This paper describes the development of a monolithic sol-gel column modified with l-hydroxyproline as a ligand exchange chiral stationary phase. It has been demonstrated that the monolithic chiral stationary phase can be used for the enantioseparation of dansyl amino acids, free amino acids, hydroxy acids, and dipeptides by capillary electrochromatography and micro-liquid chromatography. The recommended mobile phase was acetonitrile/0.50mM Cu(Ac) 2 -50mM NH 4 Ac (7:3) adjusted to pH 6.5. The characteristics of the monolithic column using hydroxyproline as chiral selector in CEC have been discussed.