Abstract: Photocatalytic degradation performance is highly related to optimized operating parameters such as initial concentration, pH value, and catalyst dosage. In this study, the impact of various parameters on the photocatalytic degradation of anaerobically digested vinasse (AnVE) has been determined through decolourization and chemical oxygen demand (COD) reduction efficiency using zinc oxide (ZnO) photocatalyst. In this context, the application of photocatalytic degradation in treating sugarcane vinasse using ZnO is yet to be explored. The COD reduction efficiency and decolourization achieved 83.40% and 99.29%, respectively, under the conditions of 250 mg/L initial COD concentration, pH 10, and 2.0 g/L catalyst dosage. The phytotoxicity assessment was also conducted to determine the toxicity of AnVE before and after treatment using mung bean (Vigna radiata). The reduction of root length and the weight of mung bean indicated that the sugarcane vinasse contains enormous amounts of organic substances that affect the plant's growth. The toxicity reduction in the AnVE solution can be proved by UV-Vis absorption spectra. Furthermore, the catalyst recovery achieved 93% in the reusability test. However, the COD reduction efficiency and decolourization were reduced every cycle. It was due to the depletion of the active sites in the catalyst with the adsorption of organic molecules. Thus, it can be concluded that the photocatalytic degradation in the treatment of AnVE was effective in organic degradation, decolorization, toxicity reduction and can be reused after the recovery process.