Rivera-Tovar, Pamela RaquelContreras-Contreras, GabrielaRivas-Reyes, Paulina IsabelPérez-Jiménez, JaraMartínez-Cifuentes, MaximilianoPérez-Correa, José RicardoMariotti-Celis, María Salomé2025-04-102025-04-102025-02-21Antioxidants, Vol.14, N°3, 250 (2025) p. 1-20https://hdl.handle.net/20.500.12254/4091The rising demand for bioactive compounds from marine resources highlights the need for sustainable separation technologies. This study introduces an integrated process combining ultrasound-assisted extraction (USAE) and resin purification (RP) to isolate phlorotannins from Durvillaea incurvata, a brown seaweed with significant biomedical potential. Using a 32.5% ethanol–water solvent system for USAE followed by RP on Diaion HP-20 resin, phlorotannins were enriched 2.4-fold, with simultaneous removal of interfering compounds such as mannitol (~100%), which was demonstrated by FTIR and HPLC-IR analysis. Advanced characterization using UHPLC-QToF-MS/MS identified five novel phlorotannins with polymerization degrees of 3 to 8 phloroglucinol units in both USAE extracts and post-RP. Mass balance based on spectrophotometric measurements indicated a purification factor of ~2, confirming process effectiveness. RP streams showed distinct phlorotannin profiles, with one phlorotannin exceeding 70% relative abundance. However, MS/MS results showed significantly lower recoveries than spectrophotometric data, revealing a novel insight into RP purification. These findings highlight the critical role of comprehensive chemical characterization in optimizing sustainable phlorotannin extraction from seaweed. They propose a framework for scalable, eco-efficient technologies for achieving high-purity phlorotannin recovery. This approach facilitates the development of phlorotannin-based applications in the nutraceutical and pharmaceutical industries.enAtribución-NoComercial-CompartirIgual 3.0 Chile (CC BY-NC-SA 3.0 CL)UHPLC-QToF MS/MSBrown seaweedIntegrated extraction–purification processesSpectrophotometricMass balanceArticlehttps://orcid.org/0000-0001-8064-3070https://orcid.org/0009-0001-7376-4656https://orcid.org/0000-0003-1357-812Xhttps://doi.org/10.3390/antiox140302502076-3921