This study focuses on establishing an efficient two-step technology, which includes: (1) consecutive adsorption-desorption, using cellulose-based membranes, bCells, and (2) photocatalytic degradation of the fungicide thiophanate-methyl (TPM), using synthesized Ag-P25 and Ce-P25 catalysts. The catalysts, obtained by controlled deposition of Ag2O/Ag and CeO2 onto P25 TiO2 carrier (Degussa), were characterized using ATR-FTIR, XRPD, BET, FESEM, HRTEM, HAADF-EDS and UV–DRS techniques. In order to establish a feasible purification technology, preconcentration of TPM was performed by adsorption, achieving 75.5 and 92.9 mg/g of TPM removal using bCell-EpL and bCell–EpL–TA membranes, respectively, followed by efficient desorption (> 95%) that provided acceptable TPM concentration for photodegradation experiments. Under optimal conditions (0.07 g/L of both catalysts), complete degradation of TPM (5 mg/L) occurred within 2 h, compared to 4 h for the base TiO2 P25. Measurements of quantum yield and the results of HPLC-MS analysis, alongside DFT calculation, assisted in understanding the TPM degradation pathways. New degradation products were detected and proposed from HPLC–MS analysis. Embryotoxic assays, performed on zebrafish (Danio rerio), applied to estimate the toxicity evolution of time-dependent generated TPM degradation products, showed low embryotoxic potential. Chemical oxygen demand (26 mg O2/L) confirmed low ecotoxicological pressure of effluent water.
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