Counter-current chromatography (CCC) with a two-phase solvent system composed of n-hexane–ethyl acetate–methanol–water was applied to the isolation and purification of pheromones from ground beetles.One new and one known sex pheromones were obtained from the crude sample in a one-step separation.Their purities were determined by HPLC.The structures of these two compounds were identified by 1D and 2D NMR and MS means.Furthermore,the absolute configurations were determined by analysis of their CD spectrum.