This paper demonstrated an electrochemical sensor based on NiO nanoparticles-graphene composite film (NiO/GR) modified glassy carbon electrode for detecting ascorbic acid (AA) in the presence of folic acid using differential pulse voltammetry. The obtained NiO/GR nanocomposite was fabricated by electro-deposition technology. The morphologies and interface properties of NiO/GR composite film were examined by scanning electron microscopy, energy dispersive X-ray spectroscopy and electrochemical impedance spectroscopy. The modified electrode exhibits excellent sensing performance for detecting AA with linear range from 0.05 to 1100 mu M and a detection limit of 0.0167 mu M (S/N = 3). Under optimal conditions, the sensor displays excellent stability and satisfactory results in real samples analysis. (C) 2014 Published by Elsevier Ltd.