Nanoscaled Ag/Fe3O4 hybrids with different Ag contents and Cu/Fe3O4 nanoshpere and microsphere were successfully synthesized with assistance of sodium citrate and (CH2)(6)N-4 via a hydrothermal process. The as-prepared samples were identified and characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), field emission scanning electron microscopy (FE-SEM), and X-ray photoelectron spectroscopy (XPS), respectively. All samples were used as electrocatalysts modified on a glassy carbon electrode for p-nitrophenol reduction in a basic solution. The catalytic activity of Ag/Fe3O4 samples increased first and then decreased by increasing Ag content from 0% to 8%, and the one with 6% Ag displayed the highest catalytic activity. All the Cu/Fe3O4 samples exhibited enhanced catalytic activity by comparison with a glassy carbon electrode, and the one prepared with the molar ratio of Cu2+, Fe3+, citrate anion, and (CH2)(6)N-4 with 1:1:3:5 exhibited the highest catalytic activity. (C) 2012 Elsevier B.V. All rights reserved.