Perillyl alcohol, abundant mainly in oranges, has chemotherapeutic activity against carcinogenesis. The peel of Korean oranges was extracted by methanol, and the extract was partitioned by methanol-extract/water/chloroform, (20/5/30 vol%). To concentrate perillyl alcohol of the water-phase in the previous partition step, a glass column (2.5 i.d. ×15cm) with reversed-phase C₁₈ packings (40-63 ㎛) was used. Finally, to obtain perillyl alcohol in a pure form, reversed-phase high-performance liquid chromatography (RP-HPLC) was applied. Mobile phases used were water, methanol, and acetonitrile. The flow rate of the mobile phase was 1 ml/min and UV wavelength was fixed at 205 nm. The resolution of perillyl alcohol from Korean orange peel was achieved on μ-Bondapak C₁₈ column (3.9×300 mm, 10 ㎛) and in-house chromatographic column packed with 15 ㎛ C₁₈ preparative packings. From the experimental results, the mobile phase composition was water/acetonitrile, (65/35 vol%) and the retention time of perillyl alcohol was 20.5 min in the analytical μ-Bondapak column. The effect of injection volumes was investigated in the preparative column.