固相萃取-液相色谱法分析环境水样中有机磷农药残留

SPE followed by HPLC for the sensitive determination of organic phosphorus pesticides in environmental water

提出环境水样中有机磷农药残留的固相萃取-液相色谱分析方法.水样用0.22μm水系膜过滤两次,C18固相萃取小柱分离富集,用乙腈洗脱目标物,洗脱液直接进行液相色谱分析.结果显示,工作曲线范围分别为甲基对硫磷2.0～80μg/L、杀螟硫磷3.0～80μg/L、对硫磷3.0～100μg/L、辛硫磷5.0～100μg/L、检测限(LOD)分别为甲基对硫磷0.11μg/L、杀螟硫磷0.52μg/L、对硫磷0.45μg/L、辛硫磷0.85μg/L.加标回收率在84.2%～102.2%范围内.该方法操作简单﹑快速﹑低成本﹑高回收率、富集效果好,适合于环境水样中有机磷农药残留的分析检测.

A solid-phase extraction(SPE) method followed by the high-performance liquid chromatography(HPLC) was established for the determination of organic phosphorus pesticides in environmental water samples.Water samples were filtered twice with 0.22 μm membrane.C18 solid phase extraction was used for the enrichment of organic phosphorus pesticides.The compounds were eluted by acetonitrile.The eluent was analyted by HPLC directly.The experimental results showed that the scope of the work curve of methyl parathion were 2.0-80 μg/L、 fenitrothion 3.0-80 μg/L、 parathion 3.0-100 μg/L、 phoxim 5.0-100 μg/L;the limit of detection(LOD) of methyl parathion,fenitrothion parathion phoxim were 0.11 μg/L、 0.52 μg/L、 0.45 μg/L、 0.85 μg/L,respectively.and recoveries were 84.2% 102.2%.The method is simple,fast,low-cost,high recovery rate and enrichment factor,and so it is suitable to the detection of organic phosphorus residues in environmental water samples.