Various water-soluble multi-hydroxyl fullerenes (fullerenols), C-60(OH)(n), C-70(OH)(n) and C-84(OH)(n), and a Gd metallo-fullerenols, Gd@C-82,(OH)(n) have been synthesized by the Kitazawa method. Elementary chemical analyses indicate that all of these fullerenols have 30-40 hydroxyl groups and 11-15 coordinated water molecules via hydrogen bonds. Electron energy loss spectroscopy (EELS) on Gd@C-82 fullerenols shows that the pi* peak area in the C K-edge spectra decreases on going from intact Gd@C-82 metallofullerene to Gd@C-82 fullerenols, indicating an increase in sp(3) character of the fullerenols. Furthermore, Gd M-4.5-edge EELS spectra show that the encapsulated Gd atom has a trivalent Gd3+ state.