<p>Pharmaceutical wastes have recently emerged as a significant source of water pollution, causing water-borne illness and significant changes to the aquatic biological cycle. Therefore, a high-performance adsorbent with high adsorption capacity, with less production cost and an environmentally friendly approach is required for wastewater treatment. The present study focuses on the methods of optimization, for the production of novel high-performance activated carbon from coconut husk (AcCH) by physical and chemical activation process, which emphasizes optimization technique based on Response Surface Methodology (RSM) of three activation variables namely; impregnation ratio of NaOH: Char, activation temperature, and activation time on the response evaluated by up taking carbamazepine and naproxen from aqueous solution. Both carbamazepine and naproxen uptake were maximized by optimizing the conditions for AcCH preparation, where the model’s predicted values agreed with the experimental results in a satisfactory manner. To evaluate AcCH potential for carbamazepine and naproxen adsorption, batch adsorption studies were conducted under various conditions, including different dosages of adsorbent, different initial concentrations of the adsorbate, pH of the experimental solutions, rpm, and temperature of the incubator shaker and kinetics, isotherm, and thermodynamic studies were also done. Adsorption data showed that the Langmuir isotherm fits the data best with an R² value of 0.999 for both carbamazepine and naproxen uptake. With the high surface area of 1241.8223 m².g⁻¹, the highest calculated adsorption capacity of AcCH for carbamazepine was 380.09&#xa0;mg.g⁻¹ and for naproxen 433.45&#xa0;mg.g⁻¹. Moreover, the result revealed that both carbamazepine and naproxen uptake by AcCH followed a pseudo-second-order kinetic model and the thermodynamic study’s negative ΔG value suggested that the adsorption process was spontaneous.</p>