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PtRu/carbon hybrid materials were prepared by hydrothermal carbonization using starch as carbon source and reducing agent and H 2 PtCl 6 .6H 2 O and RuCl 3 .xH 2 O as metal sources of the carbonization process. The materials were prepared in the following conditions: without pH adjustment, in the absence and in the presence of tetrapropylammonium chloride, and adjusting the pH using potassium hydroxide or tetrapropylammonium hydroxide. The as-synthesized materials were further treated under argon atmosphere at 900°C and characterized by energy dispersive X-ray spectroscopy, thermogravimetric analysis, BET isotherm, Fourier transform infrared spectroscopy, X-ray diffraction, transmission electron microscope, and cyclic voltammetry. The electrooxidation of methanol was studied by chronoamperometry. The addition of tetrapropylammonium ion promoted an increase in surface area and total pore volume while the alkaline medium favored smaller particle sizes. The material prepared using tetrapropylammonium hydroxide showed the best electroactivity for methanol electrooxidation compared to others obtained materials.