Abstract. Samples of mesoporous sorbents based on tetraethoxysilane and titanium dioxide in an acidic medium were obtained using the sol-gel technology. The synthesized mesoporous sorbents are characterized by a large specific surface area of 700-950 m2 / g, as well as an average diameter of 2.6-6.5 nm and a low pore volume of 0.60-0.90 cm3 / g. It was found that a hysteresis loop is observed in the mesoporous sorbents during the adsorption of benzene and water vapors. The phase composition of the sorbents was studied by X-ray diffractometry (XRD), surface characteristics by a scanning electron microscope (SEM). The mesoporous sorbents can be used as a sorbent for gas chromatographic separation of light alkanes, olefins, aromatic hydrocarbons, alcohols, aldehydes, ketones, ethers and esters.