A new method for the synthesis of the catalyst systems Pt-Mo was suggested. nPt(0)(Hx-2nMoO3)/GC electrodes were prepared by a redox reaction between the hydrogen-containing molybdenum bronzes and potassium tetrachloroplatinate (II) in acid solutions at open circuit potential. The electrodes were characterized by CVA, SEM, X-ray microanalysis, XRD, XPS and ICP-AES. Pt(0)conglomerates formation with nonuniform distribution over the molybdenum bronzes surface has been revealed. nPt(0)(Hx-2nMoO3)/GC electrodes showed high catalytic activity (not inferior to Pt-Ru-catalyst) in the oxidation of carbon monoxide and methanol as compared with Pt/CC-electrodes. Catalytic effect is apparently achieved by effective oxidation of strongly chemisorbed species (COads, HCOads), which occurs at boundaries platinum - molybdenum oxide. Therefore nPt(0)(Hx-2nMoO3) can be considered as one of perspective catalysts for DMFC. Copyright (C) 2013, Hydrogen Energy Publications, LLC. Published by Elsevier Ltd. All rights reserved.