A supercritical CO2 (Sc-CO2) extraction procedure to recover volatile compounds and polyphenols from Rosa damascena is investigated. It consists of two steps: the first by Sc-CO2 at 16 MPa and 313.15 K and on-line fractionation using two separators (S1: 7 MPa/ 298.15 K; S2: 5 MPa/ 288.15 K) for volatile compounds, the second by Sc-CO2 added with 10% ethanol-water mixture (57% v/v) at 8 MPa and 313.15 K for polyphenols. Sc-CO2 extract obtained in S2 resulted of high quality compared with essential oil. Polyphenol yield by SC-CO2 added with co-solvent resulted about 80 % of methanol extraction (3250 mg GAE/100 g dw).