The incomplete removal of emerging pollutants, such as parabens, from wastewater effluents represents a major pathway for their release into the environment. The development of advanced technologies integrated into well-known conventional systems is a solution. Advanced oxidative processes (AOP), such as ozonation and its combinations, are technologies based on the generation of hydroxyl radicals (HO•) capable of removing these pollutants, representing an alternative solution to this problem. Therefore, the present study aimed to investigate the ozonation process combined with hydrogen peroxide (O3/H2O2) in the treatment of anaerobic effluent post-treated by a real-scale upflow anaerobic sludge blanket (UASB) reactor, enriched with methylparaben (MeP). The study was conducted under optimized conditions and at neutral pH of the effluent. To investigate the influence of variables, as ozone concentration, hydrogen peroxide concentration, pH and time, a 24 Factorial experimental design followed by a 22 Doehlert optimization design was implemented. The optimal degradation occurred with 25.0 mg L−1 of O3 and 30.0 mg L−1 of H2O2 at neutral effluent pH, achieving a removal efficiency of 71.6 % after 60 min and 85.5 % after 120 min. The optimized O3/H2O2 process after 60 min achieved a 95.0 % removal of organic matter by biochemical oxygen demand (BOD), reducing the initial concentration from 138 mg L−1 to 7 mg L−1. Acute toxicity test with Artemia salina and Lactuca sativa, indicated an absence of toxicity (TU < 0.4). The findings of this study indicate the positive efficiency of combining post-UASB effluent treatment with O3/H2O2 processes for the removal of methylparaben.