Department of Environmental and Pharmaceutical Sciences, Graduate School of Biomedical Sciences, Nagasaki University, Nagasaki 852-8521, Japan.
J Chromatogr A. 2010 Feb 26;1217(9):1501-5. doi: 10.1016/j.chroma.2009.12.056. Epub 2010 Jan 4.
An adamantyl (ADM)-functionalized monolithic stationary phase was newly synthesized by a single-step copolymerization of 1-adamantyl-(alpha-trifluoromethyl) acrylate, ethylene dimethacrylate, and 2-acrylamido-2-methyl-1-propanesulfonic acid in order to prevent the peak tailing of basic solutes in capillary electrochromatography and was compared with butyl methacrylate (BMA)-based one. The ADM structure shields the negatively charged groups on the surface of monolith from basic solutes, resulting in better peak shapes than BMA-based monolithic stationary phase. As the monomers ratio decreased, the monolithic column had lower retention and higher column efficiency which was likely due to lower phase ratio and smaller globule size of monolith, respectively. The ADM-functionalized monolithic columns exhibited a good repeatability and reproducibility of column preparation with relative standard deviation values below 9% in the studied chromatographic parameters.
为了防止毛细管电色谱中碱性溶质的峰拖尾,通过 1-金刚烷基-(α-三氟甲基)丙烯酸酯、乙二醇二甲基丙烯酸酯和 2-丙烯酰胺基-2-甲基-1-丙磺酸的一步共聚反应,新合成了一种金刚烷基(ADM)功能化整体固定相,并将其与基于丁基甲基丙烯酸酯(BMA)的固定相进行了比较。ADM 结构可以防止整体固定相表面上带负电荷的基团与碱性溶质相互作用,从而获得比基于 BMA 的整体固定相更好的峰形。随着单体比例的降低,整体柱的保留时间降低,柱效率提高,这可能分别归因于较低的相比和较小的整体珠粒尺寸。ADM 功能化整体柱在研究的色谱参数中表现出良好的柱制备重现性和重现性,相对标准偏差值低于 9%。