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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 To reduce the harmful effects of extensive use of organic solvents on the environment and laboratory personnel in the process of detection, six kinds of organophosphorus pesticides (dichlorvos, dimethoate, chlorpyrifos, parathion, Methyl parathion, malathion) detection method. Methods A 1 000 ml water sample was taken and the SPE membrane was activated with ethyl acetate, methanol and ultrapure water separately using a membrane SPE. The membrane was again extracted with ethyl acetate, methylene chloride, ethyl acetate, (1 + 1, V / V). After drying over anhydrous sodium sulfate, the mixture was concentrated to 1.0 ml with a nitrogen blower. The sample was chromatographed on a medium polar capillary column (DB-1701, 30 m × 0.25 mm, ), Six kinds of organophosphorus compounds in drinking water and tap water were determined by temperature program, and quantified by Flame Photometric Detector (FPD). Results The results showed that the detection limits were 0.02μg / ml ~ 0.10μg / ml, the linear correlation coefficients were above 0.998 0, the relative standard deviations were in the range of 1% ~ 10% and the recoveries were in the range of 80% ~ 120% . Conclusion The method using less organic solvents, extraction time is shorter, and the method of high sensitivity, accurate, easy to operate, in line with the requirements of routine testing.