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The voltammetric behavior of carbon electrodes coated by a nickel macrocyclic complex-based film in alkaline aqueous solution is described. The nickel-based modified electrodes were prepared by anodic oxidation of nickel porphyrin and nickel cyclam complexes by repeated potential scans in 0.1M NaOH aqueous solution. The nickel-based films act as efficient materials for the electrocatalytic oxidation of alcohols and phenol derivatives in aqueous 0.1M NaOH and prevent the electrode from irreversible passivation during the electrocatalytic oxidation of phenols in neutral aqueous solution.