杜仲叶粗提物中高纯度绿原酸的制备工艺研究

发布时间：2018-03-10 09:03

  本文选题：绿原酸　切入点：高纯度　出处：《中国科学院烟台海岸带研究所》2017年硕士论文　论文类型：学位论文

【摘要】：绿原酸(CGA)作为一种重要的天然多酚物质,具有显著的降血压、滋肝润胆、抗菌、预防肿瘤等多种药理活性,是许多中成药的有效成分,近年来在不断受到人们的重视,并被广泛应用于化妆品、食品、医药等行业。因此,研究高纯度绿原酸的制备工艺技术,对我国国民经济和社会发展具有重要意义。本论文以杜仲叶粗提物为实验原料,通过严谨的实验设计,研究出了一条容易操作,稳定可靠的高纯度绿原酸制备工艺路线,并在此基础上进行了中试放大研究,所得主要研究结果如下:(1)定量方法的建立以高效液相色谱仪为检测仪器,建立了定量检测杜仲叶粗提物中绿原酸的方法,并对其进行方法学验证。结果显示,该HPLC法基线稳定,绿原酸与其他成分分离度高,回收率高,因此可以作为杜仲叶提取物中绿原酸的检测和定量分析方法。(2)大孔树脂初步分离纯化筛选出ADS-21最佳大孔吸附树脂,并发现该树脂在25℃条件时达到最大吸附量,同时满足Langmuir方程和伪二级动力学方程。ADS-21树脂分离纯化粗提物中绿原酸的最佳工艺条件为:1)吸附:吸附液pH=2,温度25℃,上样流速2 BV/h,上样浓度3.01 mg/m L,上样体积8 BV;2)解吸:解吸流速2 BV/h,乙醇浓度及用量为40%乙醇3 BV,50%乙醇10 BV。通过大孔树脂吸附解吸一次纯化后,得到绿原酸粗品的纯度由原来的5.01%提高到38.1%,提高了7.62倍,绿原酸回收率为92.8%。(3)树脂和硅胶除杂精制采用树脂和硅胶精制绿原酸粗品,通过研究得到X-5树脂除杂最佳工艺条件:pH≈6,当层析柱直径:高(cm:cm)=3.5:35时,料液比为M:V(g:mL)=1:10;硅胶除杂最佳工艺条件:当玻璃层析柱直径:高(cm:cm)=3.5:35时,料液比为M:V(g:m L)=1:100。解吸浓缩液通过硅胶和X-5型树脂吸附除杂后,绿原酸的纯度由38.1%提高到73.2%,产率65.3%。(4)活性炭脱色精制以活性炭为脱色材料对绿原酸粗精品进行精制,得到最佳脱色工艺条件为:1)吸附:200目以上活性炭,温度30℃,料液比M:V=2:50(g:mL),时间1.5 h;2)解吸:温度50℃,乙醇浓度50%,时间5 h,解吸量7 BV,解吸三次。通过活性炭脱色精制后,得到纯度为93.4%接近无色的绿原酸精品,产率为88.7%。(5)实验室放大研究实验室放大研究结果表明,放大实验和预实验所得绿原酸精品的纯度和总得率基本一致,均在92%和60%左右。因此,该工艺技术路线总体稳定,实用可靠,适用于从杜仲叶粗提物中工业化制备高纯度绿原酸。
[Abstract]:As an important natural polyphenol, Lv Yuan has many pharmacological activities, such as lowering blood pressure, nourishing liver and gallbladder, antibacterial, preventing tumor and so on. It is an effective component of many Chinese patent medicines, and has been paid more and more attention in recent years. It is widely used in cosmetics, food, medicine and other industries. Therefore, it is of great significance to study the preparation technology of high purity Lv Yuan acid for the development of national economy and society in China. In this paper, the crude extract of Eucommia ulmoides leaves is used as experimental material. Based on the rigorous experimental design, a stable and reliable process for the preparation of high purity Lv Yuan acid was developed, and on the basis of this, the pilot scale up study was carried out. The main results are as follows: (1) Establishment of quantitative method for quantitative determination of Lv Yuan acid in crude extract of Eucommia ulmoides leaves with high performance liquid chromatograph (HPLC). The results show that the baseline of this HPLC method is stable. Lv Yuan acid has high separation degree from other components and the recovery rate is high. Therefore, Lv Yuan acid can be used as a method for the detection and quantitative analysis of Lv Yuan acid in Eucommia ulmoides leaves extract. The macroporous resin can be preliminarily separated and purified by macroporous resin, and the best macroporous adsorption resin can be obtained. It was found that the maximum adsorption capacity of the resin was achieved at 25 鈩，

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