Journal of chromatography. A 2014-09-05

Single-step approach for fabrication of vancomycin-bonded silica monolith as chiral stationary phase.

Ming-Lung Hsieh, Lai-Kwan Chau, Yung-Son Hon

Index: J. Chromatogr. A. 1358 , 208-16, (2014)

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Abstract

A vancomycin-bonded silica monolithic column for capillary electrochromatography (CEC) was prepared by a single-step in situ sol-gel approach. This sol-gel process incorporates a synthetic sol-gel precursor which contains a macrocyclic antibiotic, vancomycin, to form a porous silica network inside a fused-silica capillary. To avoid degradation of vancomycin during the column fabrication, a mild step was adopted into the sol-gel process. The performance of the vancomycin chiral stationary phase was investigated by CEC in both the reversed-phase mode and the normal-phase mode. The vancomycin chiral stationary phase was optimized with respect to vancomycin loading in the reversed-phase mode for chiral separation of thalidomide enantiomers. The best efficiency and resolution values of 94600plates/m and 5.79, respectively, were achieved. The optimized column was further applied to chiral separation of alprenolol enantiomers. A plate height of less than 7μm for the first eluted enantiomer of alprenolol was obtained in an aqueous mobile phase at a flow rate of 0.74mm/s. Using enantiomers of seven β-blockers and some other basic enantiomers as test analytes, separation efficiencies of up to 148100plates/m in the reversed-phase mode and up to 138100plates/m in the normal-phase mode were achieved. Copyright © 2014 Elsevier B.V. All rights reserved.