The biphenilaminepropylsilica and biphenilaminepropylsilicatitania were synthesized by sol-gel method, in two steps: (a) biphenylamine reacts with chloropropyltrimethoxysilane and (b) the product of reaction was polycondensed with tetraethylorthosilicate (TEOS) or TEOS and titanium isopropoxide. The sol-gel materials were characterized using infrared spectroscopy and N(2) adsorption-desorption isotherms and they were employed as sorbents for carcinogenic N-containing compound retention, in aqueous solution, using the SPE technique. The N-containing compounds adsorption was influenced by the titania presence and the sorption process seems to happen in the pores with higher organic density.