Here, the voltammetric electrochemical approach was applied to detect uric acid (UA) in a conductive sensing medium (phosphate buffer solution-PBS) by using PbO-doped NiO nanocomposites (NCs)-decorated glassy carbon electrode (GCE) performing as working electrode. The wet-chemically prepared PbO-doped NiO NCs were subjected to characterization by the implementation of XRD, FESEM, XPS, and EDS analysis. The modified GCE was used to detect uric acid (UA) in an enzyme-free conductive buffer (PBS) of pH = 7.0. As the outcomes of this study reveal, it exhibited good sensitivity of 0.2315 µAµMcm and 0.2233 µAµMcm, corresponding to cyclic (CV) and differential pulse (DPV) voltammetric analysis of UA, respectively. Furthermore, the proposed UA sensor showed a wider detection (0.15~1.35 mM) range in both electrochemical analysis methods (CV & DPV). In addition, the investigated UA sensor displayed appreciable limit of detection (LOD) of 41.0 ± 2.05 µM by CV and 43.0 ± 2.14 µM by DPV. Good reproducibility performance, faster response time and long-time stability in detection of UA were perceived in both electrochemical analysis methods. Finally, successful analysis of the bio-samples was performed using the recovery method, and the results were found to be quite acceptable in terms of accuracy. Thus, the findings indicate a reliable approach for the development of 5th generation biosensors using metal-oxides as sensing substrate to fulfill the requirements of portable use for in situ detection.