A simple thin-layer chromatographic method for the separation of D- and L-dansylamino acids using a new resolving agent is described. The enantiomeric resolution of racemates was accomplished on reversed-phase plates pre-treated with a poly-L-phenylalaninamide-copper(II) complex using water-acetonitrile mixtures as eluent under isocratic conditions. The polymeric ligand was easily prepared by reaction of the optically active amide with ethylene glycol diglycidyl ether at room temperature. The method is rapid and sensitive, and was successfully employed to resolve various dansylamino acids.