Nickel-based catalysts have been widely recognized as highly promising electrocatalysts for oxidation. Herein, we designed a catalyst surface based on iron oxide electrodeposited on NiCo2O4 spinel oxide. Nickel foam was used as a support for the prepared catalysts. The modified surface was characterized by different techniques like electron microscopy and X-ray photon spectroscopy. The activity of the modified surface was investigated through the electrochemical oxidation of different organic molecules such as urea, ethanol, and ethylene glycol. Therefore, the modified Fe@ NiCo2O4/NF current in 1.0 M NaOH and 1.0 M fuel concentrations reached 31.4, 27.1, and 17.8 mA cm−2 for urea, ethanol, and ethylene glycol, respectively. Moreover, a range of kinetic characteristics parameters were computed, such as the diffusion coefficient, Tafel slope, and transfer coefficient. Chronoamperometry was employed to assess the electrode’s resistance to long-term oxidation. Consequently, the electrode’s activity exhibited a reduction ranging from 17% to 30% over a continuous oxidation period of 300 min.