Photocatalytic degradation experiments were done with lignin sulfonate in a circulating reactor. Catalysts (TiO 2-P25-SiO 2 + Pt, TiO 2-P25-SiO 2, TiOSO 4 _30.6 wt%, ZnO + TiO 2-P25-SiO 2), synthesized via the sol-gel method, were immobilized on porous glass support material. A comparative study was done regarding morphology of coatings, degradation rates, reaction rates, dissolved carbon (DC), formation of peaks, and fluorescence of products formed from the photocatalytic degradation of lignin sulfonate obtained from a local paper plant. Through simultaneous reaction-extraction pathways applying dialysis filtration and highly porous polystyrene divinylbenzene adsorbent resin (HR-P) for solid-phase extraction (SPE), an attempt was been made to isolate smaller molecules produced from photocatalytic degradation. Moreover, relatively high lignin sulfonate (0.5 g/L) concentrations are used in the reactions. UV-Vis spectroscopy revealed a faster reduction in the concentration values for the aliphatic moiety compared to the aromatic moiety. Peaks were observed by both fluorescence spectroscopy and high-performance liquid chromotography (HPLC), suggesting the production of new substances and fluorophores.