A facile one-step approach was adopted for the electrochemical deposition of cubic nickel hexacyanoferrate/polyaniline hybrids (NiHCF/PANI) on graphene electrode which played an important role in the electrocatalytic polymerization of aniline. NiHCF was hybridized into PANI based on the unique doping property of PANI. The obtained hybrids were characterized by cyclic voltammetry (CV), scanning electron microscope (SEM), and energy dispersive spectrometer (EDS). The non-enzymatic sensor based on the NiHCF/PANI hybrids presented significant electrocatalytic performance toward the oxidation of glucose, because PANI films on graphene could greatly increase the immobilized amount of the redox couple of Ni(OH)(2)/NiOOH. The enzyme-free sensor showed excellent analytical performance and high selectivity with no interferences from other oxidizable species. The as-prepared sensor was further applied for the assay of glucose in real samples, and the results demonstrated its potential as a sensitive glucose sensor. (c) 2014 The Electrochemical Society. All rights reserved.