固相萃取-气相色谱法测定葡萄酒中16种有机磷农药残留

Determination of 16 organophosphorous pesticide residues in grade wine by SPE-GC-FPD

利用固相萃取(SPE)/气相色谱火焰光度(GC-FPD)技术建立了葡萄酒中16种有机磷农药残留量分析方法。样品加水稀释,过HLB小柱和LC-NH2小柱净化,浓缩、定容后,用气相色谱测定,外标法定量。各农药的方法定量限(LOQ)均为为0.01 mg/kg。添加回收实验,16种有机磷农药添加浓度为0.01-0.10 mg/kg时,添加回收率为65.3-92.3%,变异系数≤10%。

A solid phase extraction （SPE）/flame photometric detector（GC- FPD ） gas chromatography spectrometry method was developed for 16 organophosphorous pesticide residues in grade wine. The organophosphorous pesticide residues were purified by HLB and LC-NH2,SPE columns, and detected by gas chromatography spectrometry （GC-FPD）. The method limit of quantification （LOQ） was 0.01 mg/kg for （Dichlorvos,Ethoprophos,Sulfotep,Phorate,Terbufos ,Monocrotophos,Fonofos, Posfolan-methyl, Phosphamidon, Parathion-methyl, Parathion, Isofenphos-methy, Phosfolan, Fenamiphos, Isazofhos, Coumaphos）. Fortified recovery was 65.3-92.3% when the spiked concentration was 0.01-0.10 mg/kg, the coefficient of variation were less than 10%.