Department of Chemistry, Soochow University, Taipei, Taiwan.
J Chromatogr A. 2013 Jul 12;1298:35-43. doi: 10.1016/j.chroma.2013.05.003. Epub 2013 May 10.
Due to the high porosity, good thermal stability, and good physical stability at high pressure, polymer monoliths have been successfully utilized as the stationary phases for capillary liquid chromatography (LC) analysis. In this study, we introduced 1,6-hexanediol ethoxylate diacrylate (HEDA) as a cross-linker to prepare alkyl methacrylate monoliths for efficient separation of polar small molecules. HEDA provided additional dipole-dipole interactions between the monolithic stationary phases and polar analytes. For comparison, ethylene dimethacrylate and 1,6-hexanediol dimethacrylate were also utilized as cross-linkers to prepare alkyl methacrylate monoliths. A series of alkyl methacrylate polymeric monoliths were synthesized in fused-silica capillaries using the three different cross-linkers. The porosity, permeability and column efficiency of the synthesized alkyl methacrylate monoliths were characterized. A mixture of phenol derivatives was employed to evaluate the applicability of the prepared monolithic columns for separating small molecules using capillary LC. The HEDA-based alkyl methacrylate monoliths offered the most efficient chromatographic separation for phenol derivatives. Moreover, the capability of applying the novel HEDA-based alkyl methacrylate monolithic columns for potential environmental analysis was demonstrated by separating eight phenylurea herbicides.
由于高孔隙率、良好的热稳定性和高压下的良好物理稳定性,聚合物整体柱已成功用作毛细管液相色谱(LC)分析的固定相。在这项研究中,我们引入 1,6-己二醇乙氧基二丙烯酸酯(HEDA)作为交联剂,制备用于高效分离极性小分子的甲基丙烯酸酯整体柱。HEDA 提供了整体固定相和极性分析物之间额外的偶极-偶极相互作用。为了进行比较,还使用了二乙二醇二甲基丙烯酸酯和 1,6-己二醇二甲基丙烯酸酯作为交联剂来制备甲基丙烯酸酯整体柱。使用三种不同的交联剂在熔融石英毛细管中合成了一系列甲基丙烯酸酯聚合物整体柱。对合成的甲基丙烯酸酯整体柱的孔隙率、渗透性和柱效进行了表征。采用苯酚衍生物混合物评估了所制备的整体柱在使用毛细管 LC 分离小分子方面的适用性。基于 HEDA 的甲基丙烯酸酯整体柱对苯酚衍生物提供了最有效的色谱分离。此外,通过分离八种苯脲类除草剂,证明了新型基于 HEDA 的甲基丙烯酸酯整体柱在潜在环境分析中的应用能力。