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The combination of graphene and nickel oxide nanoparticles yields nanostructured electrochemical sensor formed a novel kind of structurally uniform and electrocatalytic activity material. In cyclic voltammetry studies, in the presence of epinephrine, nickel oxide / graphene  composite modified electrode shows a significantly higher current response for epinephrine oxidation. Based on differential pulse voltammetry technique, the oxidation of epinephrine exhibited the dynamic range between 1.0–1800.0 μM and the detection limit was 0.42 μM. Finally, the resulting sensor was used to detect epinephrine and AC simultaneously in human serum samples.