We have successfully synthesized nanostructured cubic NiAl2O4 nanoparticles for the selective electrochemical determination of gallic acid (GA) and the prepared nanostructured composite material was characterized by (X-ray diffraction, Fourier transform infrared spectroscopy, and field-emission scanning electron microscopy analyses. The cubic NiAl2O4 nanoparticles had average sizes of similar to 26-30 nm as calculated from XRD and SEM measurements, respectively. GA-detection performance was also evaluated by cyclic voltammetry and amperometry method. NiAl2O4 glassy carbon electrode showed excellent performance in GA detection with a linear range, detection limit (SNR = 3 sb/S), limit of quantitation (LOQ = 10 sd/S) and sensitivity value of 0.03-551.18 mu M, 0.018 mu M, 0.057 mu M and 9.019 mu M mA(-1) cm(-2), respectively. The GA sensor was also used in real-sample analysis using food samples, and results showed the practicability of the proposed sensor. (c) 2019 The Electrochemical Society.