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Abstract: The novel enantiomeric separation of acidic and neutral compounds by capillary electrochromatography with beta-cyclodextrin-bonded positively charged polyacrylamide gels was examined. The columns used are capillaries filled with a positively charged polyacrylamide gel, a so-called monolithic stationary phase, to which allyl carbamoylated beta-CD derivatives covalently bind. The capillary mall was activated first by bifunctional reagent to make the resulting gel bind covalently inside the fused-silica tubing. Enantiomeric separations of sixteen acidic and two neutral compounds were achieved using the above-mentioned columns and 200 mmol dm(-3) Tris-300 mmol dm(-3) boric acid buffer (pH 8.1) as a mobile phase. High efficiencies of up to 150 000 plates m(-1) were obtained for dansyl-DL-amino acids. The within-run and between-run reproducibilities of retention time and separation factor were examined for three dansyl-DL-amino acids and warfarin. The relative standard deviations of the within-run and between-run reproducibilities of retention time were less than 1.2 and 1.3% over the six injections, respectively. Those of the separation factor were less than 0.3 and 0.2%, respectively. The gel- filled capillaries were stable for at least four months with intermittent use