The electrochemical activity was studied by cyclic voltammetry. Higher CO and methanol oxidation current densities were found for catalyst deposited on chemically treated carbon xerogel when compared with the untreated material, whereas the heat treatment of carbon supports was in detriment of the catalytic activity. Gas diffusion electrode preparation and MEA assembly allowed an in-house built direct methanol fuel cell to evaluate the performance of synthesized catalysts and supports. Polarization curves were measured and confirmed the data obtained from cyclic voltammetry regarding the negative effect of heat treatment on the catalytic activity of these materials. Normalized power density curves and maximum cell power per Pt weight are discussed in terms of the operational temperature for the different materials, in comparison with results obtained with a commercial catalyst. Moreover, relationship between catalytic activity and oxygenated surface groups was established and it seems that carboxylic groups play a key role in this respect.