NiCo 2 O 4 /Nano-ZSM-5 nanocomposite materials were prepared by the calcination of the physical mixture of NiCo 2 O 4 and Nano-ZSM-5. Materials were characterized by the complementary combination of X-ray diffraction, N 2 -adsorption and electron microscopic techniques. Electrochemical sensor based on NiCo 2 O 4 /Nano-ZSM-5 nanocomposite was constructed for the simultaneous determination of ascorbic acid, dopamine, uric acid, and tryptophan. Among the materials investigated in this study, NiCo 2 O 4 (30 %)/Nano-ZSM-5 modified glassy carbon electrode exhibited the highest electro catalytic activity with excellent stability, sensitivity, and selectivity. Under the optimum conditions, a wide linear range was obtained from 1-1200 µM for ascorbic acid, 0.6-900 µM for dopamine, 0.9-1000 µM for uric acid, and 0.9-1000 µM for tryptophan. The detection limit was found to be 0.8, 0.5, 0.7 and 0.7 µM for ascorbic acid, dopamine, uric acid, and tryptophan, respectively. The analytical performance of the developed sensor was demonstrated in the determination of ascorbic acid and dopamine in the commercial pharmaceutical preparations (vitamin C tablets and dopamine injections) and uric acid in human urine samples.The solution pH affects the electrochemical behavior of AA, DA, UA, and Trp. The effect of the pH on the electro-catalytic oxidation of AA, DA, UA, and Trp was investigated at NiCo 2 O 4 (30 %)/Nano-ZSM-5/GCE by varying the pH of the supporting electrolyte in a wider range (1-9) using DPV in a solution containing equal concentrations (10 µM) of AA, DA, UA and Trp. The anodic peak current was found to increase with increase in the pH of the medium, with a maximum anodic peak current at pH 3.5 (Fig. S8a). After pH 3.5, it was further decreased.