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采用超高效液相色谱串联质谱技术建立了水样中11种全氟化合物的检测方法。方法以ACQUITY UPLC BEH C_(18)为分析柱,甲醇和2 mmoI/L 5%甲醇乙酸铵溶液为梯度淋洗液,全氟己酸、全氟庚酸、全氟辛酸、全氟壬酸、全氟癸酸、全氟十一烷酸、全氟十二烷酸、全氟十四烷酸、全氟辛烷磺酸、全氟己基磺酸钾和全氟丁基磺酸钾可以在6min内分离,外标法定量。采用固相萃取作为前处理方法,对比研究了两种淋洗液、3种洗脱液在不同pH值下的添加回收率。在试验条件下,所选取的全氟化合物的最低检测质量浓度为0.011～0.089pg/mL,这些化合物除全氟十四烷酸外,在水样中的平均回收率为72.6%～144.7%,相对标准偏差为1.2%～9.2%。实际样品的检测显示,全氟丁基磺酸钾、全氟辛酸与全氟辛烷磺酸在所测污水中质量浓度较高。
A method for the determination of eleven perfluorinated compounds in water samples was established by using ultra performance liquid chromatography tandem mass spectrometry. Methods The analytical column of ACQUITY UPLC BEH C_ (18) was used as the analytical column. The methanol and 2 mmoI / L 5% methanolic ammonium acetate solution were gradient eluent, perfluorohexanoic acid, perfluoroheptanoic acid, perfluorooctanoic acid, perfluorononanoic acid, perfluoro Capric acid, perfluoroundecanoic acid, perfluorododecanoic acid, perfluorotetradecanoic acid, perfluorooctane sulfonic acid, potassium perfluorohexane sulfonate, and potassium perfluorobutane sulfonate can be separated within 6 min , External standard method. Solid phase extraction (SPE) was used as a pretreatment method to compare the recoveries of two eluents and three eluents at different pH values. Under the experimental conditions, the minimum detectable concentration of perfluorinated compounds was 0.011 ~ 0.089pg / mL. The average recoveries of these compounds in water sample except perfluorotetradecanoic acid were 72.6% ~ 144.7% The relative standard deviation was 1.2% ~ 9.2%. Examination of the actual samples showed that potassium perfluorobutane sulfonate, perfluorooctanoic acid and perfluorooctane sulfonate had higher mass concentrations in the measured effluent.