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<p>This study investigated a synergistic deep eutectic solvent (DES)–ethanol system combined with sequential shaking and ultrasound-assisted extraction (UAE) to maximize recovery of bioactive compounds from <i>Diospyros kaki</i> peel. Among the tested DES formulations, choline chloride–lactic acid (DES01) achieved the highest extraction of total phenolics (TPC, 26.67&#xa0;mg GAE/g DW) and total flavonoids (TFC, 122.31&#xa0;mg QE/g DW), whereas 60% ethanol favored carotenoid recovery (20.41&#xa0;µg/g DW). Incorporating ethanol into DES reduced solvent viscosity and enhanced carotenoid extraction while retaining high phenolic and flavonoid yields. The DES:EtOH (60:40, v/v) system was selected as the most balanced extraction profile, defined as the combination achieving relatively high recovery of both polar (phenolics, flavonoids) and nonpolar (carotenoids) compounds simultaneously. Sequential shaking pretreatment followed by UAE further improved extraction, yielding TPC 28.61&#xa0;mg GAE/g DW, TFC 121.12&#xa0;mg QE/g DW, and carotenoids 26.19&#xa0;µg/g DW, supported by SEM evidence of extensive cell wall disruption. LC–MS coupled with feature-based molecular networking annotated 586 compounds from 2,506 features, dominated by quercetin-, kaempferol-, and catechin-type flavonoids. DES–Shaking + UAE extracts also exhibited the strongest antioxidant activities (DPPH 126.7&#xa0;µmol Trolox/g DW; FRAP 1.98&#xa0;mmol Fe<sup>2</sup>⁺/g DW) and digestive enzyme inhibition (IC₅₀ 0.96&#xa0;mg/mL for α-amylase; 0.56&#xa0;mg/mL for amyloglucosidase). Although ethanol partially dilutes the “green” character of DES, the relatively low ethanol proportion preserves the sustainability advantages of DES over conventional organic solvents. This integrated DES–ethanol and shaking–ultrasound strategy provides an efficient and environmentally considerate approach for valorizing persimmon peel as a high-value functional ingredient.</p>

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Synergistic DES–Ethanol Extraction Combined with Sequential Shaking–Ultrasound Improves Metabolite Profiling and Functional Bioactivities of Diospyros kaki Peel

  • 期刊论文

  • 发表日期：

    2026年4月14日

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  • Chi Hai Tran,
  • Thi Le Dung Huynh,
  • Thanh Sang Nguyen,
  • Van Man Phan

摘要

This study investigated a synergistic deep eutectic solvent (DES)–ethanol system combined with sequential shaking and ultrasound-assisted extraction (UAE) to maximize recovery of bioactive compounds from Diospyros kaki peel. Among the tested DES formulations, choline chloride–lactic acid (DES01) achieved the highest extraction of total phenolics (TPC, 26.67 mg GAE/g DW) and total flavonoids (TFC, 122.31 mg QE/g DW), whereas 60% ethanol favored carotenoid recovery (20.41 µg/g DW). Incorporating ethanol into DES reduced solvent viscosity and enhanced carotenoid extraction while retaining high phenolic and flavonoid yields. The DES:EtOH (60:40, v/v) system was selected as the most balanced extraction profile, defined as the combination achieving relatively high recovery of both polar (phenolics, flavonoids) and nonpolar (carotenoids) compounds simultaneously. Sequential shaking pretreatment followed by UAE further improved extraction, yielding TPC 28.61 mg GAE/g DW, TFC 121.12 mg QE/g DW, and carotenoids 26.19 µg/g DW, supported by SEM evidence of extensive cell wall disruption. LC–MS coupled with feature-based molecular networking annotated 586 compounds from 2,506 features, dominated by quercetin-, kaempferol-, and catechin-type flavonoids. DES–Shaking + UAE extracts also exhibited the strongest antioxidant activities (DPPH 126.7 µmol Trolox/g DW; FRAP 1.98 mmol Fe2⁺/g DW) and digestive enzyme inhibition (IC₅₀ 0.96 mg/mL for α-amylase; 0.56 mg/mL for amyloglucosidase). Although ethanol partially dilutes the “green” character of DES, the relatively low ethanol proportion preserves the sustainability advantages of DES over conventional organic solvents. This integrated DES–ethanol and shaking–ultrasound strategy provides an efficient and environmentally considerate approach for valorizing persimmon peel as a high-value functional ingredient.