The method based on photogeneration of reactive oxygen species in water from catalyst composed of palygorskite-TiO2 and silver nanoparticles (AgNPs/TiO2-PAL) was developed and applied to antioxidant assays. Silver nanoparticles were synthesized using silver nitrate solution, sodium borohydride reducing agent and Caraia gum as stabilizing agent. Incorporation of AgNPs into the previously synthesized TiO2-PAL was performed. The catalyst AgNPs/TiO2-PAL were characterized by UV-vis spectroscopy, X-ray diffractometry (XRD), Scanning Electron Microscopy (SEM), Zeta potential and Dynamic Light Scattering (DLS). The catalyst AgNPs/TiO2-PAL were used to perform an antioxidant activity method which consisted in monitoring the dye discoloration , acid yellow 73 (AY73) in the presence of gallic acid antioxidant in different concentrations (10 to 100 μg.mL-1) comparing to the dye discoloration in the absence of the antioxidant. A microplate reader (Elisa Polaris) was used to measure the discoloration of the aqueous solutions of AY73 dye, irradiated by UV light for 60 minutes. The effect of reactive oxygen species (ROS) generated by AgNPs/TiO2-PAL based in photocatalytic kinetics of AY73 dye was investigated. The oxidation of AY73 dye by photocatalysis in the system with AgNPs/TiO2-PAL catalysts was carried out mainly by the participation of O2•-, HO• and 1O2 species, in this order of importance. The results showed that the synthesis of the AgNPs/TiO2-PAL catalyst was successfully carried out and the application of this material in the development of an innovative methodology for the determination of antioxidant activity was extremely promising.