School of Pharmacy, Shenyang Pharmaceutical University, Wenhua Road 103, Shenyang, Liaoning Province, PR China.
School of Applied Chemistry, Shenyang University of Chemical Technology, Shenyang, Liaoning Province, PR China.
J Chromatogr A. 2020 Jun 7;1620:460932. doi: 10.1016/j.chroma.2020.460932. Epub 2020 Jan 28.
Although various cyclodextrins (CDs) have been utilized to prepare organic polymer-based monolithic columns, there were few reports on fabrication of cyclodextrin functionalized hybrid monolithic columns. Herein, a sulfobutylether β-cyclodextrin (SBE-β-CD)-silica hybrid monolithic column was prepared by "one-step" method via the co-polymerization of hydrolyzed organosiloxane precursors and glycidyl methacrylate-sulfobutylether β-cyclodextrin (GMA-SBE-β-CD). The morphologies of prepared monolithic columns were observed by optical microscopy and scanning electron microscopy (SEM). The sulfobutylether β-cyclodextrin was incorporated into the polymeric structure, which was demonstrated by energy dispersive X-ray spectroscopy (EDS), Fourier-transform infrared spectroscopy (FTIR) spectrum and X-ray photoelectron spectroscopy (XPS). The resulting columns were used for chiral separations of twenty six racemic compounds, and satisfactory separation selectivity was obtained. Compared with other two kinds of neutral cyclodextrin (β-CD and HP-β-CD) based hybrid monoliths, sulfobutylether β-cyclodextrin-silica hybrid monolith showed superior chiral resolution. These results demonstrated the sulfobutylether β-cyclodextrin-silica hybrid monolithic column was promising in chiral compounds analysis.
尽管已经使用了各种环糊精(CDs)来制备有机聚合物基整体柱,但关于制备环糊精功能化杂化整体柱的报道却很少。本文通过水解有机硅氧烷前体与甲基丙烯酸缩水甘油酯-磺丁基-β-环糊精(GMA-SBE-β-CD)的共聚反应,采用“一步法”制备了磺丁醚-β-环糊精(SBE-β-CD)-硅胶杂化整体柱。通过光学显微镜和扫描电子显微镜(SEM)观察了制备的整体柱的形貌。通过能量色散 X 射线光谱(EDS)、傅里叶变换红外光谱(FTIR)谱和 X 射线光电子能谱(XPS)证明了磺丁醚-β-环糊精被掺入聚合物结构中。所得柱用于手性拆分 26 种外消旋化合物,得到了满意的分离选择性。与其他两种中性环糊精(β-CD 和 HP-β-CD)基杂化整体柱相比,磺丁醚-β-环糊精-硅胶杂化整体柱显示出更高的手性分辨率。这些结果表明磺丁醚-β-环糊精-硅胶杂化整体柱在手性化合物分析中具有广阔的应用前景。