Process Optimization for Polyphenol Extraction from Macroalgae Residues and Assessment of Their Compositions, Antioxidant Activities, and Glycosidase Inhibition

Macroalgae are often used to produce sodium alginate, but their by-products have not been fully utilized. This study aimed to optimize the extraction of bound polyphenols (BPs) from <i>Macrocystis pyrifera</i> (L.) residues, analyze the composition of free polyphenols (FPs) and BPs, and evaluate their antioxidant activities and ability to inhibit glycosidase activity. The optimal conditions for extracting BPs achieved by the response surface method were as follows: 50 °C, a solid-liquid ratio of 1:50, an alkaline hydrolysis time of 2.38 h, and a NaOH concentration of 8 mol/L. Polyphenol content determination results indicated that FPs had significantly higher total polyphenols (13.02 ± 0.05 μg GAE/mg) and phlorotannin (3.44 ± 0.04 μg PE/mg) than BPs (6.57 ± 0.07 μg GAE/mg and 1.32 ± 0.20 μg PE/mg). HPLC/ESI-QTOF-MS showed distinct profiles: FPs had one polyhydroxy phenol, nine flavonoids, and four additional compounds, whereas BPs had five flavonoids and four other compounds. Antioxidant activity was found to be higher in FPs than in BPs (DPPH: 3.03 vs. 1.79 μg TE/mg; FRAP: 19.40 vs. 7.43 μg TE/mg). Furthermore, FPs exhibited 4.59- and 11-fold higher inhibition capacity toward α-amylase and α-glucosidase, respectively, compared to BPs. The results provide valuable basic data for the application of macroalgae residues in the marine biological industry and reveal their potential hypoglycemic ability.