Fullerene-rich soot generated by resistive heating of graphite has been gently extracted with toluene, in order to remove some C60 and C70 compounds, followed by extraction with boiling 1,2,4-trichlorobenzene at 214°C. After filtration and removal of the solvent, the residue was re-dissolved in dichloromethane and characterized by non-aqueous reversed phase liquid chromatography coupled on-line with atmospheric pressure chemical ionization mass spectrometry. Several novel fullerenes were detected, including C72, C80, C86, and C88 as well as other fullerenes up to C108 and higher. The results indicate that chromatographic separation of large fullerene molecules can be achieved with low boiling point solvents and conventional liquid chromatographic techniques. ; Peer reviewed: Yes ; NRC publication: Yes