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目的为有效检测生活饮用水中的有机磷农药,建立一种大体积固相萃取毛细管柱气相色谱法。方法水样经装有C_(18)固相萃取小柱的大体积固相萃取仪,以二氯甲烷和乙酸乙酯分步提取、净化、洗脱,提取液经氮吹仪浓缩后,采用DB-1701石英毛细管柱(30 m×0.32 mm×0.25μm),火焰光度检测器(FPD)进行测定。结果敌敌畏、乐果、毒死蜱、甲基对硫磷、马拉硫磷、对硫磷6种农药在一定浓度范围内呈良好的线性关系(r=0.999),每种农药添加浓度为0.5μg/ml时,加标回收率为87.1%~103.1%,相对标准偏差(RSD)为4.7%~6.1%;每种农药添加浓度为1.0μg/ml时,加标回收率为90.5%~104.2%,相对标准偏差(RSD)为3.2%~6.0%。结论该方法快速、准确、灵敏、成本低,操作简便,能同时满足生活饮用水中6种有机磷农药检测的要求。
Objective To detect organophosphorus pesticides in drinking water effectively and establish a large-volume solid-phase extraction capillary gas chromatography. Methods The water samples were separated and purified by large volume solid phase extraction (SPE) with C_ (18) solid phase extraction cartridges and fractionated by dichloromethane and ethyl acetate. The extracts were concentrated by nitrogen blowing and concentrated DB-1701 quartz capillary column (30 m × 0.32 mm × 0.25 μm) and flame photometric detector (FPD). Results There was a good linear relationship between dichlorvos, dimethoate, chlorpyrifos, methyl parathion, malathion and parathion in a certain range of concentration (r = 0.999), and the concentration of each pesticide was 0.5 μg / ml, the recoveries ranged from 87.1% to 103.1% and the relative standard deviations (RSDs) ranged from 4.7% to 6.1%. The spiked recoveries ranged from 90.5% to 104.2% with 1.0μg / ml of each pesticide. The relative standard deviation (RSD) was 3.2% ~ 6.0%. Conclusion The method is rapid, accurate, sensitive, low cost and easy to operate. It can meet the requirements of testing 6 kinds of organophosphorus pesticides in drinking water at the same time.