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As the most popular chiral selectors, β-cyclodextrin (β-CD) and its derivatives have been widely used in enantiomer separations. Among functionalized β-CDs, sulfated β-CDs are recognized as the most effective chiral additives in capillary electrophoresis (CE) separations. Herein, we describe the preparation of a novel sulfated poly β-CD-modified silica-based monolithic column and its use for the enantioseparation of some chiral compounds in the capillary electrochromatography (CEC) mode.