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目的建立水中6种有机磷农药(敌敌畏、乐果、甲基对硫磷、马拉硫磷、毒死蜱、对硫磷)的固相膜萃取-气相色谱-串联质谱(GC-MS)测定方法。方法水样p H控制在3.0~7.0,经HLB固相萃取膜萃取后,用乙酸乙酯洗脱。采用DB-5MS毛细管柱分离,在选择离子扫描(SIM)模式下测定,外标法定量。结果在0.05~2.0 mg/L的线性范围内,所得6种有机磷农药的回归方程均呈较好的线性关系,r>0.998。方法的检出限为0.07~0.15μg/L,定量下限为0.25~0.40μg/L,平均回收率为87.2%~105.8%,RSD为2.1%~5.3%。结论该方法有机溶剂用量少,操作简便快速,灵敏度和准确度均较高,适用于水中6种有机磷农药污染物的测定。
Objective To establish a solid-phase membrane extraction-gas chromatography-tandem mass spectrometry (GC-MS) method for the determination of six organophosphorus pesticides (dichlorvos, dimethoate, parathion, malathion, chlorpyrifos and parathion) in water. Methods The pH of water sample was controlled at 3.0-7.0. After extraction by HLB solid phase extraction membrane, it was eluted with ethyl acetate. Using DB-5MS capillary column separation, in the selected ion scan (SIM) mode determination, external standard quantitative. Results The regression equation of the six organophosphorus pesticides showed good linearity within the linear range of 0.05-2.0 mg / L, r> 0.998. The detection limit was 0.07 ~ 0.15μg / L, the limit of quantification was 0.25 ~ 0.40μg / L, the average recovery was 87.2% ~ 105.8%, RSD was 2.1% ~ 5.3%. Conclusion This method has the advantages of less organic solvent, simple and quick operation, high sensitivity and accuracy, and is suitable for the determination of six kinds of organophosphorus pesticide contaminants in water.