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In this work, Pt, Fe and Co nanoparticles were prepared by chemical reduction of the metal salts in chitosan as the support. NaBH4 was used as the reducing agent Pt-Fe, Pt-Co and Pt-Fe-Co-chitosan nanocomposites were synthesized and characterized by UV–Vis spectra and Transmission electron microscopy images. GC/Pt-chitosan, GC/Pt-Co-chitosan, GC/Pt-Fe-chitosan and GC/Pt-Co-Fe-chitosan electrodes were prepared. The performances of these electrodes for methanol electrooxidation were investigated through cyclic voltammetric and chronoamperometric curves. The effect of some experimental factors such as the amounts of Fe and Co nanoparticles dispersed in chitosan, methanol concentration and scan rate were studied and the optimum conditions were determined. The effect of temperature was also investigated and the activation energies were calculated. The performance of Pt-Fe-Co-chitosan nanocomposites was determined in a direct methanol fuel cell in different conditions. The electrochemical and fuel cell measurements showed that Pt-Fe-Co-chitosan nanocatalyst has the best activity for electrooxidation of methanol among all different compositions electrodes.