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用于磁场增强管内固相微萃取水中汞形态的任务特定整体柱,用于在线 HPLC 定量之前。

Task specific monolith for magnetic field-reinforced in-tube solid phase microextraction of mercury species in waters prior to online HPLC quantification.

机构信息

Key Laboratory of the Ministry of Education for Coastal and Wetland Ecosystems, Fujian Provincial Key Laboratory for Coastal Ecology and Environmental Studies, College of the Environment and Ecology, Xiamen University, Xiamen 361005, PR China.

College of Chemistry and Chemical Engineering, Xiamen University, Xiamen 361005, PR China.

出版信息

J Hazard Mater. 2021 Jun 5;411:125141. doi: 10.1016/j.jhazmat.2021.125141. Epub 2021 Jan 15.

Abstract

In this study, a novel sorbent based on task specific monolith doped with FeO was in situ fabricated in capillary and acted as the extraction medium of magnetic field-reinforced in-tube solid phase microextraction (MFR/IT-SPME) to trap and preconcentrate mercury species which were coordinated with dithizone to form chelates. Various characterization technologies evidenced that the obtained monolithic adsorbent presented porous and super paramagnetic properties, and possessed abundant functional groups. Results evidenced that the implementation of magnetic field during extraction stages enhanced the extraction efficiency of studied Hg chelates from 48.5% to 75.3% to 69.9-94.4%. Under the optimized extraction parameters, the introduced MFR/IT-SPME was online coupled to HPLC/DAD to quantify mercury species at ultra-trace levels in various water samples. Limits of detection varied from 0.0067 μg/L to 0.016 μg/L, and the RSDs for precision were below 7.5%. Additionally, related extraction mechanism was deduced and revealed multiple forces co-contributed to the enrichment. The reliability and accuracy of suggested online approach for speciation analysis of mercury was well proved by confirmatory experiments.

摘要

在这项研究中,一种新型的基于任务特异性整体的吸附剂被原位制备在毛细管中,并作为磁场增强管内固相微萃取(MFR/IT-SPME)的萃取介质,用于捕获和预浓缩与二硫腙配位形成螯合物的汞物种。各种特征化技术证明,所获得的整体吸附剂具有多孔和超顺磁性,并具有丰富的官能团。结果表明,在萃取阶段施加磁场可将研究的 Hg 螯合物的萃取效率从 48.5%提高到 75.3%至 69.9-94.4%。在优化的萃取参数下,引入的 MFR/IT-SPME 在线与 HPLC/DAD 耦合,用于在各种水样中超痕量水平定量测定汞形态。检出限范围为 0.0067μg/L 至 0.016μg/L,精密度的 RSD 低于 7.5%。此外,还推导了相关的萃取机制,揭示了多种力共同作用于富集。通过确证实验,证明了所提出的在线分析汞形态的方法的可靠性和准确性。

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