Derivatization method for sensitive determination of fluorotelomer alcohols in sediment by liquid chromatography-electrospray tandem mass spectrometry

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• 作者：Hui Peng ; Kejun Hu ; Fanrong Zhao ; Jianying Hu ; ^{hujy@urban.pku.edu.cn}
• 关键词：Derivatization ; LC&ndash ; ESI-QTOF-MS ; CID-MS/MS ; Perfluorinated compounds ; Fluorotelomer alcohol
• 刊名：Journal of Chromatography A
• 出版年：2013
• 出版时间：3 May, 2013
• 年：2013
• 卷：1288
• 期：Complete
• 页码：48-53
• 全文大小：658 K

文摘

Fluorotelomer alcohols (FTOHs) are the main precursors of environmentally ubiquitous perfluorinated acids, and determination of FTOHs at low concentrations presents significant challenges. In this study, a new liquid chromatography-electrospray mass spectrometry (LC-ESI-MS) method in conjunction with low-energy collision dissociation tandem mass spectrometry (CID-MS/MS) was developed by employing an optimized derivatization reaction with dansyl chloride (DNS) in acetonitrile under catalysis of 4-(dimethylamino)-pyridine (DMAP). The instrument detection limits (IDLs) of the newly developed method were 0.014, 0.015, 0.014, 0.0075 and 0.0093 ¦Ìg/L for 4:2 FTOH, 6:2 FTOH, 8:2 FTOH, 10:1 FTOH and 10:2 FTOH respectively, which were 7.5-241 times lower than those without derivatizaiton and 57-357 times lower than previous GC/MS method. The method was successfully applied to analyze FTOHs in sediments combined with WAX and silica cartridges cleanup. The overall method recoveries were from 67 ¡À 6.0 % to 83 ¡À 9.4 % with matrix effects of <15 % . The limits of quantification for all FTOHs were 0.017-0.060 ng/g dry weight (dw). The method was applied to analyze six marine sediment samples from Liaodong Bay, China. All FTOHs except for 10:1 FTOH were detected, and the total concentrations of FTOHs were 0.19-0.52 ng/g dw. The developed method provides a new method to sensitively determine FTOHs in environmental matrices.