| Summary: | <i>Hizikia fusiforme</i> has a long history of consumption and medicinal use in China. It has been found that natural plants containing polyphenol–polysaccharide complexes have better activity compared with polyphenols and polysaccharides. Therefore, in this study on enzymatic hydrolysis and fractional alcohol precipitation, two kinds of polyphenol–polysaccharide complexes (PPC), PPC1 and PPC2, were initially obtained from <i>Hizikia fusiforme</i>, while the dephenolization of PPC1 and PPC2 produced PPC3 and PPC4. Through in vitro assays, PPC2 and PPC4 were found to have higher antioxidant activity, and thus were selected for testing the PPCs’ anti-aging activity in a subsequent in vivo experiment with D-gal-induced aging in mice. The results indicated that PPCs could regulate the expressions of antioxidant enzymes and products of oxidation, elevate the expressions of genes and proteins related to the Nrf2 pathway in the mouse brain, enrich the gut microbiota species and increase the <i>Bacteroidota</i>–<i>Firmicute</i> (B/F) ratio. Above all, the <i>Hizikia fusiforme</i> polyphenol–polysaccharide complex has potential in the development of natural anti-aging drugs.
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