The electroreforming of glucose/xylose mixtures has been evaluated at Pd 1-x Au x /C anodes in 0.10 mol L À 1 NaOH electrolyte. The catalysts synthesized by a wet chemistry route are comprehensively characterized by physicochemical and electrochemical techniques. From linear scan voltammetry and in situ Fourier transform infrared spectroscopy measurements, it was shown that the Pd 0.3 Au 0.7 /C material led to the best electrocatalytic behavior towards the electrooxidation of glucose/ xylose mixtures in terms of activity (higher current densities at lower potentials) and selectivity (lower dissociative adsorption). Six-hour chronoamperometry measurements were performed at 293 K in a 25 cm 2 electrolysis cell at + 0.4 V and + 0.6 V and the reaction products were analyzed by high performance liquid chromatography. The main products were gluconate and xylonate, but the contributions of xylose to all formed products was always lower in percentages than the initial xylose ratios in solutions, showing that glucose was more electro-reactive than xylose at Pd 0.3 Au 0.7 surface.