Measurement of 18 perfluorinated organic acids and amides in human serum using on-line solid-phase extraction
Measurement of 18 perfluorinated organic acids and amides in human serum using on-line solid-phase extraction
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DOI：
10.1021/ac050671l
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发表时间：
2005-09-15
影响因子：
7.4
通讯作者：
Calafat, AM
中科院分区：
文献类型：
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作者：
Kuklenyik, Z;Needham, LL;Calafat, AM
建立了一种在线固相萃取-高效液相色谱-串联质谱联用（SPE/MS/ MS）测定血清中痕量18种全氟化合物（3种全氟磺酸盐、8种全氟羧酸盐、7种全氟磺酰胺）的方法。在没有蛋白沉淀的情况下，仅用0.1 M甲酸稀释，将100 μ L血清的一个等分试样进样到商业柱切换系统中，该系统允许同时进行SPE和HPLC-MS/MS采集。首先，分析物在C18 SPE柱上浓缩。然后，将该柱自动置于C8分析HPLC柱前，用于分析物的色谱分离。使用负离子TurbolonSpray电离，电喷雾电离，MS/MS的变体进行检测和定量。所有分析物，包括挥发性磺酰胺衍生物，在使用传统的离线SPE方法之前无法确定，实现了良好的回收率。使用小样品体积（100 μ L血清）和同位素稀释定量的高通量和低检测限（0.05-0.8 ng/mL）使该方法适用于大规模流行病学研究。
We have developed an on-line solid-phase extraction (SPE) method coupled to high-performance liquid chromatography (HPLC)-tandem mass spectrometry (MS/ MS) for measuring trace levels of 18 perfluorinated chemicals (3 perfluorosulfonates, 8 perfluorocarboxylates, 7 perfluorosulfonamides) in serum. Without protein precipitation, only dilution with 0.1 M formic acid, one aliquot of 100 mu L of serum was injected into a commercial column switching system that allowed for concurrent SPE and HPLC-MS/MS acquisition. First, the analytes were concentrated on a C18 SPE column. Then, this column was placed automatically in front of a C8 analytic HPLC column for chromatographic separation of the analytes. Detection and quantification were done using negative-ion TurbolonSpray ionization, a variant of electrospray ionization, MS/MS. Excellent recovery was achieved for all analytes including the volatile sulfonamide derivatives that could not be determined before using traditional offline SPE methods. The high throughput and low limits of detection (0.05-0.8 ng/mL) using a small sample volume (100 mu L of serum) and isotope dilution quantification make this method suitable for large-scale epidemiologic studies.