固相萃取-超高效液相色谱-串联质谱法测定生活饮用水中11种全氟化合物

目的建立固相萃取-超高效液相色谱串联质谱(ultra performance liquid chromatography tandem mass spectrometry,UPLC-MS/MS)同时测定生活饮用水中11种全氟化合物的方法。方法采用WAX固相萃取柱对生活饮用水样品中的目标物进行富集净化,5 mL甲醇和7 mL 0.1%氨水-甲醇溶液洗脱,洗脱液用氮气吹至近干,30%(V/V)甲醇水溶液定容至1 mL,UPLC-MS/MS进行测定。结果11种目标分析物在0.5~50μg/L范围内具有良好的线性关系,方法检出限和定量限分别为0.03~0.7 ng/L和0.5~3.0 ng/L,低、中、高浓度加标回收率分别为90.0%~122.3%、87.1%~130.0%和80.0%~113.7%,相对标准偏差分别为1.95%~8.59%、1.27%~9.08%和2.17%~10.51%(n=6)。结论该方法线性范围宽,方法检出限和定量限低,适用于我国生活饮用水中11种全氟化合物的测定和监测。

Determination of 11 perfluorinated compounds in drinking water by solid phase extraction-ultra high performance liquid chromatography tandem mass spectrometry

OBJECTIVE To develop a method for the determination of 11 perfluorinated compounds(PFCs)in drinking water by solid phase extraction-ultra performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS).METHODS The target analytes in water samples were concentrated and purified by Oasis WAX SPE column and eluted with 5 mL methanol and 7 mL 0.1%ammonia-methanol solution.The eluent was blown to near dryness under a nitrogen gas,diluting with methanol water solution(3∶7,V/V)to 1 mL for analysis by UPLC-MS/MS.RESULTS There were good liner relationship in the range of 0.5-50μg/L.The detection limit and the limit of quantitation were 0.03-0.7 ng/L and 0.5-3.0 ng/L,respectively.The recoveries of 11 PFCs at three different spiked concentrations were 90.0%-122.3%,87.1%-130.0%and 80.0%-113.7%,respectively,and the relative standard deviation were 1.95%-8.59%,1.27%-9.08%and 2.17%-10.51%(n=6),respectively.CONCLUSION This method has wide linear range,low detection limit and limit of quantitation,applicable for simultaneous analysis and monitorting of 11 PFCs in drinking water.