Caffeine and diclofenac are molecules with high human intake, and both belong to the ‘emergent’ class of contaminants. These compounds have been found at different concentrations in many sources of water worldwide and have several negative impacts on aquatic life systems; that is why the search for new alternatives for their removal from aqueous media is of transcendental importance. In this sense, adsorption processes are an option to attack this problem and for this reason, biochar could be a good alternative. In this regard, were prepared six different biochar from fique bagasse (FB), a useless agroindustry by-product from fique processing. The six biochar preparations were characterized through several physicochemical procedures, while for the adsorption processes, pH, adsorption time and concentration of caffeine and diclofenac were evaluated. Results showed that the biochar obtained by pyrolysis at 850 °C and residence time of 3 h, labeled as FB850-3, was the material with the highest adsorbent capacity with values of 40.2 mg g−1 and 5.40 mg g−1 for caffeine and diclofenac, respectively. It was also shown that the experimental data from FB850-3 fitted very well the Redlich–Peterson isotherm model and followed a pseudo-first and pseudo-second-order kinetic for caffeine and diclofenac, respectively.