摘要
目的为减少检测过程中大量使用有机溶剂对环境和实验人员的危害,建立膜固相萃取-毛细管气相色谱测定饮用水及水源水中6种有机磷农药(敌敌畏、乐果、毒死蜱、对硫磷、甲基对硫磷、马拉硫磷)的检测方法。方法取1 000 ml水样,采用膜固相萃取仪,分别用乙酸乙酯、甲醇、超纯水对固相萃取膜进行活化,再分别用乙酸乙酯、二氯甲烷、乙酸乙酯与二氯甲烷(1+1,V/V)进行洗脱,加无水硫酸钠干燥后用氮吹仪浓缩至1.0 ml,采用中等极性毛细柱(DB-1701,30 m×0.25 mm,0.25μm),以程序升温的方式,测定饮用水及水源水中的6种有机磷化合物,以火焰光度检测器(FPD)定量。结果 6种有机磷农药分离良好,方法检出限为0.02μg/ml^0.10μg/ml,线性相关系数在0.998 0以上,相对标准偏差在1%~10%,回收率在80%~120%。结论该方法使用有机溶剂较少,萃取时间较短,且方法灵敏度高,准确,操作简便,符合日常检测的要求。
Objective In order to reduce the harms to the environment and laboratory technician due to the use of a large amount of organic solvent in the process of examination,a membrane solid phase extract-capillary gas chromatography method was built up to determine 6 kinds of organic phosphorus pesticide（ DDVP,dimethoate,chlorpyrifos,parathion,methyl-parathion and malathion） in the drinking water and water source. Methods 1 000 ml water sample was taken and the membrane solid phase extraction（ MSPE） apparatus was adopted. Solid phase extraction membrane was activated by ethyl acetate,methanol and ultrapure water respectively. And then it was once again eluted by using ethyl acetate,dichloromethane,ethyl acetate ＋dichloromethane（ 1∶1,V/V）. Finally,anhydrous sodium-sulphate was added in the sample which was then dried up and concentrated to 1. 0 ml with nitrogen-blowing device. Medium-polar capillary column（ DB 1701,30 m × 0. 25 mm,0. 25 μm）was used to determine the 6 kinds of organic phosphorus as contained in the drinking water and the water-source through temperature-programmed route. The result was quantified by flame photometric detector（ FPD）. Results Six kinds of organic phosphorus pesticide were well separated. The examining limitation was within 0. 02 μg/ml-0. 10 μg/ml,the linear relative coefficients were greater than 0. 998 0,and the relative standard deviation was within 1%-10%,with the recovery rate of80%-120%. Conclusion The method used less organic solvent,shorter time for the extraction,but had a high sensitivity,accuracy and easy operation. The method can meet the requirement of the daily examination.
出处
《中国卫生检验杂志》
CAS
2017年第21期3065-3067,共3页
Chinese Journal of Health Laboratory Technology
关键词
有机磷
水
气相色谱
膜萃取
Organic phosphorus
Water
Gas chromatography
Membrane solid phase extraction
