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Fe3O4@C@PANI 磁性微球的制备及其用于水样中酚类化合物的气相色谱-质谱分析。

Preparation of Fe3O4@C@PANI magnetic microspheres for the extraction and analysis of phenolic compounds in water samples by gas chromatography-mass spectrometry.

机构信息

Department of Chemistry, Fudan University, Shanghai, China.

出版信息

J Chromatogr A. 2011 May 20;1218(20):2841-7. doi: 10.1016/j.chroma.2011.03.044. Epub 2011 Apr 12.

Abstract

In this work, core-shell structure Fe(3)O(4)@C@polyaniline magnetic microspheres were synthesized using simple hydrothermal reactions. The carbon-coated magnetic microspheres (Fe(3)O(4)@C) were first synthesized by a hydrothermal reaction, and then aniline was polymerized on the magnetic core via another hydrothermal reaction. Then, the obtained Fe(3)O(4)@C@polyaniline magnetic microspheres were applied as magnetic adsorbents for the extraction of aromatic molecules due to π-π interactions between polyaniline shell and aromatic compounds. In our study, five kinds of phenols including phenol, 2,4-dichlorophenol (DCP), 2,4,5-trichlorophenol (TCP), pentachlorophenol (PCP) and bisphenol A (BPA) were selected as the model analytes to verify the extraction ability of Fe(3)O(4)@C@PANI microspheres. After derivatization, the phenols were detected using gas chromatography-mass spectrometry (GC-MS). The dominant parameters affecting enrichment efficiency were investigated and optimized. Under the optimal conditions, the proposed method was evaluated, and applied to the analysis of phenols in real water samples. The results demonstrated that our proposed method based on Fe(3)O(4)@C@polyaniline magnetic microspheres had good linearity (r(2)>0.991), and limits of quantification (2.52-29.7 ng/mL), high repeatability (RSD<13.1%) and good recovery (85.3-110.6%).

摘要

在这项工作中,使用简单的水热反应合成了核壳结构的 Fe(3)O(4)@C@聚苯胺磁性微球。首先通过水热反应合成了碳包覆磁性微球(Fe(3)O(4)@C),然后通过另一个水热反应在磁性核上聚合苯胺。然后,由于聚苯胺壳与芳香族化合物之间的π-π相互作用,将得到的 Fe(3)O(4)@C@聚苯胺磁性微球用作芳香族分子的磁性吸附剂。在我们的研究中,选择了五种酚类化合物,包括苯酚、2,4-二氯苯酚(DCP)、2,4,5-三氯苯酚(TCP)、五氯苯酚(PCP)和双酚 A(BPA)作为模型分析物,以验证 Fe(3)O(4)@C@PANI 微球的萃取能力。衍生化后,使用气相色谱-质谱联用仪(GC-MS)检测酚类化合物。研究并优化了影响富集效率的主要参数。在最佳条件下,对所提出的方法进行了评估,并应用于实际水样中酚类化合物的分析。结果表明,基于 Fe(3)O(4)@C@聚苯胺磁性微球的我们提出的方法具有良好的线性(r(2)>0.991)、定量限(2.52-29.7 ng/mL)、高重复性(RSD<13.1%)和良好的回收率(85.3-110.6%)。

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