Proton sponge-functionalized silica as high performance adsorbents for solid-phase extraction of trace perfluoroalkyl sulfonates in the environmental water samples and their direct analysis by MALDI-TOF-MS
Proton sponge-functionalized silica as high performance adsorbents for solid-phase extraction of trace perfluoroalkyl sulfonates in the environmental water samples and their direct analysis by MALDI-TOF-MS
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质子海绵功能化二氧化硅作为高性能吸附剂，用于固相萃取环境水样中的痕量全氟烷基磺酸盐并通过 MALDI-TOF-MS 直接分析。
DOI：
10.1039/c2an16190g
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发表时间：
2012-01-01
期刊：
影响因子：
4.2
通讯作者：
Zhou, Yiqi
中科院分区：
文献类型：
--
作者：
Cao, Dong;Hu, Ming;Zhou, Yiqi
将经典的质子海绵1，8-双二甲氨基萘（DMAN）功能化在硅胶颗粒上，制成一种新型固相萃取（SPE）吸附剂（DMAN@silica），用于萃取全氟烷基磺酸盐（PFSs）。在较宽的pH范围（3.0~8.5）内，PFSs的重现性高，提取能力强。1，8-双（四甲基胍基）萘（TMGN）溶液是一种质子海绵，其质子亲合性比DMAN高，可有效洗脱DMAN@SiO2吸附剂上的PFSs。以TMGN为基质，洗脱液可直接用MALDI-TOF-MS分析。由于未观察到基质离子干扰，因此获得了PFS的清晰质谱。提出了一种基于DMAN@silica-SPE富集、MALDI-TOF-MS分析的新方法，并应用于环境水样中PFSs的定量分析。每种目标分析物的校准曲线显示出宽的线性动态响应范围（全氟辛烷磺酸（PFOS）、全氟己基磺酸（PFHxS）和全氟丁基磺酸（PFBS）为0.1-10 ng L（-1）），超过2个数量级。全氟辛烷磺酸、全氟HxS和全氟BS的检测限分别为0.021、0.016和0.013纳克/升（-1）（S/N = 3）。在加标河水样本中，全氟辛烷磺酸、全氟硫化氢和全氟溴磺酸的回收率分别为92- 104%、95- 102%和98-109%。这些结果表明，所制备的DMAN@硅胶吸附剂能够有效地富集PFSs，所提出的方法是可靠的。
1,8-Bis(dimethylamino)naphthalene (DMAN), a classical 'proton sponge', was functionalized on silica particles as a novel solid-phase extraction (SPE) adsorbent (DMAN@silica) for extracting perfluoroalkyl sulfonates (PFSs). High reproducibility and excellent extraction capability for PFSs were obtained in a wide pH range (3.0~8.5). The adsorbed PFSs on DMAN@silica sorbents could be efficiently eluted by 1,8-bis(tetramethylguanidino)naphthalene (TMGN) solution which is a proton sponge with higher proton affinity than DMAN. The elution could be directly analyzed by MALDI-TOF-MS using TMGN as matrix. Clear mass spectra for the PFSs were obtained due to no matrix ions interference observed. Furthermore, a novel strategy based on the DMAN@silica-SPE enrichment, followed by MALDI-TOF-MS analysis, was proposed and applied for PFSs quantification in environmental water samples. The calibration curves of each of the target analytes showed a wide linear dynamic range of response (0.1-10 ng L(-1) for perfluorooctane sulfonate (PFOS), perfluorohexyl sulfonate (PFHxS) and perfluorobutylsulfonate (PFBS)), which were over 2 orders of magnitude. The detection limits for PFOS, PFHxS, and PFBS were 0.021, 0.016, and 0.013 ng L(-1), respectively (S/N = 3). Recoveries of PFOS, PFHxS, and PFBS are in the ranges of 92-104%, 95-102%, and 98-109% for spiked river water samples. These results indicated that the prepared DMAN@silica adsorbents could efficiently enrich PFSs and that the proposed method is reliable.