Poly(methacrylic acid-co-3-(methacryloxy)propyltrimethoxysilane) (P(MAA-co-MPS)) organic-inorganic hybrid microspheres were prepared by distillation-precipitation copolymerization of MAA and MPS in acetonitrile in absence of any surfactant and additive. The resultant hybrids had a spherical shape when the MPS inorganic precursor was varied from 0% to 60% in the comonomers during the polymerization. The hybrid microspheres can be facilely cross-linked via the hydrolysis of methoxy groups of polyMPS network and further self-condensation of the hydroxyl groups of silanols. As a result, the hybrid microspheres were facilely converted to mesoporous silica particles via the removal of the organic component through calcination. The narrow dispersed mesoporous silica had a high surface area of 554.2 m(2)/g as well as the average pore size of 8 nm and pore volume of 0.24 cm(3)/g. The corresponding microspheres were characterized by TEM, FT-IR, TGA, and nitrogen sorption-desorption. (C) 2013 Elsevier Inc. All rights reserved.