The applicability of silica gel, modified with ketoimine groups, to solid phase extraction (SPE) was tested. Basic characteristics of the modified silica were determined using elemental analysis, and 29 Si CP MAS NMR spectroscopy, as well as measurement of specific surface area. Some applications of the sorbent studied to preconcentration and further determination of organic compounds, such as benzene, phenol, and o-chlorophenol, by means of solid-phase extraction (SPE) and gas chromatography are presented. The determined recovery rates were about 95%-98%.