Herein, a facile one step synthesis of Ni–Cu supported on TiO2 alloy nanoparticles through the polyol method, which reflect high catalytic performance in enzymeless electrochemical glucose sensing and applied onto glassy carbon, is reported. The morphology imaging and physical properties of the Ni–Cu/TiO2 nanocomposite were characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD) analysis, and energy dispersive X-ray spectroscopy (EDS). The electrochemical studies/characterizations of glucose oxidation were realised in a basic medium and the new sensor was found to be a better electrochemical glucose sensor than Ni/TiO2/Ti and CuO/TiO2/Ti modified electrodes. The fabricated sensor was highly sensitive (719.9 μA mM-1 cm-2), had a wide linear range (from 0.1 to 6 mM), selective and tolerant towards endogenous species, such as ascorbic acid, uric acid, acetaminophen and sodium chloride.