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CO2超临界流体、闪式提取槐花和花生废弃物中有效成分工艺研究

Studies on the Technology of Supercritical CO2and Homognate Extraction of Active Components from Sophora Japonic a and Peanuts Waste Meterial

【作者】 朱晓娜

【导师】 李明静;

【作者基本信息】 河南大学 , 分析化学, 2012, 硕士

【摘要】 我国槐花和花生资源丰富,槐花、花生壳中的黄酮类物质和花生红衣中的多酚类物质具有多种生理活性,广泛应用于食品、药品、化妆品和保健品等领域。本论文以国槐槐花和开封近郊的花生废弃物为研究对象,建立了CO2超临界流体提取槐花和花生壳总黄酮的工艺;并采用高速逆流色谱从槐花中分离制备了两种黄酮类物质;同时建立了花生红衣总多酚的闪式提取工艺。主要内容如下:1、槐花和花生废弃物的研究进展对近年来国内外学者关于槐花、花生壳黄酮和花生红衣多酚类物质在提取、分离纯化和含量测定方面进行简要综述,阐述了其主要的生理活性,针对传统提取工艺溶剂消耗大、提取时间长等缺点,在此基础上提出了本论文的研究课题—建立新的“绿色”、高效的提取工艺的必要性。2、槐花和花生壳总黄酮的CO2超临界流体提取的工艺研究通过正交试验确定了CO2超临界流体提取槐花和花生壳总黄酮的工艺条件,筛选出十二烷基苯磺酸钠对槐花总黄酮提取工艺进行优化。确立了槐花总黄酮最佳的提取工艺:十二烷基苯磺酸钠的质量分数为2%,夹带剂为75%的乙醇溶液,提取压力为350bar,提取温度为50℃,在此条件下,槐花总黄酮的平均提取率为32.16%。确定了CO2超临界流体提取花生壳总黄酮最适宜的表面活性剂为十二烷基硫酸铵,十二烷基硫酸铵的加入,使花生壳总黄酮的提取率达到28.39%,比没有加表面活性剂时提高了0.822倍。3、离子液体在高速逆流色谱分离制备槐花黄酮中的应用研究以正己烷-乙酸乙酯-乙醇-水-冰醋酸(1:1:1:1:0.05, v/v)为两相溶剂体系,应用高速逆流色谱对槐花黄酮粗提物进行分离,可从50mg槐花黄酮粗提物中一步分离制备得到芦丁18.2mg,槲皮素9.6mg,其纯度均在97%以上。1mL离子液体1-丁基-3-甲基咪唑六氟化硼酸([Bmim]BF6)的加入使出峰时间由原来的85min提前到55min,分离度由0.9提高到1.8,达到完全分离,分离效果得到明显改善。4、花生红衣总多酚的闪式提取与纯化工艺研究通过单因素实验和正交试验,确定了闪式提取花生红衣总多酚最佳工艺条件:乙醇浓度80%,料液1:25(g/mL),提取功率90V,提取两次,每次2min,此工艺条件下,花生红衣总多酚的平均提取率为96.94%。利用AB-8树脂对花生红衣总多酚进行富集纯化,纯化后的总多酚产品纯度为63.76%,得率为12.3%。所得到的花生红衣多酚纯度高,可为今后进一步开发利用打下基础。

【Abstract】 Sophora japonica L. and peanuts are rich natural resources in China. Polyphenols of peanut testa andflavonoids of Sophora japonica and peanut shells with a variety of biological activity are widely used inthe fields of food, medicines, cosmetics and health products. In this paper, we take the Sophora japonicaand waste meterial of peanut in Kaifeng outskirts as research subject. The optimum technology ofextracting total flavones of Sophora japonica.and peanut shell by supercritical CO2was established.Moreover high-speed countercurrent chromatography was developed for separating two flavonoids fromSophora japonica. And the technology of homogenate extraction was developed to extract the totalpolyphenol of peanut testa. The main contents are as follows:1. Review on the development of Sophora japonica. and peanut waste materialA brief overview of Sophora japonica and peanut waste meterial in recently years is reviewed,inclcding extraction, separation, purification, determination and physiological activity, and theshortcomings of traditional extraction process are summarized. On these basises, we put forward thesubject–to create a new "green" and efficient extraction process.2. Study on technology of supercritical CO2extraction of total flavones from Sophora japonicaand peanut shellAdding the sodium dodecyl benzene sulfonate (SDBS), the extraction rate of total flavones fromSophora japonica increased by0.937times. The optimal technology parameters: temperature50℃,pressure350bar, SDBS amount2%,75%ethanol concentration. Under these conditions, the averageextraction rate of total flavones was32.16%. The most suitable surfactant to extract total flavones from peanut shells by supercritical CO2wasammonium lauryl sulfate. The addition of ammonium lauryl sulfate enhanced Peanut shells flavonoids’extraction to28.39%, which was0.822times than that without added surfactant.3. Application of ionic liquids in separation and preparation of the two flavonoids of Sophorajaponica by HSCCCTwo flavonoids were prepared, isolated and purified from Sophora japonica by high-speedcountercurrent chromatography (HSCCC) using ionic liquids to improve the separation effect. A two-phasesolvent system composed of n-hexane-ethylacetate-ethanol-water-acetic acid (1:1:1:1:0.05, v/v) was used.The results indicated that18.2mg of rutin and9.6mg of quercetin with their purities over97%wereobtained from50mg crude extract of Sophora japonica. The peak time was advanced from85min to55min by adding Ionic liquids, the degree of separation from0.9to1.8, which had achieved completeseparation. The separation was significantly improved. The established method can be used for theseparation and purification of flavonoids from the Sophora japonica.4. Homogenate extraction and purification of the total polyphenol from peanut red flashThe optimum technology of extracting total Polyphenols of peanut testa by homogenate extractionwas established using single factor experiment and orthogonal test. The optimum extraction conditionswere as follows: ethanol concentration of80%, solid to liquid ratio of1:25(g/mL),90V power, two timesextraction, each for2min. Under this conditions, extraction rate of total polyphenols was96.94%.Polyphenols were enriched and purifted by AB-8resin. The purity and yield of the purified polyphenolproduct was63.76%and12.3%, respectively.

  • 【网络出版投稿人】 河南大学
  • 【网络出版年期】2012年 10期
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