Aquifers are increasingly threatened by the uncontrolled release of non-biodegradable chemicals derived from anthropogenic activities. The development of new remediation strategies has therefore focused on the use of sustainable adsorbent materials, including synthetic organic hydrogels and biochars produced from agricultural residues. In this study, the removal of two organic pollutants, the herbicide Metribuzin (MEB) and Propyl Paraben (PrP), from aqueous environments was investigated using negatively charged hydrogels and biochars derived from lime peel, respectively. Propyl Paraben (PrP) and Metribuzin (MEB) are among the pollutants frequently found in aquatic environments, and the effective and sustainable removal approaches remain under investigation. The hydrogels studied (P(DMAM co-ANax)) were based on sodium methacrylate (ANa) copolymerized with N,N-dimethylacrylamide (DMAM). The adsorption performance of the materials was evaluated through UV-Visible absorption spectrophotometry and High-Performance Liquid Chromatography (HPLC). The results of this study showed that the hydrogel achieved a very high removal efficiency for MEB, which was over 80% for the concentration range studied (max = 0.386 mg/g). Similar behavior was also recorded for the biochar from lime peel, which achieved almost complete removal of PrP (~100%) at the lowest concentrations of the contaminant (5 mg/L) and maintained high removal rates (78%) at 10 mg/L (max = 0.187 mg/g). These results demonstrate the potential of both types of materials to efficiently remove the studied contaminants from water, indicating their suitability for environmental remediation applications. This work contributes to the development of cost-effective and eco-friendly adsorbents for the treatment of water pollution caused by emerging organic compounds.