Institute of Food Safety and Environmental Monitoring, Fuzhou University, Fuzhou 350108, China.
J Chromatogr A. 2012 Oct 19;1260:174-82. doi: 10.1016/j.chroma.2012.08.053. Epub 2012 Aug 23.
A novel electroneutral and polar silica-based hybrid monolith was developed by an in situ copolymerization of 2-hydroxyethylmethacrylate (HEMA) and polyhedral oligomeric silsesquioxane methacryl substituted (POSS-MA), and successfully employed for hydrophilic interaction capillary electrochromatography (HI-CEC). A good mechanical stability of the prepared monolith was gained with the permeability decreasing from 6.52×10(-14) m2 to 4.61×10(-14) m2 when mobile phase changed from ACN to water. A significant cathodal EOF was obtained through attracting ions from the mobile phase despite the fact that it was devoid of ionizable functional groups on the surface of stationary phases, and a typical HI-CEC mechanism was achieved. The morphologies of the hybrid silica-based monolithic matrixes were observed, and the performance of this silica-based hybrid monolith was also investigated. Satisfactory column performances were carried out for both the neutral and charged analytes with HI-CEC. The analytes including uncharged amides and phenols, charged nucleic acid bases and nucleosides and enkephalins, were well separated with good peak symmetry. High separation efficiencies of charged alkaloids and enkephalins could get up to 145,000 plates/m and 75,000 plates/m, respectively.
一种新型的中性和极性的基于二氧化硅的杂化整体柱通过 2-羟乙基甲基丙烯酸酯(HEMA)和多面体低聚倍半硅氧烷甲基丙烯酰基取代物(POSS-MA)的原位共聚反应制备而成,并成功地应用于亲水相互作用毛细管电色谱(HI-CEC)。所制备的整体柱具有良好的机械稳定性,当流动相从 ACN 变为水时,渗透率从 6.52×10(-14) m2 降低到 4.61×10(-14) m2。尽管固定相表面没有可离子化的官能团,但通过从流动相中吸引离子,仍获得了明显的阴极电渗流,实现了典型的 HI-CEC 机制。观察了基于杂化二氧化硅的整体柱基质的形态,并研究了这种基于二氧化硅的杂化整体柱的性能。通过 HI-CEC 对中性和带电分析物进行了令人满意的柱性能测试。包括非带电酰胺和酚类、带电核酸碱基和核苷以及脑啡肽在内的分析物都得到了很好的分离,峰形对称。带电生物碱和脑啡肽的高分离效率分别可达 145,000 板/m 和 75,000 板/m。