A preparative high-speed counter-current chromatography (HSCCC) method was successfully used for isolation of two new minor compounds--alsaticol and alsaticocoumarin A. A two-phase solvent system composed of n-hexane-ethyl acetate-methanol-water (1:1:1:1) was developed. Compounds were obtained from the dichloromethane extract of Peucedanum alsaticum fruits and their identification was performed with NMR and MS methods. Optimized HSCCC offers a rapid method of obtaining new natural compounds.