A novel magnetic nanomaterials-loaded electrode developed for photoelectrocatalytic (PEC) treatment of pollutants was described. Prior to electrode fabrication, magnetic TiO2/SiO2/Fe3O4 (TSF) nanoparticles were synthesized and characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM) and FT-IR measurements. The nanoparticles were dispersed in ethanol and then immobilized on a graphite electrode surface with aid of magnet to obtain a TSF-loaded electrode with high photoelectrochemical activity. The performance of the TSF-loaded electrode was tested by comparing the PEC degradation of methylene blue in the presence and absence of magnet. The magnetically attached TSF electrode showed higher PEC degradation efficiency with desirable stability. Such a TSF-loaded electrode was applied to PEC degradation of diclofenac. After 45 min PEC treatment, 95.3% of diclofenac was degraded on the magnetically attached TSF electrode. (C) 2011 Elsevier B.V. All rights reserved.