Gabriel Cabral da Fonseca, Marcela Konjevod, Ameer Y. Taha, Roberto Fernández de Luis, Maibelín Rosales, Rosa M. Alonso, S. Lanceros‐Méndez, Antonio Veloso-Fernández, Erlantz Lizundia, Jorge Sáiz
Per- and polyfluoroalkyl substances (PFAS) are a class of persistent and bioaccumulative contaminants of emerging concern increasingly detected in water bodies worldwide, presenting serious environmental and human health risks. In this study, we designed and developed a sustainable, bifunctional cryogel adsorbent based on the combination of natural biopolymers (including bacterial cellulose, chitosan, and pectin) for the simultaneous adsorption of 27 short- and long-chain PFAS from aqueous matrices. When integrated into solid-phase extraction (SPE) cartridges, the cryogel enabled the simultaneous extraction of 27 PFAS, outperforming a commercial Oasis WAX/GCB cartridge for long-chain PFAS while maintaining recoveries above 50% for short-chain species. The material was successfully applied to the determination of PFAS in river water samples using SPE–LC–MS/MS, detecting perfluoroalkyl acids, fluorotelomer sulfonates, and chlorinated PFAS at ppt and sub-ppt levels. A cradle-to-gate life cycle assessment revealed a reduced carbon footprint of 53.2 kg CO₂-eq per kg of cryogel, highlighting the environmental advantages of this biopolymer-based platform. Overall, this work demonstrates the potential of biopolymer cryogels as environmentally sustainable and effective adsorbents for PFAS extraction and analysis in water monitoring applications.