A well-dispersed Au nanoparticle grown on carbon nanofibers (AuNPs/CNFs) with excellent electroanalytical activity and sensitivity towards the detection of heavy metal ions was synthesized via electrospinning technology and in situ thermal reduction. Field-emission scanning electron microscopy (FE-SEM) and transmission electron microscopy (TEM) images show that a large amount of AuNPs with a diameter of 5-15 nm was homogenously distributed on the surface of the nanofibers. The AuNPs/CNFs hybrids modified electrode was utilized as the working electrode for the simultaneous detection of heavy metal ions such as Cd2+, Pb2+ and Cu2+ through the square wave anodic stripping voltammetry (SWASV) method. The electrochemical results indicate that the simultaneous detection of Cd2+, Pb2+ and Cu2+ with a low concentration of 0.1 mu M can be obtained. This work may provide an easy way to construct electrochemical sensors for the quick detection of trace heavy metal ions. (C) 2016 Elsevier Ltd. All rights reserved.