The objective of the present study was preparation of a new hybrid of highly ordered organic-inorganic mesoporous silica (MCM-48) with spherical morphology. Firstly, the synthesis process carried out at room temperature by Tetraethyl orthosilicate (TEOS) as silica source in water/ethanol solution containing ammoniac and in the presence of cetyltrimethylammonium bromide (CTAB) as templating agent [1]. Obtained mesoporous materials functionalized by 3-Aminopropyl trimethoxysilane (APTMS) with post-synthesis methods [2]. The Structural features of the produced material characterized by means of X-ray diffraction (XRD), nitrogen adsorption-desorption (BET), thermogravimetric analysis (TGA), Scanning electron microscopy (SEM), and Fourier transform infrared (FT-IR) spectroscopy. SEM results reveal that MCM-48 particles size exhibited from 500 to 800 nm with spherical morphology. The XRD pattern of the resulting product revealed not only an ordered typical pattern of Ia3d cubic structure, but also the maintenance of the structural order of the synthesized materials after functionalization. On the other hand, FT-IR analysis indicates that successful grafting of organic amine into the pore surface. The thermograms of MCM-48 and NH2-MCM-48 revile the complete surfactant removal and successful functionalization. In addition, The BET results revealed that the pore sizes was about 2.44 nm, specific surface areas up to 1326 m2.g-1 and total pore volumes of 1.11 cm3.g-1.