The study focuses on the analytical characterization of resin fractions from vacuum gas oils (VGO) obtained by LC fractionation. These complex matrices are often considered as containing polar compounds, but are rather defined by their physico-chemical properties than by their chemical structures. Therefore resin fractions remain almost unknown. Owing to the energetic context, which imposes to convert heavy petroleum fractions into transportation fuels, they become key matrices to study. Therefore, to obtain detailed structural information, high resolutive analytical techniques have been implemented: high temperature comprehensive two-dimensional gas chromatography (HT-2D-GC) and Fourier Transform Ion Cyclotron Resonance Mass Spectrometry (FT-ICR/MS). This study provides a unique opportunity to compare these two techniques. Finally innovative compilation of data enables to access unprecedented quantitative extended distributions by carbon atoms number and chemical families on VGO resin fractions. These results are a real progress for the implementation of conversion processes, and open up new prospects for their optimization via kinetic modeling. (C) 2011 Elsevier Ltd. All rights reserved.