建立超高效液相色谱-串联质谱测定复杂水质中25种全氟/多氟化合物(PFASs)含量的分析方法.样品经直接过滤、乙腈提取或固相萃取,用Agilent Eclipse Plus C18色谱柱分离,以含0.01%甲酸的甲醇溶液和水作为流动相,梯度洗脱,在电喷雾负离子模式下,采用多反应监测模式检测,用内标法定量.25种PFASs的质量浓度在0.5～100 μg/L范围内与色谱峰面积线性关系良好,相关系数均大于0.999,3种样品处理方法的检出限分别为0.06～0.20、0.002～0.006 μg/L和0.1～0.2 ng/L.样品加标平均回收率为69.9%～115%,测定结果的相对标准偏差为2.9%～19.6%(n=6).该方法简单快捷、重现性好、灵敏度较高,适用于氟化工园区污水、地表水和地下水中25种PFASs的测定.
Determination of 25 per-and polyfluoroalkyl substances in complex water by ultra high performance liquid chromatography-tandem mass spectrometry
A method of determination of 25 per-and polyfluoroalkyl substance(PFASs)in complex water by ultra high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)was established.The samples were subjected to directly filter,acetonitrile extraction or solid-phase extraction,and then separated by Agilent Eclipse Plus C18 with 0.01%formic acid methanol solution and water as the mobile phase for gradient elutionisation and determined by UPLC-MS/MS,in which negative electrospray ionization as well as multiple reaction monitoring mode was used in the detection,and quantified by internal standard method.The mass concentration of 25 PFASs had a good linear relationship with the chromatographic peak area in the range of 0.5-100 μg/L,the correlation coefficients were all more than 0.999,and the detection limit of direct injection,acetonitrile extraction and solid phase extraction were 0.06-0.20,0.002-0.006 μg/L and 0.1-0.2 ng/L,respectively.The average spiked recoveries of the samples were 69.9%-115%,and the relative standard deviations of the determination results were 2.9%-19.6%(n=6).The method is simple,rapid,reproducible,and sensitive,and it can meet the determination of 25 PFASs in fluorochemical industrial park sewage,surface water and groundwater.
per-and polyfluoroalkyl substancesultra high performance liquid chromatography-tandem mass spectrometrydirect injectionacetonitrile extractionsolid phase extraction
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维普
