Emerging contaminants and pollution are environmental problems threatening public health. Antibiotic ciprofloxacin and methylene blue dye are pollutants frequently detected in water systems worldwide. Photocatalysis is a process for water treatment. TiO2-based catalysts synthesized with natural gums show improved photocatalytic properties. Here, the sol–gel method synthesized TiO2/Arabic gum for photocatalytic performance. The innovation of this work was synthesized at 400 °C and investigated their photocatalytic proprieties using methylene blue and ciprofloxacin as model pollutants. XRD showed that the photocatalyst was in the anatase phase. The result showed that TiO2 with a band gap of 3.29 eV was achieved at a calcination temperature of 400 °C. Corresponding FTIR results suggest only the existence of functional groups related to TiO2. The SEM and BET method characterization indicated that TiO2/Arabic gum were spherical-shaped nanoparticles arranged in clusters with a mesoporous structure, contributing to photocatalytic performance. In addition, photocatalytic studies showed that the methylene blue dye and ciprofloxacin antibiotic degradation rates reached 99% and 94% under UV light, respectively. The hole (h+) and OH ⦁ radicals are essential in photodegradation. The synthesized material showed excellent photostability and maintained almost the same degradation percentage in the three consecutive cycles tested on the different pollutants. The TiO2/Arabic gum is an excellent candidate for future use in treating contaminants in aqueous media using photocatalysis. Therefore, TiO2/Arabic gum nanoparticles are a promising material for wastewater treatment.