超高效液相色谱-串联质谱法测定水中全氟辛酸和全氟辛基磺酸

Determination of Perfluorooctanoic Acid and Perfluorooctane Sulfonate in Water by Ultra High Performance Liquid Chromatography Tandem Mass Spectrometry

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 develop a liquid-liquid extraction（ LLE）-ultra high performance liquid chromatography/tandem mass spectrometry（ UPLC-MS/MS） method for the determination of perfluorooctanoic acid（ PFOA） and perfluorooctane sulfonate（ PFOS）. Methods PFOA and PFOS were extracted with ethyl acetate. The organic phase was concentrated to near dryness with nitrogen stream and the residue was dissolved in the mobile phase. After being filtered through a 0. 22 μm millipore filter,the filtrate was injected into UPLC-MS/MS for analysis. The separation of PFOA and PFOS was performed on a C18 column with gradient elution using methanol and 2 mmol/L ammonium acetate as mobile phases. Multiple reaction monitoring（ MRM）technique was used for tandem mass analysis and the calibration curve was plotted for quantitative analysis.Results Good linearity of PFOA and PFOS was obtained in the range of 0. 2-100 ng/ml. The detection limits of the method for PFOA and PFOS were 2. 5 ng/L. The average recoveries of PFOA and PFOS were 70. 0%-121% and 95. 8%-114%,respectively. The relative standard deviations of PFOA and PFOS were 11. 7% and 13. 7%. Conclusion The method is rapid,easy,accurate and sensitive and can be applied for determination of PFOA and PFOS.