固相萃取富集净化-高效液相色谱串联质谱法测定饮用水中全氟化合物

目的建立固相萃取浓缩与高效液相色谱串联质谱法(HPLC-MS/MS)测定饮用水中全氟辛酸(PFOA)、全氟辛烷磺酸(PFOS)、全氟癸酸(PFDA)等全氟化合物的方法。方法样品经C18固相萃取浓缩净化,应用负离子电喷雾电离,检测方式为多级反应离子监测(MRM)模式,高效液相色谱串联质谱法(HPLC-MS/MS)进行测定。结果PFOA、PFOS、PFDA在50~1000pg/ml线性范围内,线性相关系数均>0.99。在8、20.0pg/g添加水平的回收率为65%~111%,相对标准偏差为3.6%~14.6%(n=6),定量检出限为8pg/g。结论该法适用于饮用水中PFOA、PFOS、PFDA等全氟化合物的测定,具有快速、定量准确、检测灵敏等优点。

A method of perfluorinated organic compounds in drinking water determinated by HPLC-MS/MS

Objective To establish a method of perfluorinated organic compounds(POCs) in drinking water determinated by HPLC-MS/MS.Methods The contents of selected POCs (i.e., perfluorooctanesulfonate (PFOS), perfluorooctanoate (PFOA) and perfluorodecanoate (PFDA)) in water samples were extracted by the C_ 18 solid-phase extraction (SPE). The extraction samples were then identified and quantitated by high performance liquid chromatography-negative electrospray mass spectrometry (HPLC-ESI-MS/MS). Results Linear calibration curves were obtained at the concentration ranges from 50pg/ml to 1000 pg/ml(the correlation coefficients were above 0.99).The average recoveries for PFOA,PFOS and PFDA spiked in water ranged from 65 to 111% and their relative standard were between 3.6% and 14.6%.The limit of quantification (LOQ) of the method was 8pg/g. Conclusion The method for determination of POCs in drinking water could be simple, sensitive and accurate.