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 µAµM−1cm−2 and 0.2233 µAµM−1cm−2, 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.