Vinasse is the main residue generated during alcohol, sugar and blue rum production by fermentation process. This residue is effluent that could cause serious environmental pollution due to high organic load when is not treated adequately. The aim of this work consists of evaluating the efficiency and application of heterogeneous photocatalysis with TiO 2 , followed by a biological treatment (activated sludge system) to reduce organic load in the referred effluent. Complete factorial designs indicated the best experimental conditions subsequent to photacatalytic and biological treatments providing a reduction of non-purgeable organic carbon (NPOC) as a variable response. After the photocatalytic process, the sample from the best experiment condition was treated by a biological process in order to verify the degradation efficiency of the effluent organic matter studied according to the hybrid system (Advanced Oxidation Process-Activated Sludge System). This system, which presented more efficiency, had a photochemical treatment of 180 minutes carried out in aerated solutions, pH 9 and effluent in natura, while the biological treatment was performed at pH 8 and sludge concentration of 5 gL -1 . The reduction of biochemical oxygen demand (BOD) was >80%. Load the percolation until underground waters, causing an incompatible salubrity for human and animal feeding [7,8].The purpose of this work consisted in evaluating both the efficiency and the application of heterogeneous photo-