The shock loading of wastewater treatment plants (WWTPs) with toxic pollutants remains a critical problem with crucial significance for the technologies. On 5 November 2014, 30 tons of mazut were emitted in Sofia's WWTP ‘Kubratovo’, passing through equipment and damaging the functioning of the technological modules. The rehabilitation of activated sludge (AS) after shock loading as well as the development of detoxification activity were investigated. The hydrocarbon index of petroleum products, filamentous index (FI), sludge biotic index, sludge volume index (SVI), chemical oxygen demand (COD), biochemical oxygen demand (BOD5), oxygenases and succinate dehydrogenase activities were analyzed for a period of two weeks. The results show that independently from prolonged rehabilitation period, AS remained with filamentous bulking (SVI over 200 ml/g and FI over 1.107 μm/mg). At the same time, the detoxification potential of the AS was developed. Although the morphological and functional structure was still not fully recovered, the AS developed two adaptive mechanisms. First, activation of shorter, more effective ways for benzene ring cleavage, operated by catechol 2,3-dioxygenase; second, strong increase of succinate dehydrogenase activity, which is consistent with the activation of the degradation of trivial substrates for energy generating to overcome the intoxication and synthesis of oxygenases.