Liaohe VGO, CGO and HCO were separated into saturates, monoaromatics, diaromatics, polyaromatics and resins by preparative liquid chromatography and synchronous fluorescence spectrometry (LC-SFS). The analyses of aromatics by gas chromatography and mass spectrometry (MS), respectively, confirmed that there were little overlaps between fractions. The order of monoaromatic contents of the three samples is VGO > CGO > HCO, while the reverse order is obtained for the polyaromatic contents of the three samples, HCO > CGO > VGO >. The comparison of the group-type results of the three samples by LC-SFS method and by MS group-type method indicated that the MS group-type results of CGO and HCO were suspect.