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The mesoporous silica particles were prepared by the sol–gel method in one-step synthesis, in acidic conditions, from tetraethoxysilane (TEOS) and methyltriethoxysilane (MTES), varying the mole ratio of the silica precursors. Nitric acid was used as catalyst at room temperature and hexadecyltrimethyl ammonium bromide (CTAB) as structure directing agent. Optical properties, porosity and microstructure of the materials in function of the MTES/TEOS ratio were evaluated using infrared spectroscopy, nitrogen adsorption and small angle X-ray scattering. All materials showed the ordered pore structure and the high specific surfaces, making them suitable as the drug delivery systems. Drug loading and release tests using ketoprofen were performed to assess their performance for drug delivery applications. The amount of the methylated precursor used in the synthesis had little effect on the drug loading capacity, but had a strong influence on the initial rate of the drug release.