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Uniform and porous CoNi 2 Se 4 was successfully synthesized by electrodeposition onto a composite electrode comprising reduced graphene oxide (rGO) anchored on a Ni foam substrate (prepared hydrothermally). This CoNi 2 Se 4 –rGO@NF composite electrode has been employed as an electrocatalyst for the direct oxidation of glucose, thereby acting as a high-performance non-enzymatic glucose sensor. Direct electrochemical measurement with the as-prepared electrode in 0.1 M NaOH revealed that the CoNi 2 Se 4 –rGO nanocomposite has excellent electrocatalytic activity towards glucose oxidation in an alkaline medium with a sensitivity of 18.89 mA mM −1 cm −2 and a wide linear response from 1 μM to 4.0 mM at a low applied potential of +0.35 V vs. Ag|AgCl. This study also highlights the effect of decreasing the anion electronegativity on enhancing the electrocatalytic efficiency by lowering the potential needed for glucose oxidation. The catalyst composite also exhibits high selectivity towards glucose oxidation in the presence of several interferents normally found in physiological blood samples. A low glucose detection limit of 0.65 μM and long-term stability along with a short response time of approximately 4 seconds highlights the promising performance of the CoNi 2 Se 4 –rGO@NF electrode for non-enzymatic glucose sensing with high precision and reliability.