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山东大学学报 (医学版) ›› 2026, Vol. 64 ›› Issue (5): 29-41.doi: 10.6040/j.issn.1671-7554.0.2025.0835

• 重点专题——活性天然产物研究 • 上一篇    

响应面优化超声辅助低共熔溶剂提取惠白菊总黄酮工艺

王艳萍1,王玉波2,董林1,唐娜1,徐晴晴1,郭广君1,郭时金1,杨丽梅1,徐子贤1,张浩天3,张文勇4,徐倩倩1   

  1. 1.山东省滨州畜牧兽医研究院, 山东 滨州 256600;2.滨州医学院附属医院胸外科, 山东 滨州 256603;3.山东惠白菊农业发展有限公司, 山东 滨州 251702;4.惠民县菊润农业科技有限公司, 山东 滨州 251700
  • 发布日期:2026-05-13
  • 通讯作者: 徐倩倩. E-mail:qianqian19830125@163.com
  • 基金资助:
    国家自然科学基金(31872513);山东省自然科学基金面上项目(ZR2023MC212);2024年滨州市渤海科技创新券产学研合作“揭榜挂帅”项目

Optimisation of ultrasound-assisted deep eutectic solvent extraction of total flavonoids from Chrysanthemum morifolium using response surface methodology

WANG Yanping1, WANG Yubo2, DONG Lin1, TANG Na1, XU Qingqing1, GUO Guangjun1, GUO Shijin1, YANG Limei1, XU Zixian1, ZHANG Haotian3, ZHANG Wenyong4, XU Qianqian1   

  1. 1. Shandong Binzhou Animal Science and Veterinary Research Academy, Binzhou 256600, Shandong, China;
    2. Department of Thoracic Surgery, Binzhou Medical University Hospital, Binzhou 256603, Shandong, China;
    3. Shandong Huibaiju Agricultural Development Co., Ltd., Binzhou 251702, Shandong, China;
    4. Huimin County Jurun Agricultural Science and Technology Co., Ltd., Binzhou 251700, Shandong, China
  • Published:2026-05-13

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摘要： 目的 研究系统优化超声辅助低共熔溶剂(deep eutectic solvents, DES)提取惠白菊总黄酮工艺替代传统有机溶剂提取的改进方案,探讨其提取效率与环境友好性。 方法 筛选并制备8种DES;以总黄酮得率为指标,考察DES含水量、液料比、提取时间、温度及超声功率的影响;采用Box-Behnken响应面法优化提取工艺,并对提取物进行纯化和活性评价。 结果 甜菜碱-尿素(1∶2, mol/mol)为最佳DES(DES-1),其提取效率显著优于其他溶剂;DES-1含水量30wt%、液料比30 mL/g、温度40 ℃、超声时间30 min、功率320 W(80%),在该条件下总黄酮得率达(120.31±2.16)mg/g,较60%(v/v)乙醇回流法(96.19 mg/g)提升25.10%。经AB-8大孔树脂纯化后,总黄酮纯度提升至35.49%,且具有较强的1,1-二苯基-2-三硝基苯肼(1,1-piphenyl-2-picrylhydrazyl, DPPH)自由基清除能力(IC50=0.64 mg/mL)。 结论 甜菜碱-尿素DES联合超声提取技术可实现惠白菊总黄酮的高效绿色提取,兼具提取率提升(>25%)与环境友好优势,为天然产物绿色提取提供新策略。

关键词: 低共熔溶剂, 总黄酮, 超声辅助, 响应面, 工艺优化

Abstract: Objective To optimise the ultrasonic-assisted deep eutectic solvent(DES)extraction process for total flavonoids from Chrysanthemum morifolium(Huibaiju)in order to replace the traditional method of extraction using organic solvents, and to explore extraction efficiency enhancement and environmental friendliness. Methods A total of eight DES were synthesized and screened, and the effects of key parameters, such as DES water content, liquid-to-solid ratio, extraction time, temperature, and ultrasonic power were investigated based on total flavonoid yield.The critical parameters were modelled and optimised using Box-Behnken response surface methodology(RSM). The extracts were then purified and evaluated for activity. Results Betaine-urea DES(1∶2 molar ratio, denoted as DES-1)exhibited superior extraction efficiency under the following conditions: 30wt% water content in DES-1; a liquid-to-solid ratio of 30 mL/g; an extraction temperature of 40 ℃; 30 min of ultrasonication, and an ultrasonic power of 320 W(80%). Under these conditions, the total flavonoid yield was 120.31±2.16 mg/g, which is a 25.10% increase on the yield obtained using conventional 60%(v/v)ethanol reflux extraction(96.19 mg/g). Following purification using AB-8 macroporous resin, the total flavonoid purity increased to 35.49%, demonstrating a strong 1,1-diphenyl-2-picrylhydrazyl(DPPH)radical scavenging capacity(IC50=0.64 mg/mL). Conclusion The use of betaine-urea DES coupled with ultrasound-assisted extraction enables the efficient and eco-friendly recovery of total flavonoids from Huibaiju, achieving a yield that is over 25% higher while reducing environmental impact. This strategy provides a sustainable method of extracting natural products.

Key words: Deep eutectic solvent, Total flavonoids, Ultrasound-assisted, Response surface optimization, Process optimization

中图分类号: 

  • R284.2
[1] Gong JY, Chu BQ, Gong LX, et al. Comparison of phenolic compounds and the antioxidant activities of fifteen Chrysanthemum morifolium Ramat cv. ‘hangbaiju’ in China[J]. Antioxidants, 2019, 8(8): 325. doi:10.3390/antiox8080325
[2] Lii CK, Lei YP, Yao HT, et al. Chrysanthemum morifolium Ramat. reduces the oxidized LDL-induced expression of intercellular adhesion molecule-1 and E-selectin in human umbilical vein endothelial cells[J]. J Ethnopharmacol, 2010, 128(1): 213-220.
[3] 夏玲, 周桂生, 严辉, 等. 菊花提取工艺的优化[J]. 中成药, 2022, 44(8): 2636-2640. XIA Ling, ZHOU Guisheng, YAN Hui, et al. Optimization of extraction process for Chrysanthemum morifolium[J]. Chinese Traditional Patent Medicine, 2022, 44(8): 2636-2640.
[4] 李金凤, 刘华敏, 谷令彪, 等. 怀菊花中总黄酮的提取及其抗氧化性研究[J]. 食品工业科技, 2018, 39(11): 211-218. LI Jinfeng, LIU Huamin, GU Lingbiao, et al. Study on extraction of flavones in Huaiju Chrysanthemum and its antioxidant activity[J]. Science and Technology of Food Industry, 2018, 39(11): 211-218.
[5] Zhang ZJ, Hu WJ, Yu AQ, et al. Review of polysaccharides from Chrysanthemum morifolium Ramat.: Extraction, purification, structural characteristics, health benefits, structural-activity relationships and applications[J]. Int J Biol Macromol, 2024, 278(3): 134919. doi:10.1016/j.ijbiomac.2024.134919
[6] Roselli V, Leuci R, Pugliese G, et al. Deep eutectic solvents(DESs)as alternative sustainable media for the extraction and characterization of bioactive compounds from winemaking industry wastes[J]. Molecules, 2025, 30(8): 1855. doi:10.3390/molecules30081855
[7] Sahu S, Kumari D, Kusam, et al. Deep eutectic solvent extraction of polyphenol from plant materials: current status and future prospects in food applications[J]. Food Chem, 2025, 482: 144125. doi:10.1016/j.foodchem.2025.144125
[8] Jovanovi c J, Jovi c M, Trifkovi c J, et al. Green extraction of bioactives from Curcuma long ausing natural deep eutectic solvents: unlocking antioxidative, antimicrobial, antidiabetic, and skin depigmentation potentials[J]. Plants, 2025, 14(2): 163. doi:10.3390/plants14020163
[9] Peng WL, Wang XG, Wang WM, et al. Comparison, optimization and antioxidant activity of ultrasound-assisted natural deep eutectic solvents extraction and traditional method: a greener route for extraction of flavonoid from Moringa oleifera Lam. leaves[J]. Ultrason Sonochem, 2024, 109: 107003. doi:10.1016/j.ultsonch.2024.107003
[10] Martinovi c M, Krgovi c N, Neši c I, et al. Conventional vs. green extraction using natural deep eutectic solvents-differences in the composition of soluble unbound phenolic compounds and antioxidant activity[J]. Antioxi-dants, 2022, 11(11): 2295. doi:10.3390/antiox11112295
[11] 孙平, 董萍萍, 董丹华, 等. 超声波辅助低共熔溶剂提取野菊花总黄酮的工艺研究[J]. 食品工业科技, 2020, 41(20): 147-152. SUN Ping, DONG Pingping, DONG Danhua, et al. Ultrasound-assisted deep eutectic solvent extraction of total flavonoids from Chrysanthemum indicum[J]. Science and Technology of Food Industry, 2020, 41(20): 147-152.
[12] 黄文睿, 唐超凡, 陶雨峰, 等. 绿色低共熔溶剂提取野菊花中黄酮类化合物[J]. 精细化工, 2022, 39(3): 569-576. HUANG Wenrui, TANG Chaofan, TAO Yufeng, et al. Extraction of flavonoids from Chrysanthemum indicum L.by green deep eutectic solvents[J]. Fine Chemicals, 2022, 39(3): 569-576.
[13] Teixeira G, Abranches DO, Silva LP, et al. Liquefying flavonoids with terpenoids through deep eutectic solvent formation[J]. Molecules, 2022, 27(9): 2649. doi:10.3390/molecules27092649
[14] 向思颖, 鲁治宇, 张硕, 等. 超声辅助天然低共熔溶剂提取柚皮总黄酮及其抗氧化活性评价[J]. 粮食与油脂, 2024, 37(8): 78-84. XIANG Siying, LU Zhiyu, ZHANG Shuo, et al. Ultrasonic-assisted extraction of total flavonoids from pomelo peel by natural deep eutectic solvents and its antioxidant activity evaluation[J]. Cereals & Oils, 2024, 37(8): 78-84.
[15] 张霞. 低共熔溶剂在提取分离枸杞黄酮类化合物的应用[D]. 兰州: 中国科学院大学, 2020.
[16] 肖咪, 罗蓉, 赵红玉, 等. 超声波辅助低共熔溶剂提取淫羊藿总黄酮的工艺优化及其降糖活性研究[J]. 中国医院药学杂志, 2025, 45(2): 135-140. XIAO Mi, LUO Rong, ZHAO Hongyu, et al. Optimization of extracting total flavonoids from Epimedium brevicornu by ultrasonic-assisted deep eutectic solvent and their hypoglycemic activity[J]. Chinese Journal of Hospital Pharmacy, 2025, 45(2): 135-140.
[17] 杨枝中, 张文平, 张磊, 等. 超声辅助低共熔溶剂提取肾茶黄酮和多酚的工艺及其抗氧化活性[J]. 云南农业大学学报(自然科学), 2024, 39(3): 99-106. YANG Zhizhong, ZHANG Wenping, ZHANG Lei, et al. Ultrasonic-assisted extraction of flavonoids and polyphenols from Clerodendranthus spicatus by deep eutectic solvents and its antioxidant activity[J]. Journal of Yunnan Agricultural University(Natural Science), 2024, 39(3): 99-106.
[18] 关兆峰, 曾庆达, 吴昊, 等. 低共熔溶剂提取光果甘草渣中光甘草定和总黄酮及预处理效果[J]. 应用与环境生物学报, 2024, 30(2): 360-366. GUAN Zhaofeng, ZENG Qingda, WU Hao, et al. Extraction of glabridin and total flavonoids from Glycyrrhiza glabra L. residues using deep eutectic solvents and its pretreatment effect[J]. Chinese Journal of Appliedand Environmental Biology, 2024, 30(2): 360-366.
[19] 雷永伟, 刘欣, 安艳霞, 等. 低共熔溶剂提取荞麦壳黄酮的工艺优化[J]. 食品研究与开发, 2023, 44(13): 160-166. LEI Yongwei, LIU Xin, AN Yanxia, et al. Optimization of extraction technology of buckwheat hull flavonoids in deep eutectic solvent[J]. Food Research and Development, 2023, 44(13): 160-166.
[20] 赵慧, 杜会枝. 低共熔溶剂提取连翘不同部位总黄酮及抗炎抗氧化活性研究[J]. 山西大学学报(自然科学版), 2023, 46(3): 689-698. ZHAO Hui, DU Huizhi. Extraction of total flavonoids from different parts of Forsythia suspensa with deep eutectic solvents and its anti-inflammatory and antioxidant activities[J]. Journal of Shanxi University(NaturalScienceEdition), 2023, 46(3): 689-698.
[21] 邱志, 洋甘菊总黄酮的提取、分离及其护肤功效研究[D]. 广州: 华南理工大学, 2023.
[22] 李芳, 独一味总黄酮的提取纯化及抗炎抗氧化研究[D]. 济南: 山东中医药大学, 2022.
[23] 杨永涛. 罗布麻总黄酮的提取、分离纯化及其抗氧化性能研究[D]. 广州: 华南理工大学, 2018.
[24] Zhao JL, Zhang MP, Zhou HL. Microwave-assisted extraction, purification, partial characterization, and bioactivity of polysaccharides from Panax ginseng[J]. Molecules, 2019, 24(8): 1605. doi:10.3390/molecules24081605
[25] Liu YJ, Zhang H, Yu HM, et al. Deep eutectic solvent as a green solvent for enhanced extraction of narirutin, naringin, hesperidin and neohesperidin from Aurantii Fructus[J]. Phytochem Anal, 2019, 30(2): 156-163.
[26] Zhen SY, Chen S, Geng S, et al. Ultrasound-assisted natural deep eutectic solvent extraction and bioactivities of flavonoids in Ampelopsis grossedentata leaves[J]. Foods, 2022, 11(5): 668. doi:10.3390/foods11050668
[27] Jin L, Yun D, Zhang W, et al. Polyphenols coordinated with Cu(II)in an aqueous system build ion-channel coatings on hair surfaces[J]. Materials, 2023, 16(4): 1333. doi:10.3390/ma16041333
[28] Liu JH, Guo XS, Miao QW, et al. Deep eutectic solvent extraction of myricetin and antioxidant properties[J]. RSC Adv, 2024, 14(26): 18126-18135.
[29] Getachew AT, Holdt SL, Meyer AS, et al. Effect of extraction temperature on pressurized liquid extraction of bioactive compounds from Fucus vesiculosus[J]. Mar Drugs, 2022, 20(4): 263.
[30] 雷倩. 基于低共熔溶剂的超声辅助绿色高效萃取防己中生物碱类活性成分研究[D]. 赣州: 赣南师范大学, 2023.
[31] Li SS, Wang GY, Zhao JJ, et al. Ultrasound-assisted extraction of phenolic compounds from celtuce(Lactuca sativa var. augustana)leaves using natural deep eutectic solvents(nades): process optimization and extraction mechanism research[J]. Molecules, 2024, 29(10): 2385. doi:10.3390/molecules29102385
[32] Wu WX, Jiang S, Liu MM, et al. Simultaneous process optimization of ultrasound-assisted extraction of polyphenols and ellagic acid from pomegranate(Punica granatum L.)flowers and its biological activities[J]. Ultrason Sonochem, 2021, 80: 105833. doi:10.1016/j.ultsonch.2021.105833
[33] 杨欣欣, 包永睿, 王帅, 等. 防己生物碱类成分提取纯化工艺研究[J]. 中成药, 2014, 36(6): 1306-1309. YANG Xinxin, BAO Yongrui, WANG Shuai, et al. Extraction and purification process for alkaloids from Stephania tetrandra[J]. Chinese Traditional Patent Medicine, 2014, 36(6): 1306-1309.
[34] 李婷婷, 易超凡. 不同来源菊花总黄酮含量及其抗氧化活性研究[J]. 辽宁中医药大学学报, 2015, 17(5): 72-74. LI Tingting, YI Chaofan. Study on the contents of total flavonoids in Chrysanthemum from different sources and its antioxidant activity[J]. Journal of Liaoning University of Traditional Chinese Medicine, 2015, 17(5): 72-74.
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