Robust Cu2S‐Cu3P@C Nanomatrix electrode material has been synthesized via a two‐step process involving carbonization of Cu‐MOF, HKUST‐1, followed by simultaneous phosphorization and sulphurization of the carbonized product. This seamless approach leads to the efficient incorporation of highly active Cu2S‐Cu3P hybrid nanostructures within a conductive carbon matrix, exhibiting exceptional electrochemical glucose sensing performance. Synergistic interactions between Cu2S‐Cu3P and the carbon matrix boost glucose electro‐oxidation kinetics. The resulting Cu2S‐Cu3P@C displays a broad linear response (0.005–5 mM), low detection limit (2.3 μM), and high sensitivity (10,790 μA mM−1 cm−2), with excellent selectivity towards glucose even in the presence of interferents. This biomimetic Cu2S‐Cu3P@C nanomatrix catalyst holds promise for biosensor development in bioanalysis and clinical diagnosis.