In this work a new route for preparation of nickel ferrites nanoparticles has been developed. The synthesis is carried out in an electrochemical cell using three electrodes, a sheet of iron was employed as cathode and two sheets of iron and nickel were used as sacrificial anodes. The obtained nanoparticles were washed several times with distilled water, separated magnetically and dried under vacuum with constant temperature for 12 h. The characterization of the nanoparticles was carried out by X-ray diffraction (XRD), transmission electron microscopy (TEM), and Inductively coupled plasma mass spectrometry (ICP-MS). Magnetic measurements were carried out using a vibrating sample magnetometer (VSM). To evaluate the catalytical properties of these nanoparticles against the oxidation of glucose a graphite paste electrode (GPE) was made. The proportions of the nanoparticles in GPE were 5, 10, 20 and 50% in weight. The electrode shows promising properties for its use as catalyst in the glucose oxidation. (c) 2011 Elsevier B.V. All rights reserved.