Synthesis of a novel thermally stable mesoporous ceria-titania phase using a neutral templating route is reported. The as-made inorganic-template hybrid mesostructured matrix showed a broad low-angle XRD peak characteristic of mesoporous materials. Careful thermal treatment of the matrix allowed the subsequent densification (of the pore walls) of the inorganic component and removal of the organic component so that a high-quality mesoporous ceria-titania was formed as observed by TEM analysis. The calcined material showed the formation of fluorite type structure of CeO2 but no crystalline titania phase was observed. The mesoporous structure remained even after high-temperature treatment. The material had high surface area after calcination up to the temperature of 973 K, with well-dispersed ceria and titania components and negligible bulk oxide formation (from XRD, UV-vis, and XPS analysis). These novel mesoporous ceria-titania materials showed high performance for the removal of volatile organic compound (toluene). The toluene removal performance was further enhanced for Pt impregnated mesoporous ceria-titania.