A simple and general method suitable for the determination of cyclodextrin content in various matrices is described. The proposed method involves selective cleavage of C–C bonds with vicinal hydroxyl groups by means of periodate (Malaprades reaction). The amount of produced iodate is monitored by capillary electrophoresis. Optimized electrophoretic conditions (20 mM disodium tetraborate with 1 mM tetradecyltrimethylammonium bromide, direct UV detection λ