This work reports a study on two forms of persulfate activation (solar irradiation and anodic oxidation-AO) for the degradation of active pharmaceutical ingredients (APIs). A solution containing a mixture of levonorgestrel and fluoxetine ([LNG]0 = 0.29 ?? 0.03 mg L-1; [FLX]0 = 5.02 ?? 0.34 mg L-1) was treated with persulfate ([PS]0 = 0.07 mol L-1) and irradiated or electrolyzed for 60 min under similar conditions. The results revealed similar decays of APIs in the two activation forms studied, solar/PS (k LNG = 6.6 ?? 10-2 min-1; k FLX = 7.7 ?? 10-2 min-1) and AO/PS (k LNG = 7.8 ?? 10-2 min-1; k FLX = 9.7 ?? 10-2 min-1), with slightly better results for the electrochemical process. However, acute toxicity accessed with Daphnia similis indicated that AO/PS provided a three-fold increase in the values of toxic units.Coordena????o de Aperfei??oamento de Pessoal de N??vel Superior (CAPES)Funda????o de Amparo ?? Pesquisa do Estado de S??o Paulo (FAPESP)Conselho Nacional de Desenvolvimento Cient??fico e Tecnol??gico (CNPq)CAPES: 001; 88887.340964/2019-00FAPESP: 19/24158-9; 21/10919-8; 18/21271-6CNPq: 307481/2017-4; 311230/2020-2