响应面优化超声辅助低共熔溶剂提取惠白菊总黄酮工艺

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

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。

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.

关键词

低共熔溶剂 / 总黄酮 / 超声辅助 / 响应面 / 工艺优化

Key words

Deep eutectic solvent / Total flavonoids / Ultrasound-assisted / Response surface optimization / Process optimization

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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