Antibiotic contamination of water sources is a significant environmental and public health concern. This contamination is classified among the most dangerous types of pollution currently because of their harmful effects. Therefore, it is essential to identify effective and environmentally friendly ways to deal with those dangerous compounds. Within this context, this video looked into whether soils made from volcanic ash could be used as cost-effective adsorbents to remove the antibiotic trimethoprim (TRM) from aqueous solutions. To examine the impacts of the main operating parameters on TRM removal, which are the initial antibiotic concentration (C), contact time (t), stirring speed (S), and solid-to-liquid ratio (R), a Central Composite Design (CCD) based on the Response Surface Methodology (RSM) was employed. Full quadratic polynomial models were used to correlate the experimental data, allowing for the estimation of each factor’s influence. With a predicted removal efficiency of 77.59%, the removal process optimization yielded the following set of optimal conditions: C = 4.5 mg/L, t = 45.5 min, S = 747 rpm, and R = 0.04 g/mL. Experiments conducted under predicted ideal conditions supported both the result and the previously developed model’s capacity for prediction. Additionally, the adsorption mechanism was also proposed based on the characterization of the adsorbent before and after the treatment. The study’s findings provide the possibility of using soils formed from volcanic ash as a cost-effective adsorbent material for the removal of TRM and likely other similar pollutants from contaminated waters.