For developing effective electrochemical sensor of p-hydroxyaniline (p-HAD), graphene/hollow carbon nanospheres (GN/HCNS) hybrids were produced via a self-assembly approach and further decorated gold nanoparticles (AuNPs) to enhance detection sensitivity. The obtained AuNPs/GN/HCNS nanohybrids could exhibit the unique properties of AuNPs, GN and HCNS for voltammetric sensing p-HAD. After characterizingmorphology and structure of AuNPs/GN/HCNS and optimizing detective conditions, the simple and sensitive voltammetric sensor of p-HAD was constructed successfully. The results demonstrated that AuNPs/GN/HCNS modified electrode has a low detection limit (0.01 mu M) and wide linear range (0.1-40.0 mu M) toward p-HAD. Also, the reproducibility, stability, selectivity and practical application performance of AuNPs/GN/HCNS were evaluated, and the obtained results are satisfactory. (c) 2017 The Electrochemical Society. All rights reserved.