Poly (1-amino-2-methyl-9,10-anthraquinone) (PAMAQ) modified electrode (ME) was synthesized at glassy carbon electrode in a binary solvent mixture containing acetonitrile and 5.0 M H2SO4 (1:1) employing a continuous cyclic voltammetry (CV) technique. Nickel (II) nanoparticle ions (NiNPs) were incorporated into the polymer by immersing the ME in an aqueous 1.0 M nickel chloride (NiCl2 6H(2)O) solution for 30 min. ME polarization process was performed in an aqueous 0.1 M NaOH solution using CV technique by sweeping the potential between 0.0 and 0.8 V with a potential sweep rate of 0.1 V s(-1) for 30 scans to improve its electrochemical response. The obtained NiNPs/PAMAQ-polarized ME was characterized electrochemically using CV technique. The surface morphology of the NiNPs/PAMAQ-polarized ME was analyzed by scanning electron microscopy which demonstrates the presence of NiNPs within the surface of the film. NiNPs/PAMAQ-polarized ME showed excellent catalytic activities toward electrochemical oxidation of ascorbic acid (AA), uric acid (UA), and glucose (Glu) using square-wave voltammetry technique in their single, binary, and ternary mixtures. The ME was applied for the determination of UA, AA, and Glu in real samples.