A simple and effective strategy was proposed for synthesis of nickel nanoparticls dispersed at poly1,5-diaminonaphthalene(NiNPs@P-1,5-DAN). NiNPs@P-1,5-DAN was prepared by using repeated potential cycling technique in an acidic solution containing 1.5 mM 1,5-diaminonaphthalene at glassy carbon electrode surface, giving the GC modified electrode (P-1,5-DAN/GC). The transition metal ions of Ni(Pi) were incorporated to the polymer by immersion of the modified electrode in a 1.0 M nickel chloride solution, NiNPs@P-1,5-DAN modified electrode was obtained and characterized by scanning electron microscope (SEM). The electrochemical characterization of this modified electrode exhibits stable redox behavior of Ni(III)/Ni(II) couple in 0.1 M NaOH aqueous solution. The electrooxidation of single glucose (Glu), ascorbic acid (AA) and dopamine (DA) in 0.1 M NaOH was studied by using square wave voltammetry (SWV). NiNPs@P-1,5-DAN/GC modified electrode was applied for the electrocatalytic oxidation and simultaneous determination of Glu, AA and DA in alkaline solution. The calibration curves for Glu, AA and DA were plotted. The detection limits were 0.252, 0.010 and 0.011 mu M for Glu, AA and DA respectively. (C) 2012 Elsevier Ltd. All rights reserved.