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Composite catalysts containing Pt and Mo-oxides are promising materials for anodic catalyst preparation in PEMFCs due to their high tolerance for CO-poisoning. The search for optimal preparation methods for these materials is an important task in modern electrochemical energetics. Two synthetic routines, namely electrodeposition and deposition under open-circuit conditions, were used for Pt-MoO x catalyst preparation. The prepared catalysts were characterized by a variety of modern physical methods (XRD, XPS, SEM, EDX); it was established that the material prepared by electroless deposition contains platinum shell upon platinum core. The materials obtained were tested in the reactions of CO adsorbate electrodeposition and dissolved CO-oxidation. It was found that molybdenum oxides in the composites prepared by electrodeposition broaden the major peak of CO-oxidation, but the peak maximum does not shift toward less positive values. Therefore, the CO monolayer is destabilized as a result of the contact with molybdenum oxides; however, only a small part of CO can be oxidized at these low potentials. Nevertheless, these catalysts are suitable for dissolved carbon monoxide oxidation. aPt·b(H x -2MoO3) composites were synthesized by the redox reaction of K2PtCl4 with reduced forms of hydrogen containing molybdenum bronzes. The CO desorption peak is broadened and shifted toward less positive potentials. aPt·b(H x -2MoO3) catalysts demonstrate high catalytic activity in the reaction of both adsorbed and dissolved CO oxidation. Therefore, one can conclude that both electrodeposition and electroless deposition are suitable methods for preparing PEMFC anode catalysts. Figure 1