The ability to measure uric acid (UA) non-enzymatically in human blood has been demonstrated through the use of a simple and efficient electrochemical method. A phytochemical extract from radish white peel extract improved the electrocatalytic performance of nickel–cobalt bimetallic oxide (NiCo2O4) during a hydrothermal process through abundant surface holes of oxides, an alteration of morphology, an excellent crystal quality, and increased Co(III) and Ni(II) chemical states. The surface structure, morphology, crystalline quality, and chemical composition were determined using a variety of analytical techniques, including powder X-ray diffraction (XRD), scanning electron microscopy (SEM), high-resolution transmission electron microscopy (HR-TEM), and X-ray photoelectron spectroscopy (XPS). The electrochemical characterization by CV revealed a linear range of UA from 0.1 mM to 8 mM, with a detection limit of 0.005 mM and a limit of quantification (LOQ) of 0.008 mM. A study of the sensitivity of NiCo2O4 nanostructures modified on the surface to UA detection with amperometry has revealed a linear range from 0.1 mM to 4 mM for detection. High stability, repeatability, and selectivity were associated with the enhanced electrochemical performance of non-enzymatic UA sensing. A significant contribution to the full outperforming sensing characterization can be attributed to the tailoring of surface properties of NiCo2O4 nanostructures. EIS analysis revealed a low charge-transfer resistance of 114,970 Ohms that offered NiCo2O4 nanostructures prepared with 5 mL of radish white peel extract, confirming an enhanced performance of the presented non-enzymatic UA sensor. As well as testing the practicality of the UA sensor, blood samples from human beings were also tested for UA. Due to its high sensitivity, stability, selectivity, repeatability, and simplicity, the developed non-enzymatic UA sensor is ideal for monitoring UA for a wide range of concentrations in biological matrix
