AbstractTiO2 nanoparticles co‐doped with iron and carbon were tested in photocatalytic processes using visible radiation to degrade Acid Orange 7 and Paracetamol from aqueous solutions. In our previous reports, the mesoporosity and crystallinity of the samples were analyzed along with the calcination temperature effect. In this work, it was possible to verify the efficiency of a synergistic effect between dopants when a calcination at 150 °C was applied, favoring their localization in key sites of titania structure which improves the response under visible light. Such accomplishments could be also confirmed through photoluminescence analysis. Thus, the optimized solid showed an enhanced photocatalytic performance, reaching at only one hour of reaction, a complete degradation of both dye and drug while some intermediate species were reduced according to mineralization degree (around 80 %), and biodegradability achieved. Therefore, the proposed photocatalytic system presents potential as a previous step to a biological treatment for aqueous effluents.