Phenolic compounds, prevalent in both human life and the natural environment, pose a significant threat to human health due to their toxic effects. Therefore, accurate determination of these compounds are crucial. Herein, we developed a new electrochemical sensor based on a NiO/C@reduced graphene oxide nanocomposite (NiO/C@rGO) to simultaneously assess three phenolic compounds: hydroquinone (HYQ), catechol (CAT), and bisphenol A (BPA). The NiO/C@rGO nanocomposite was synthesized via Ni(gallate)@GO pyrolysis and extensively characterized using various techniques. Subsequently, a glassy carbon electrode (GCE) modified with the NiO/C@rGO nanocomposite was utilized as the electrochemical sensor to simultaneously detection. The developed nanosensor (NiO/C@rGO/GCE) exhibited exceptional selectivity and a broad linear ranges for HYQ, CAT, and BPA, spanning from 0.01 to 100 μM, with impressively low detection limits. Furthermore, the NiO/C@rGO nanocomposite demonstrated remarkable stability and high reproducibility. Moreover, we successfully applied the NiO/C@rGO-based sensor to evaluate the three phenolic compounds in tap water, drinking water, and mineral water samples. The results underscore the potential of the developed electrochemical sensor as a reliable tool for the sensitive and fast detection of phenolic compounds in various water sources, addressing the critical need for safeguarding human health and the environment from their adverse effects.