Advanced Oxidative Processes (AOPs) are perspective technologies that may be used for solving problem in wastewater treatment. AOPs based on ability of hydroxyl radicals to degrade organic compounds into the end products of carbon dioxide and water. Advanced oxidation has been used to treat wastewater, groundwater and drinking water contaminated by dyes, organic pollutants and etc. In last years advanced oxidation processes have been widely studied using Fenton reagent (Fe2+/H2O2) in homogeneous systems. However, developing Fenton-like processes using solid systems for radical generation is rather attractive. In particular systems containing ions other than ferric or ferrous ones are of interest. We describe here the preparation and characterization of silica doped with cerium and silver ions, a comparison of the catalysts with cobalt and nickel-containing samples and their application in oxidative degradation of 2-nitro-aniline in aqueous solution. The catalysts were synthesized by sol-gel technique. The samples were characterized using XRD, scanning electron microscopy, energy-dispersive X-ray spectroscopy (EDX), nitrogen adsorption-desorption measurements. Chemiluminescence of luminol was used for an estimation of radical activity of the samples. The data obtained allowed to demonstrate efficiency of cerium- and silver-containing samples in process of 2-nitro-aniline degradation. Cobalt and nickel doped materials were less active. The effect of matrix on activity of the investigated samples was evaluated. The activity was rather low regardless the support used.