Abstract This study presents the synthesis of cobalt-doped MoS₂/reduced graphene oxide (Co-MoS₂/RGO) nanocomposites via a microwave-assisted technique. These nanocomposites were meticulously characterized, revealing intricate details of their nanostructure and surface morphology. Electrochemical analyses demonstrated distinct sensing mechanisms for the electrochemical oxidation of ascorbic acid (AA) and uric acid (UA) at the Co-MoS₂/RGO interface. The sensor exhibited a diffusion-controlled behavior, achieving remarkable detection limits of 0.013 µM for AA, 0.06 µM for UA, 0.248 µM for AA in the presence of UA, and 0.36 µM for UA in the presence of AA. Additionally, the Co-MoS₂/RGO composite demonstrated impressive individual and selective sensitivities for AA, measuring 8.42 µA µM⁻¹ cm⁻² and 2.786 µA µM⁻¹ cm⁻², respectively, and for UA, measuring 10.628 µA µM⁻¹ cm⁻² and 7.25 µA µM⁻¹ cm⁻², respectively. These results highlight the exceptional capability of the Co-MoS₂/RGO nanocomposite to distinguish and accurately quantify concentrations of AA and UA, both individually and simultaneously. Furthermore, the Co-MoS₂/RGO sensor demonstrated outstanding repeatability and reproducibility, consistently delivering high performance even after 15 days. These findings underscore the potential of the Co-MoS₂/RGO-based electrochemical sensor as an ultra-sensitive, highly selective, and dependable tool for real-time sample analysis in practical applications.