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在硅胶球表面原位生长 COF-rLZU1 作为高效液相色谱的固定相。

In situ growth of COF-rLZU1 on the surface of silica sphere as stationary phase for high performance liquid chromatography.

机构信息

Shanghai Key Laboratory of Functional Materials Chemistry, School of Chemistry & Molecular Engineering, East China University of Science and Technology, Shanghai, 200237, PR China.

Shanghai Key Laboratory of Functional Materials Chemistry, School of Chemistry & Molecular Engineering, East China University of Science and Technology, Shanghai, 200237, PR China.

出版信息

Talanta. 2021 Jan 1;221:121612. doi: 10.1016/j.talanta.2020.121612. Epub 2020 Sep 2.

DOI:10.1016/j.talanta.2020.121612
PMID:33076142
Abstract

The composite materials consist of Covalent Organic Frameworks (COFs) and silica have been regarded as a kind of promising stationary phases due to combination of the large specific surface area and good mechanical strength of porous silica microspheres and the porous structure and the excellent stability of COFs. Herein, a novel COFs-silica composite (SiO@rLZU1, reduced Lan Zhou University-1) was prepared via an in-situ growth strategy with a 32 nm-thick COFs layer on the surface of silica and a 2.2 nm-thick COFs layer on the inner surface of the mesopores of spherical silica (5 μm, 120 Å). With secondary amine and phenyl groups, the novel stationary phase provided hydrophilic, hydrophobic and π-π interactions when used in HPLC, showing different selectivity from typical reversed-phase stationary phases. Probe molecules with aromatic moieties varying in polarity, including acidic (phenol, pyrocatechol, and pyrogallol), basic (aniline, 4-chloroaniline, and 4-nitroaniline) and neutral (benzene homologues) compounds, were all baseline separated on the SiO@rLZU1 column, indicating its excellent separation performance. Besides, the SiO@rLZU1 column also exhibited great repeatability with intraday RSDs of the retention time of three anilines less than 0.31% (n = 6) and peak area less than 1.63% (n = 6). On the SiO@rLZU1 column, satisfied results were achieved in the separation of real samples such as fullerenes and coking wastewater, suggesting the great potential of the as-synthesized stationary phase in HPLC applications.

摘要

复合材料由共价有机骨架(COFs)和二氧化硅组成,由于多孔二氧化硅微球的大比表面积和良好的机械强度以及 COFs 的多孔结构和优异的稳定性,因此被认为是一种很有前途的固定相。在此,通过原位生长策略制备了一种新型 COFs-二氧化硅复合材料(SiO@rLZU1,还原兰州大学-1),其表面有 32nm 厚的 COFs 层,多孔二氧化硅微球(5μm,120Å)的中孔内表面有 2.2nm 厚的 COFs 层。新型固定相具有仲胺和苯基,在 HPLC 中提供亲水性、疏水性和π-π相互作用,与典型的反相固定相表现出不同的选择性。具有不同极性芳基部分的探针分子,包括酸性(苯酚、邻苯二酚和焦儿茶酚)、碱性(苯胺、4-氯苯胺和 4-硝基苯胺)和中性(苯同系物)化合物,均在 SiO@rLZU1 柱上基线分离,表明其具有优异的分离性能。此外,SiO@rLZU1 柱还表现出良好的重复性,三个苯胺的保留时间日内 RSD 小于 0.31%(n=6),峰面积小于 1.63%(n=6)。在 SiO@rLZU1 柱上,对富勒烯和焦化废水等实际样品的分离也取得了满意的结果,表明所合成的固定相在 HPLC 应用中具有很大的潜力。

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