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Nanostructured nickel on porous carbon-silica matrix (N-CS) has been synthesized using a sol gel process and subsequent pyrolysis treatment at a temperature of 650 °C. The morphology and microstructure of the N-CS sample has been investigated using XRD (X-ray Diffraction), SEM-EDS (Scanning Electron Microscopy-Energy Dispersive X-ray Spectroscopy), and BET (Brunauer-Emmett-Teller) analysis. The synthesized nanocomposite has been used for developing NCS-modified screen-printed electrodes (NCS-SPCEs) and was applied in the electrochemical monitoring of glucose. After electrochemical activation, via cycling the modified electrode in a potential window from 0 to 0.8 V in 0.1 M KOH solution, the fabricated NCS-SPCEs electrodes were evaluated for the voltammetric and amperometric determination of glucose. The developed sensors showed good sensing performance towards glucose, displaying a sensitivity of 585 µA/mM cm−1 in the linear range from 0.05 to 1.5 mM, a detection limit lower than 30 µM with excellent selectivity. [ABSTRACT FROM AUTHOR]