离子液体提取山楂绿原酸的工艺优化

    Process optimization of chlorogenic acid extraction from Crataegus Pinnatifida Bge using aqueous ionic liquid

    • 摘要: 绿原酸是许多植物中的活性成分,因其有显著的药理活性和生物活性而被广泛关注,选择合适的提取溶剂、提取方法和工艺参数是绿原酸得以进一步应用的重要环节。该文以离子液体为溶剂,采用超声辅助方法提取山楂中的绿原酸,首先选择离子液体种类,再通过单因素试验确定离子液体浓度、提取时间和固液比3个主要因素的参数,并用响应面法分析法优化提取工艺参数。结果表明,优化工艺为以离子液体1-乙基咪唑盐酸盐EImCl的水溶液为提取溶剂,当其浓度为1.19 mol/L,固液比为1∶19.67 g/mL,每次提取时间为42.83 min时,理论的绿原酸提取率为4 179.48 ?g/g,获得工艺参数的回归模型。验证试验绿原酸提取率为4 128.28 ?g/g,与模型符合很好。另外,因离子液体的价格昂贵、难降解和不可预知的毒性,进行了离子液体和目标物质的分离操作,在酸性条件下,以乙酸乙酯为反萃取剂萃取出绿原酸,其得率为提取液中质量分数的96.3%;离子液体通过减压蒸馏、在65℃烘干后循环使用,提取率达到第1次的92.96%。此外,试验考察了离子液体与普通溶剂比较,在提取率上和循环使用上具有明显优势,是一种高效、绿色萃取溶剂。

       

      Abstract: Abstract: As an active component in many plants, chlorogenic acid (CA) received extensive attention, for it possess lots of pharmacological activities and biological activities. Selection of suitable extraction solvent, extraction method and technological parameters is an important step to further purification and application of CA. The extraction efficiency of organic solvent in extraction of CA from Crataegus Pinnatifida Bge (CPB) is higher than that of water, but it is restricted for its toxicity causing damage to the human body and the environment. As a green and environmentally friendly solvent, ionic liquid was attracting increasing attention in the field of extraction, and ultrasonic-assisted extraction (UAE) method with the advantages of easy-operating, time-saving, energy-efficient and high efficiency was widely applied. Extraction of CA from CPB using ionic liquids as the solvent with UAE method was studied in this paper. Firstly, ionic liquid was selected from seven kinds of ionic liquids in the study, then the single factor experiments provided the extraction efficiencies of three main factors involving the concentration of ionic liquid, extraction time and solid-liquid ratio; furthermore, response surface methodology (RSM) was applied to optimize the three parameters of extraction. The content of CA was confirmed by fluorescence spectrometer with standard curve method. The results showed that ionic liquid, EImCl, was selected as the suitable solvent, and the optimum conditions were EImCl concentration of 1.19 mol/L, solid-liquid ratio of 19.67 g/mL and extraction time of 42.83 min, which obtained a theoretical CA content of 4 179.48 mg/g. Under the optimum conditions, the verification experiment of the extraction of CA was carried out with the result of CA content of 4 128.28 mg/g, which was agreed well with the regression model. In addition, separation of ionic liquid and CA was finished due to that the ionic liquid is expensive, difficult to degrade and has unpredictable toxicity. Under acidic condition, CA in the ionic liquid was extracted using ethyl acetate as the extraction agent, in which yield of CA was 96.3% of that in the extract; while the purification of ionic liquid was operated by reduced pressure distillation in the rotary evaporator, then dried at 65℃ in the vacuum drying oven, and the extraction efficiency of CA reached 92.96% when it was recycled for extraction of CA. Moreover, the comparison between the ionic liquid and traditional solvent by experimental investigation indicated that ionic liquid has obvious advantages in the extraction efficiency and recycling, and is a kind of high efficient, green extraction solvent.

       

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