Metal Endohedral C-60 (M@C-60 M: Ca, Y, Cel Pr, Nd, Gd) were extracted with aniline from the soots synthesized by are-heating of metal oxide/graphite rods. The extracted solutions, which contain C-60, C-70 and metal endohedral higher fullerenes other than M@C-60, were purified by high performance liquid chromatography (HPLC) technique with aniline as eluent. The laser desorption time-of-flight (LD-TOF) mass spectra for purified solutions exhibited pronounced peaks for M@C-60, indicating the enrichment of M@C-60 in the extracted solutions.