添加浓度分别为0.05,0.1,0.2 mg/kg时,回收率为58.2%～106.3%。方法的最低检测限和添加回收率均符合农药残留分析的要求。

A rapid multi-residual analysis for organophosphorus pesticides in the products of animal origin using gas chromatography coupled with accelerated solvent extraction and gel permeation chromatographic purification

A rapid method has been developed to determine the multi-residues of 36 organophosphorus pesticides in the products of animal origin using capillary gas chromatography with flame photometric detector (GC-FPD (P)). The organophosphorus pesticides were extracted with acetonitrile by accelerated solvent extraction, and cleaned up by auto gel permeation chromatography and primary secondary amine (PSA) packing material. The collected solution was analyzed by the GC-FPD (P) and quantified by internal standard method. The 36 organophosphorus pesticides were separated efficiently from impurity in high sensitivity and reproducibility by GC-FPD (P). The limits of detection (LODs) ranged from 0.0012 mg/kg (phorate) to 0.014 mg/kg (pyraclofos), and the limits of quantitation (LOQs) ranged from 0.004 mg/kg (phorate) to 0.047 mg/kg (pyraclofos). The recoveries ranged from 58.2% to 106.3% in blank samples spiked with 0.05, 0.1 and 0.2 mg/kg of 36 organophosphorus pesticides. The LODs, LOQs and the recoveries of the method all satisfy the requirement of pesticide residue analysis.