A nanohybrid of graphene oxide and multiwalled carbon nanotubes (GO-CNTs) was synthesized through pi-pi interaction. The nickel-cobalt hybrid hexacyanoferrate decorated GO-CNTs (NiCoHCF/GO-CNTs) was prepared by electrodeposition of NiCoHCF in different ratios of Co2+ to Ni2+ solution on GO-CNTs. The characterization was performed by UV-vis, FT-IR, Raman spectroscopy, and SEM. The electrochemistry behavior of NiCoHCF/GO-CNTs was studied by cyclic voltammetry. The NiCoHCF/GO-CNT modified GCE (NiCoHCF/GO-CNT/GCE) exhibited greatly improved electrocatalytic activity towards electrooxidation of hydroxylamine. The modified electrode exhibited a wide linear range from 0.2 mu M to 150 mu M and a low detection limit (LOD) of 0.08 mu M. (C) 2015 Published by Elsevier B.V.