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Silica-based monolithic column is typically synthesized by sol-gel processing and can be functionalized by means of siloxane bond to anchor the stationary inplace.One drawback of this approach is the poor hydrolytic stability of the bonded stationary phase.Vinyl-functionalized hybrid monolith prepared by incorporting vinyl-based co-precusor provides a viable platform for producing monolithic column with stationary bonded through a stable silicon-carbon bond and vinyl groups for further modifications.Calixarenes have emerged as attractive molecules for host-guest chemistry and have resulted in wide applications in varying areas, especially in separation science.Extensive studies on calixarene as the staionary phase for capillary elelctrochromatography were made by many researchers in the past a few years.And here we present the preparation and evaluation of calix-modified,vinyl-functionalized hybrid silica monolithic column for capillary electrochromatography for the first time.