<p>Adsorptive removal and photocatalytic degradation of organic pollutants in wastewater is an important process in terms of energy and cost in water decontamination. This study focused on the development of a nanocomposite in which both mesoporous TiO₂ and boron were integrated into SBA-15 matrix for the production of photocatalyst with effective adsorptive and photocatalytic potential. SBA-15-mesoTiO₂-B(X) nanocomposites were prepared by grafting boron at different molar ratios onto the SBA-15-mesoTiO₂ prepared by sol–gel synthesis and tested in the adsorption followed by photocatalysis of Doxorubicin (DOX) anticancer agent. FT-IR analysis indicated that Ti–O–Si and Ti–O–B bonds were formed for boron-grafted photocatalysts. XRD analysis disclosed that substitutional Ti was placed in the amorphous channels of SBA-15, and N₂-adsorption/desorption analysis revealed an increase in surface area up to 1001.2 m²/g. The highest photoactivity was obtained with SBA-15-mesoTiO₂-B(0.5) nanocomposite toward DOX (91% discoloration efficiency). Moreover, almost complete degradation of DOX was achieved, which is the ultimate goal for water pollution removal. XPS and UV/Vis analyses have proven that substitutional and interstitial incorporation of boron causes the formation of surface defects and also increase photoactivity with the presence of different Ti environments. From the scavenge test, it was concluded that the major reactive species responsible for DOX degradation were •OH radicals, and no significant degradation was caused by •O₂ ⁻ radicals. Furthermore, the success of the prepared photocatalyst in reuse with only 22% loss was also considerably high. This study provides insights into the potential application of SBA-15-mesoTiO₂-B(X) nanocomposites for combined adsorption/photocatalysis wastewater treatment process.</p>