Plasma techniques have been extensively utilized in catalysis. Catalyst preparation using plasma treatment allows to improve dispersion, enhancing the catalyst performance and stability. In this paper, the low-pressure radio frequency (RF) discharge is shown as an efficient method to enhance the activity of cobalt tetramethoxyphenylporphyrin (CoTMPP)-based electrocatalyst for the reduction of hydrogen peroxide. It was found that a carbon-supported CoTMPP catalyst (20% CoTMPP/C) treated by plasma presents two-fold higher catalytic activity than catalyst prepared without plasma treatment. The influence of catalyst treatment on elemental surface and bulk concentration and performance of catalysts for hydrogen peroxide in a fuel cell was investigated.