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Bimetallic cobalt–nickel supported on carbon fiber (Co-Ni@CF) was synthesized by a straightforward homogeneous co-precipitation approach. Electrochemical results demonstrated that the modified Co-Ni@CF electrode demonstrated excellent electrooxidation activity toward dopamine (DA) and hydroquinone (HQ) without any other activating treatments, which could be modified as an electrochemical biosensor for DA and HQ detection simultaneously. The as-proposed biosensor was developed for simultaneous detection of DA and HQ, featuring low detection limits (LODs) of 0.4698 μM for DA and 0.2388 mM for HQ, respectively. The sensor also offers broad linear ranges for DA (5.0–30 μM), and HQ (0.5–5.0 mM). Along with these attractive features, the Co-Ni@CF electrode also performed good long-term stability and reproducibility, making it a promising candidate for electrochemical biosensing of DA and HQ.