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制备并表征基于乙烯基咪唑的聚合物整体固定相用于反相和亲水相互作用毛细管液相色谱。

Preparation and characterization of vinylimidazole-based polymer monolithic stationary phases for reversed-phase and hydrophilic interaction capillary liquid chromatography.

机构信息

Department of Chemistry, Soochow University, 70 Linhsi Road, Shihlin, 11102 Taipei, Taiwan.

Department of Chemistry, Soochow University, 70 Linhsi Road, Shihlin, 11102 Taipei, Taiwan.

出版信息

Talanta. 2018 Sep 1;187:73-82. doi: 10.1016/j.talanta.2018.05.013. Epub 2018 May 3.

Abstract

In this study, we applied 1-vinylimidazole (VIM) as the functional monomer to prepare a series of VIM-based monolithic stationary phases for both reversed-phase and hydrophilic interaction capillary liquid chromatography (LC) using various dimethacrylates (EDMA: ethylene dimethacrylate; HDDMA: 1,6-hexanediol dimethacrylate; DDDMA: 1,10-decanediol dimethacrylate) as cross-linkers. With a simple thermally initiated free-radical cross-linking polymerization process, VIM-based monolithic stationary phases have been successfully prepared. The porosity, permeability, and column efficiency of synthesized VIM-based monolithic stationary phases were characterized. With similar total porosity (85-90%), the VIM-HDDMA monoliths showed the lowest permeability among the three sets of VIM-based stationary phases. Various sets of non-polar (alkyl benzenes and polycyclic aromatic hydrocarbons) and polar analytes (phenol derivatives and amphenicol antibiotics) were applied as model compounds to further investigate the retention behavior of the VIM-based monolithic stationary phases for reversed-phase capillary LC analysis using selected VIM-based monolithic columns. While a mixture of organic acids was employed to perform HILIC analysis using the selected VIM-based monolithic columns. The separation selectivity and retention behavior of the VIM-based monolithic stationary phases were compared to those obtained using three previously prepared alkyl methacrylate-based monolithic columns. Strong retention and good resolution of polar analytes (such as phenol derivatives, amphenicol antibiotics, and organic acids) were observed using the selected VIM-based monolithic columns. The strong retention and good resolution might be attributed to the additional hydrogen-bonding between the hydrogen-donating analytes and the hydrogen-accepting imidazolium functionality on the VIM-based stationary phase. The applicability for both reversed-phase and HILIC capillary LC analysis has also been demonstrated using the selected VIM-based monolithic columns.

摘要

在这项研究中,我们应用 1-乙烯基咪唑(VIM)作为功能单体,使用各种二甲基丙烯酸酯(EDMA:乙二醇二甲基丙烯酸酯;HDDMA:1,6-己二醇二甲基丙烯酸酯;DDDMA:1,10-癸二醇二甲基丙烯酸酯)作为交联剂,为反相和亲水相互作用毛细管液相色谱(LC)制备了一系列基于 VIM 的整体固定相。通过简单的热引发自由基交联聚合过程,成功制备了基于 VIM 的整体固定相。合成的基于 VIM 的整体固定相的孔隙率、渗透性和柱效进行了表征。在三组基于 VIM 的固定相中,VIM-HDDMA 整体具有相似的总孔隙率(85-90%),但具有最低的渗透性。各种非极性(烷基苯和多环芳烃)和极性分析物(苯酚衍生物和安普青霉素抗生素)被用作模型化合物,进一步研究了 VIM 基整体固定相在反相毛细管 LC 分析中的保留行为,使用选定的 VIM 基整体柱。而使用选定的 VIM 基整体柱进行亲水相互作用分析时,采用了有机酸混合物。与之前制备的三种烷基甲基丙烯酸酯基整体柱相比,比较了 VIM 基整体固定相的分离选择性和保留行为。使用选定的 VIM 基整体柱观察到极性分析物(如苯酚衍生物、安普青霉素抗生素和有机酸)的强保留和良好的分辨率。强保留和良好的分辨率可能归因于供氢分析物与 VIM 基固定相上的氢键供体功能之间的额外氢键。使用选定的 VIM 基整体柱也证明了其在反相和 HILIC 毛细管 LC 分析中的适用性。

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