Surfactants after their use are discharged into aquatic ecosystems. These compounds may be harmful to fauna and flora in surface waters or can be toxic for microorganisms of the activated sludge or biofilm in WWTP. In order to determine effectiveness of different advanced oxidation processes on the degradation of surfactants, in this study the degradation of anionic surfactants in aqueous solution using photolysis by 254 nm irradiation and by advanced oxidation process in a H2O2/UVC system was investigated. Two representatives of anionic surfactants, linear alkyl benzene sulphonate (LAS-R11–14) and ether carboxylic derivate (EC-R12–14E10) were tested. The influence of pH, initial surfactant concentration and dose of hydrogen peroxide on the degradation was also studied. Results show outstanding effectiveness of the H2O2/UVC system in the removal of surfactant from aqueous solutions.