Novel MCM-41 modified catalytic materials were synthesized by impregnation of MCM-41 with niobium and gallium salts. A number of techniques, including nitrogen adsorption, X-ray diffraction, FT-IR and Raman spectroscopies, have been used to characterize a series of gallium and niobium-containing composite materials, aimed especially at the rationalization of the nature of oxides species formed. Generally, the presence of highly dispersed NbOx and GaOx moieties in the mesoporous materials could be deduced from this approach. It has been demonstrated that incorporation of gallium and niobium into the MCM-41 type silica matrix leads to formation of active and selective catalysts for the oxidation of hydrocarbons. (c) 2007 Elsevier B.V. All rights reserved.