Fullerene holds a potentially important application value in biology for its special structure. However, its indissolubility in water limits its further application in relative fields. Preparation of water-soluble fullerene derivatives has been proved to be an effective way to solve the problem. In this paper, UV light with 254 nm wavelength was used as the irradiation source. Fullerene molecules can be attacked by hydroxyl radicals (·OH) produced from photo-decomposition of hydrogen peroxide (H,2,O,2,) via subsequent additive reaction. Then fullerenol was successfully synthesized and its structure was characterized by FT-IR, 1H-NMR and UV-vis. The experimental results show that the molecular structure of fullerenol is C,60,(OH),26,. It may be a novel method to synthesize water-soluble fullerenol easily by the UV oxidation.