A silica monolithic column prepared by the sol-gel process for enantiomeric separation by capillary electrochromatography

• Published in: Electrophoresis Vol. 23; no. 7-8; pp. 1116 - 1120
• Main Authors: Kang, Jingwu, Wistuba, Dorothee, Schurig, Volker
• Format: Journal Article
• Language: English
• Published: Weinheim WILEY-VCH Verlag GmbH 01.04.2002; WILEY‐VCH Verlag GmbH
• Subjects: Capillary electrochromatography; Chromatography, Micellar Electrokinetic Capillary - instrumentation; Cyclodextrins - chemistry; Enantiomeric separation; Gels; Microscopy, Electron, Scanning; Molecular Structure; Monolithic column; Reproducibility of Results; Siloxanes - chemistry; Sol-gel process; Stereoisomerism
• ISSN: 0173-0835; 1522-2683
• DOI: 10.1002/1522-2683(200204)23:7/8<1116::AID-ELPS1116>3.0.CO;2-O

A method for the preparation of a silica monolithic capillary electrochromatography (CEC) column for the separation of enantiomers has been developed. The porous silica monolith was fabricated inside a fused‐silica capillary column by using the sol‐gel process. After gelation for 24 h, hydrothermal treatment at 100°C for 24 h was performed to prevent the sol‐gel matrix from cracking. The prepared monolith was then coated with Chirasil‐β‐Dex which represents a chiral polymer prepared by grafting permethyl‐β‐cyclodextrin to polymethylsiloxane with an octamethylene spacer. Immobilization of Chirasil‐β‐Dex was performed by heat treatment at 120°C for 48 h to give a nonextractable coating. The column performance was evaluated by using racemic hexobarbital as a model compound. The efficiency of 9.2×104 theoretical plates/m for the first eluted enantiomer of hexobarbital was obtained at an optimal flow rate of the mobile phase. The effect of mobile phase composition on enantiomeric separation of hexobarbital was also investigated. The column proved to be stable for more than one hundreds of runs during a two‐months period. The enantiomers of several neutral and negatively charged chiral compounds were baseline separated on this column.