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Nickel aluminate nanoparticles (NiAl2O4 NPs) spinel structure is synthesized via a simple solution combustion method using aqueous nickel nitrate, aluminum nitrate and citric acid. The crystal structure and microstructure of the prepared NiAl2O4 NPs are confirmed by powder X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), Fourier transform infrared (FTIR) spectrum, scanning and transmission electron microscopy (SEM/TEM). The characterized NiAl2O4 NPs are applied on a glassy carbon electrode (GCE) to design electrochemical sensor for the detection of dopamine (DA) using cyclic voltammograms (CV) and differential pulse anodic stripping voltammograms. The proposed electrochemical sensor exhibits excellent sensing activity with a low detection limit of 1.78 μM and applicable for a wide linear concentration range of 10 μM–140 μM. Further, the proposed electrode exhibits well resolved differential pulse voltammogram for the dopamine in presence of interfering uric acid and ascorbic acid.