Supercritical fluid extraction of cold-pressed orange oil was carried out in the total reflux operation and continuous countercurrent operation. Internal reflux induced by temperature gradient along the column was applied to achieve the effective separation. For a total reflux operation, raffinate could not be withdrawn at the bottom of the column having a temperature gradient from 313 K at the bottom to 333 K at the top of the column at 8.8 MPa, because the homogeneous phase is formed at the bottom of the column. For the total reflux operation using the column with a uniform temperature at 333 K and 8.8 MPa, terpenes concentration in raffinate was dramatically reduced with an increase in CO, flow rate and the selectivity between terpenes and oxygenated compounds was increased. For a continuous operation, the effect of the reflux on the selectivity was investigated. A new extraction process which can selectively and simultaneously fractionate the terpenes, oxygenated compounds, and waxes in citrus oil into extract, side stream, and raffinate, respectively, were proposed.