Citation: LIU Xiao-Lei, LIU Jie, GUO Rui, ZHAO Xing-Ru, SHEN Jin-Shan. Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry for Determination of Per-and Polyfluorinated Compounds in Surface Water. Chinese Journal of Analytical Chemistry, 2018, 46(9): 1400-1407. doi: 10.11895/j.issn.0253-3820.171373 [复制]
Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry for Determination of Per-and Polyfluorinated Compounds in Surface Water
建立了固相萃取-超高效液相色谱-串联质谱（SPE-UPLC-MS/MS）同时测定水中全氟烷基羧酸（PFCAs）、全氟烷基磺酸（PFSAs）、全氟烷基膦酸（PFPAs）、全氟烷基次膦酸（PFPis）和多氟烷基膦酸二酯（diPAPs）等23种全氟及多氟化合物的分析方法。固相萃取柱WAX柱依次用6 mL甲醇（含1%（V/V）NH4OH）、12 mL甲醇和12 mL超纯水活化，上样后，用6 mL乙腈（含0.5%（V/V）NH4OH）、6 mL甲醇（含1%（V/V）NH4OH）和6 mL乙腈（含1%（V/V）NH4OH）洗脱。样品萃取液分为3份，一份用于分析PFCAs和PFSAs，溶液组成为等体积萃取液与超纯水；一份用于分析PFPAs，溶液组成为等体积萃取液与25 mmol/L四丁基硫酸氢铵；另一份用于分析PFPis和diPAPs，溶液组成为甲醇。结果表明，水中23种全氟及多氟化合物平均加标回收率为55%~125%，相对标准偏差为0.3%~15.0%，方法检出限和定量限分别为0.003~0.215 ng/L和0.010~0.714 ng/L。本方法简便、灵敏度高、重现性好，适用于同时检测水中多类全氟及多氟化合物。
A method for simultaneous determination of perfluoroalkyl carboxylic acids (PFCAs), perfluoroalkyl sulfonic acids (PFSAs), perfluoroalkyl phosphonic acids (PFPAs), perfluoroalkyl phosphinic acids (PFPis) and polyfluoroalkyl phosphoric acid diesters (diPAPs) from water by solid phase extraction-ultra performance liquid chromatography-tandem mass spectrometry (SPE-UPLC-MS/MS) was established. During solid phase extraction process, 6 mL of ammonia-methanol (1.0%, V/V), 12 mL of methanol, 12 mL of ultrapure water were used to activate the WAX cartridges. After sample loading, the cartridges were eluted with 6 mL of ammonia-acetonitrile (0.5%, V/V), 6 mL of ammonia-methanol (1.0%, V/V) and 6 mL ammonia-acetonitrile (1.0%, V/V). Before instrumental analysis, the sample extract was divided into three parts. For the PFCAs and PFSAs, equal parts of ultrapure water were added to the extract. For the PFPAs, equal parts of 25 mmol/L of tetra-butyl ammonium sulfate were added to the extract. For the PFPis and diPAPs, the solution was methanol. The results showed that the recoveries of target compounds were between 55%-125% with relative standard deviation varying from 0.30% to 15%. Method detection limit and quantitative limit were 0.003-0.215 ng/L and 0.01-0.714 ng/L, respectively. This method was simple with high sensitivity and good reproducibility, and suitable for simultaneous determination of five kinds of per-and polyfluorinated substances in water.
EPA 800-F-16-003, Fact Sheet:PFOA and PFOS Drinking Water Health Advisories. Environmental Protection Agency of U.S.