The electrochemical performance of NiCo2O4 with urea precursors was evaluated in order to develop a non-enzymatic urea sensor. In this study, NiCo2O4 nanostructures were synthesized hydrothermally at different concentrations of urea and characterized using scanning electron microscopy and X-ray diffraction. Nanostructures of NiCo2O4 exhibit a nanorod-like morphology and a cubic phase crystal structure. Urea can be detected with high sensitivity through NiCo2O4 nanostructures driven by urea precursors under alkaline conditions. A low limit of detection of 0.05 and an analytical range of 0.1 mM to 10 mM urea are provided. The concentration of 006 mM was determined by cyclic voltammetry. Chronoamperometry was used to determine the linear range in the range of 0.1 mM to 8 mM. Several analytical parameters were assessed, including selectivity, stability, and repeatability. NiCo2O4 nanostructures can also be used to detect urea in various biological samples in a practical manner.