Bartolomé Mónica, Gallego-Picó Alejandrina, Huetos Olga, Lucena Miguel Ángel, Castaño Argelia
Environmental Toxicology, National Centre for Environmental Health, Instituto de Salud Carlos III, Carretera Majadahonda-Pozuelo km 2, 28220, Majadahonda, Spain.
Department of Analytical Sciences, Faculty of Sciences, National University of Distance Education (UNED), 28040, Madrid, Spain.
Anal Bioanal Chem. 2016 Mar;408(8):2159-70. doi: 10.1007/s00216-016-9319-0. Epub 2016 Jan 20.
We have developed and validated an on-line TurboFlow solid-phase extraction procedure coupled to high-performance liquid chromatography with tandem mass spectrometry for the analysis of six perfluoroalkyl substances (PFAS), two sulfonates (perfluorooctane sulfonate and perfluorohexane sulfonate), three carboxylates (perfluorooctanoic acid, perfluorononanoic acid and perfluorodecanoic acid), and one sulfonamide (N-methylperfluorooctane sulfonamide), in human serum samples. This method requires only 100 μL of sample and involves a short pre-treatment with acetonitrile followed by addition of a labelled internal standard for quantification and ultracentrifugation. All PFAS were detected with a run time of 8.5 min. Linearity ranges stay between 0.1 and 20 μg L(-1) (R (2) > 0.9960). Recoveries were determined by spiking blank serum samples with a mixture of six PFAS and found to be in the range 96-110 % for all compounds. Isotopic dilution was used to quantify the selected analytes. The low limits of quantification obtained, between 0.16 and 0.34 μg L(-1), small volume of sample required and short run time used (from two to three times shorter than any other described method), make this validated method highly recommended for human biomonitoring studies.
我们开发并验证了一种在线TurboFlow固相萃取程序,该程序与高效液相色谱-串联质谱联用,用于分析人血清样品中的六种全氟烷基物质(PFAS)、两种磺酸盐(全氟辛烷磺酸和全氟己烷磺酸)、三种羧酸盐(全氟辛酸、全氟壬酸和全氟癸酸)以及一种磺酰胺(N-甲基全氟辛烷磺酰胺)。该方法仅需100 μL样品,先用乙腈进行简短预处理,然后添加标记内标进行定量和超速离心。所有PFAS在8.5分钟的运行时间内均可检测到。线性范围保持在0.1至20 μg L⁻¹之间(R²>0.9960)。通过向空白血清样品中加入六种PFAS的混合物来确定回收率,发现所有化合物的回收率在96%至110%之间。采用同位素稀释法定量选定的分析物。获得的低定量限在0.16至0.34 μg L⁻¹之间,所需样品体积小,运行时间短(比其他任何所述方法短两到三倍),使得这种经过验证的方法非常推荐用于人体生物监测研究。