A novel route (electrodeposition) for the fabrication of porous ZnO nanofilms attached multi-walled carbon nanotubes (MWCNTs) modified glassy carbon electrodes (GCEs) was proposed. The morphological characterization of ZnO/MWCNT films was examined by scanning electron microscopy (SEM) and X-ray powder diffraction (XRD). The performances of the ZnO/MWCNTs/GCE were characterized with cyclic voltammetry (CV), Nyquist plot (EIS) and typical amperometric response (i-t). The potential utility of electrodes constructed was demonstrated by applying them to the analytical determination of hydroxylamine concentration. An optimized limit of detection of 0.12 mu M was obtained at a signal-to-noise ratio of 3 and with a fast response time (within 3 s). Additionally, the ZnO/MWCNTs/GCE exhibited a wide linear range from 0.4 to 1.9 x 10(4) mu M and higher sensitivity. The ease of fabrication, high stability, and low cost of the modified electrode are the promising features of the proposed sensor. (C) 2010 Elsevier Ltd. All rights reserved.