Ultrasonic-Assisted Water-Rich Natural Deep Eutectic Solvents for Sustainable Polyphenol Extraction from Seaweed: A Case Study on Cultivated .

This case study introduces a green, 1 h single-step method using water-rich natural deep eutectic solvent (WRNADES) for ultrasound-assisted extraction (UAE) of polyphenols from, a commercially cultivated brown seaweed. The extraction efficiency was evaluated using a selective quantitative NMR method (s-qNMR) and the traditional nonselective colorimetric total phenolic content assay (TPC). Initial 6 h extractions in traditional solvents (methanol, ethanol, acetone, and ethyl acetate) showed a 40-60% increase in polyphenolic yields in 50% aqueous solutions measured by the TPC method. Six different water-rich (50%) NADES (WRNADES) combinations were tested (choline chloride/betaine with lactic acid, citric acid, and 1,3-butanediol), with betaine and 1,3-butanediol (1:1) proving most effective. Parameters for the WRNADES were optimized using Box-Behnken design response surface methodology, resulting in a 1:20 w/w biomass to solvent ratio and a 1 h extraction time at 50 °C. The WRNADES extraction process was refined into a scalable, single-step procedure and compared with traditional solvent extractions (6 h, 50% aqueous methanol and acetone). A final XAD-7 polyphenol recovery step was included in all extractions. The optimized WRNADES extraction yielded 15.97 mg GAE/g of the dry weight recovered polyphenolic extract (s-qNMR), exceeding the 6 h 50% aqueous methanol (12.4 mg GAE/g) and acetone (11.4 mg GAE/g) extractions. Thus, the UAE-WRNADES method presented in this case study provides a cost-effective, sustainable, and eco-friendly alternative for the extraction of phenolic compounds from seaweed. It promotes the development of environmentally friendly production processes within the seaweed biorefinery.