Higher fullerenes, including newly identified C86, were purely isolated by HPLC (High Performance of Liquid Chromatography). The precise mass spectroscopy by LD-TOF (Laser Desorption - Time of Flight) method leads to an observation of a new oxidized product during the HPLC process, which can be assigned to C58-C60O pair fullerenes by comparing with the LD-TOF mass spectrum of chemically oxidized C60.