In this study, we reported a facile and rapid synthesis of NiAl LDH/ERGO and reduced by electrochemical method. Compared with previous studies, this experiment greatly decreased the use of reductive solvents and was environmentally friendly. The nanocomposite material was characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) & transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS) and Fourier transform infrared spectrometer (FT-IR). A series of electrochemical methods were applied to test the electrochemical performance of modified electrodes. When the modified electrode was used to detect AA, DA and UA, the three substances can be clearly separated and the limits of detection for AA, DA and UA can be 0.85 μM in the range 12.48-232 μM, 0.38 μM in the range 1.06-13.26 μM and 0.42 μM in the range 1.25-23.20 μM (S/N = 3), respectively. The modified electrode could provide a reproducible and stable platform to detect AA, DA, and UA simultaneously. [ABSTRACT FROM AUTHOR]