We demonstrated a nonenzymatic electrochemical sensor based upon vanadium-doped nickel oxide composite with graphitic carbon nitride. The g-C3N4 was prepared by annealing Urea at 550 °C for 3 h in a muffle furnace. The nanocomposite was synthesized using a microwave-assisted method, followed by thermal annealing at different temperatures. The successful formation of V–NiO/g-C3N4 was confirmed by X-ray diffraction, scanning electron microscopy (SEM), transmission electron microscopy (TEM), and X-ray photoelectron spectroscopy. SEM images show the layered sheets with porous structure, which depends on annealing temperature; as we increase the temperature, the porosity increases. Afterwards, the electrochemical sensing properties were verified by CV, LSV, DPV, and amperometric studies in 0.2 M KOH in the presence of Ascorbic acid and Dopamine. The experimental results show that our prepared sample has excellent electrochemical biosensing abilities towards AA and DA with LOD 1.16 μM and 0.16 μM, respectively. It also offers good selectivity, exceptional reproducibility, and long-term stability owing to the combined effect of NiO and g-C3N4. Finally, the electrochemical sensing of H2O2 was detected in the same environment by conducting CV and amperometric studies. Our modified electrode has proven its noble ability to sense H2O2 with excellent repeatability, stability and low LOD 0.2 μM with a wide linear working range (0.5 mM–4 mM). It has the potential to be used for multi-molecule selection biosensing with excellent selectivity and sensitivity.
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