Development of a solid-phase extraction-HPLC/single quadrupole MS method for quantification of perfluorochemicals in whole blood
Development of a solid-phase extraction-HPLC/single quadrupole MS method for quantification of perfluorochemicals in whole blood
复制标题
DOI：
10.1021/ac049023c
复制
发表时间：
2005-02-01
影响因子：
7.4
通讯作者：
Lindström, G
中科院分区：
文献类型：
--
作者：
Kärrman, A;van Bavel, B;Lindström, G
建立了一种同时测定人全血中全氟辛烷磺酸（PFOS）和全氟辛酸（PFOA）以及10种密切相关的全氟化合物（PFCs）的方法。全氟辛烷磺酸和全氟辛酸用于各种用途，例如作为表面活性剂和塑料添加剂，由于其持久性，需要进行环境和健康研究。人体血液中PFCs数据的主要部分来自血清样本，主要通过离子对萃取、高效液相色谱（HPLC）和负电喷雾（ESI）串联质谱（MS/MS）进行分析。本文开发的分析方法适用于人全血，包括固相萃取（SPE）和HPLC负电喷雾单四极杆质谱（HPLC/ES-MS）。用甲酸处理全血等分试样，并在十八烷基（C18）SPE柱上提取。用甲醇分离PFCs，以全氟庚酸为内标，单四极杆质谱法进行定量。在0.3-194 ng/mL范围内进行了验证，回收率为64 - 112%，研究的12种PFC中有11种的检测限为0.1-0.5 ng/mL。我们采用这种方法收集了20全血样本，1997-2000年从瑞典人口在24-72岁。检测到12种PFCs中的11种，并使用三重四极杆LC/MS/MS分析对其进行定量和定性确认。对所有样本中的全氟辛烷磺酸、全氟辛烷磺酰胺、全氟己烷磺酸、全氟辛酸和全氟壬酸进行了定量。此外，在一些样品中检测到全氟己酸、全氟癸酸、全氟癸磺酸盐、全氟十一烷酸、全氟十二烷酸和全氟十四烷酸。本研究表明，固相萃取和单四极杆质谱可用于提取和定量人全血中的PFCs，导致选择性和低检测限。
A method for the determination of perfluorooctane-sulfonate (PFOS) and perfluorooctanoic acid (PFOA) simultaneously with 10 closely related perfluorochemicals (PFCs) in human whole blood was developed and validated. PFOS and PFOA are used in various applications, for example, as surfactants and plastic additives, and are subject to environmental and health research due to their persistence. The main part of the data on PFCs in human blood is from serum samples, analyzed mainly by ion pair extraction followed by high-performance liquid chromatography (HPLC) and negative electrospray (ESI) tandem mass spectrometry (MS/MS). The analytical method developed here is suitable for human whole blood and involves solid-phase extraction (SPE) and HPLC negative electrospray single quadrupole mass spectrometry (HPLC/ES-MS). A whole blood aliquot was treated with formic acid and extracted on a octadecyl (C18) SPE column. The PFCs were isolated with methanol, and quantification was performed using single quadrupole mass spectrometry and perfluoroheptanoic acid as internal standard. Validation was performed in the range 0.3-194 ng/mL with recovery between 64 and 112% and limit of detection in the 0.1-0.5 ng/mL range for 11 of the 12 PFCs studied. We applied this method to 20 whole blood samples collected in 1997-2000 from the Swedish population in the ages 24-72. Eleven of the 12 PFCs were detected, and they were quantitatively and qualitatively confirmed using triple quadrupole LC/MS/MS analysis. PFOS, perfluorooctanesulfonamide, perfluorohexanesulfonate, PFOA and perfluorononanoic acid were quantified in all samples. In addition, perfluorohexanoic acid, perfluorodecanoic acid, perfluorodecanesulfonate, perfluoroundecanoic acid, perfluorododecanoic acid, and perfluorotetradecanoic acid were detected in some samples. This study shows that SPE and single quadrupole MS can be applied for extraction and quantification of PFCs in human whole blood, resulting in selectivity and low detection limits.