Preparation of Perphenylcarbamoylated 尾-Cyclodextrin-silica Hybrid Monolithic Column with 鈥淥ne-Pot鈥?Approach for Enantioseparation by Capillary Liquid Chromatography

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• 作者：Zhenbin Zhang ; Minghuo Wu ; Ren鈥檃n Wu ; Jing Dong ; Junjie Ou ; Hanfa Zou
• 刊名：Analytical Chemistry
• 出版年：2011
• 出版时间：May 1, 2011
• 年：2011
• 卷：83
• 期：9
• 页码：3616-3622
• 全文大小：885K
• 年卷期：v.83,no.9(May 1, 2011)
• ISSN：1520-6882

文摘

Perphenylcarbamoylated 尾-cyclodextrin-silica (Ph-尾-CD-silica) hybrid monolithic columns for enantioseparation in capillary liquid chromatography (cLC) have been prepared by a 鈥渙ne-pot鈥?approach via the polycondensation of alkoxysilanes and in situ copolymerization of mono (6^A-N-allylamino-6^A-deoxy)-Ph-尾-CD and vinyl group on the precondensed siloxanes. The morphologies of the Ph-尾-CD-silica hybrid monolithic columns were characterized by optical microscopy and scanning electron microscopy (SEM), showing the uniform monolithic matrixes tightly bonded onto the capillary wall. The content of Ph-尾-CD incorporated in monolithic matrix by the 鈥渙ne-pot鈥?approach was ca. 2.9 times higher than that by postmodification method. The permeability of the Ph-尾-CD-silica chiral hybrid monolithic column was 3.63 脳 10^鈭?4 m², and the minimum plate height was 12 渭m corresponding to 83鈥?00 theoretical plates/meter. Enantioseparations of 13 racemates were achieved by the Ph-尾-CD-silica hybrid monolithic column. In this work, since the prepolymerization system mainly consisted of organic solvent (methanol (MeOH), N,N-dimethylformamide (DMF)), the limitation and difficulty of the use of water insoluble organic monomers in the previously reported 鈥渙ne-pot鈥?method was circumvented. Therefore, various 尾-CD derivatives as well as other hydrophobic monomers could thus be used to prepare organic鈭抯ilica hybrid monolithic columns with the 鈥渙ne-pot鈥?process.