| Summary: | This study aimed to extract and purify polyphenols from <i>Acanthopanax senticosus</i>. A new green method was developed, in which ionic liquids (ILs) were used as aqueous two-phase (ATP) adjuvants to extract the polyphenols from <i>A. senticosus</i>. An ionic liquid-assisted aqueous two-phase system (IL-ATPS) was established. The purification of the polyphenols from the extraction fluid by AB-8 macroporous resin was conducted, and the kinetic mechanisms were studied. The reuse of ionic liquids was executed. The results showed that an [OMIM]Br-assisted ethanol/NaH<sub>2</sub>PO<sub>4</sub> system (IL-ATPS) was the best extraction solvent. In this study, the following optimal extraction conditions were determined: 32 wt.% ethanol, 25 wt.% NaH<sub>2</sub>PO<sub>4</sub>, 9 wt.% additional ionic liquid, a solid–liquid ratio of 1:40 g/mL, an extraction temperature of 50 °C, a pH of 4.0, an extraction time of 50 min, and an extraction rate of the polyphenols at 15.90 mg/g. The optimum adsorption parameters of the macroporous resin AB-8 were as follows: a flow rate of 3.5 BV·h<sup>−1</sup>, a sample volume of 40 mL, an elution flow rate of 3.5 BV·h<sup>−1</sup>, an eluent volume of 80 mL, and an eluant that was constituted by an 85% volume fraction of ethanol. The decolorization effect of 4% activated carbon was better than the other amounts; in addition, a decolorization rate of 76.81% and an ionic liquid recovery rate of 81.12% were found to be the most optimal. Compared with the traditional extraction methods, IL-ATPS has the advantages of requiring simple operation, saving time, and high efficiency. In addition, it can be used for the extraction of the polyphenolic compounds.
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