In the present work, efforts have been made to fabricate a non‐enzymatic electrochemical biosensor based on MgO nanoparticles modified graphene oxide‐molybdenum disulfide (MgO@rGO‐MoS2) nanohybrid for ultra‐sensitive detection of water‐polluting dihydroxy benzene compound. The one‐pot hydrothermal method has been used to synthesize MgO@rGO‐MoS2 nanohybrid followed by electrophoretic deposition of the nanohybrid onto ITO‐coated glass substrate. The excellent conducting and catalytic ability of MoS2 and MgO facilitates the superior electroanalytical ability of fabricated electrodes, as revealed by the electrochemical studies, whereas the non‐enzymatic approach boosts the stability and sensitivity of the transducing matrix. The fabricated biosensor exhibits linear response in the 0.1 to 200.0 μM concentration range for hydroquinone (Hqn) with a detection limit of 0.086 μM and 0.04 μA μM−1 cm−2 sensitivity. The validation of the biosensor with tap and running river water shows an outstanding recovery rate.