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目的建立液液萃取-超高液相色谱仪串联质谱对水样中全氟辛酸(Perfluorooctanoic Acid,PFOA)和全氟辛基磺酸(perfluorooctane sulfonate,PFOS)的分析方法。方法水中全氟化物以乙酸乙酯萃取,取有机相用氮气吹干,残渣用流动相定容至1.0 ml,0.22μm滤膜过滤后进超高液相色谱串联质谱分离分析。超高效液相色谱以C18柱为分离柱,以2mmol/L乙酸铵溶液和甲醇为流动相。质谱采用多反应监测模式,标准曲线法定量。结果方法的线性范围是0.2 ng/ml~100 ng/ml,全氟辛酸和全氟辛基磺酸的方法检出限为2.5 ng/L,PFOA和PFOS的水样加标回收率分别为70.0%~121%和95.8%~114%,方法精密度分别为11.7%和13.7%。结论该方法快速简单,灵敏准确,适用于水中PFOA和PFOS的测定。
Objective To establish a method for the determination of perfluorooctanoic acid (PFOA) and perfluorooctane sulfonate (PFOS) in water samples by liquid-liquid extraction coupled with ultra-high performance liquid chromatography. Methods The perfluorinated compounds in water were extracted with ethyl acetate. The organic phase was blown dry with nitrogen. The mobile phase was eluted with a volume of 1.0 ml. The filtrate was filtered through 0.22 μm membrane and analyzed by tandem mass spectrometry. Supercritical CO2 was separated on C18 column and 2mmol / L ammonium acetate solution and methanol as mobile phase. Mass spectrometry using multiple reaction monitoring mode, standard curve method. Results The linear range of the method was 0.2 ng / ml ~ 100 ng / ml. The detection limit was 2.5 ng / L with perfluorooctanoic acid and perfluorooctane sulfonic acid. The recovery rates of PFOA and PFOS were 70.0% 121% and 95.8% ~ 114% respectively. The precision of method was 11.7% and 13.7% respectively. Conclusion The method is rapid, simple, sensitive and accurate and is suitable for the determination of PFOA and PFOS in water.