To separate perillyl alcohol (POH), a potential anti-cancer agent, the peel of citrus unshiu was extracted by supercritical CO2 extraction (SCE) system at 50 ℃, 200 bar and 6 kg CO2/hr/kg sample. The extracts were partitioned by acetonitrile/hexane (90/10, vol%). POH was eluted in the acetonitrile phase. An open-tubular chromatography with silica gel (40-63 μm) was used to purify POH from the acetonitrile phase. Mobile phase was hexane/ethyl acetate (90/10, vol%). To obtain POH in a pure form, finally preparative high-performance liquid chromatography was applied. The collection of POH from citrus unshiu peel was achieved on a laboratory-prepared chromatographic column (300×3.9 mm) packed with 15 μm C18 preparative packings. The composition of mobile phase was water/acetonitrile (50/50, vol%). The flow rate of the mobile phase was 1 ml/min and UV wavelength was fixed at 205 nm. It was found that the total yield of POH was 1.6×10(-3) (wt%) as the dry powder of citrus unshiu peel.