藏木香活性成分提取及质量标准研究

NWIPB OpenIR

	藏木香活性成分提取及质量标准研究
	续艳丽
学位类型	硕士
导师	胡凤祖
	2010-05
学位授予单位	中国科学院研究生院
学位授予地点	北京
学位专业	植物学
关键词	藏木香土木香内酯异土木香内酯菊糖超临界co2萃取超声波提取质量标准
摘要	藏木香（Inula racemosa Hook.f）为菊科（Compositae）旋覆花属（Inulae）植物。以根入药，是藏医、蒙医常用药材，具有行气镇痛、健脾消食、温中和胃、胸腔胀痛、食积不消等功效。现代药理学研究表明，藏木香中含有丰富的菊糖，土木香内酯和异土木香内酯等活性成分，具有驱虫、抑菌、降血糖、助消化，显著的抗炎、保肝活性，可抑制感染人型结核杆菌和清除活性氧自由基等作用。藏木香大部分作为生药入药，虽有少数提取物，但都采用传统的有机溶剂萃取，工艺复杂、效率低，纯度不高，留有溶剂残留。超临界CO2萃取技术是目前世界上从动植物中提取有效成分的先进生物分离技术，操作简单、安全、高效、无溶剂残留，可以生产极高附加值的产品。本论文选用青海栽培藏木香为原料，以土木香内酯和异土木香内酯的收率为考察指标，通过正交实验优化了超临界CO2萃取藏木香倍半萜类活性成分的工艺条件，并对提取物的分离纯化、质量标准制定，超临界CO2萃取后藏木香残渣中菊糖的提取工艺条件等进行了研究，得到以下结论： 1. 对藏木香传统溶剂提取法进行研究，并与超临界CO2萃取结果进行比较。结果表明，超临界CO2萃取藏木香具有产率高，活性成分含量高，无溶剂残留等优点，具有实际工业应用价值。 2. 通过单因素试验，研究了萃取压力、萃取温度、萃取时间、CO2流量、原料粒度等因素对萃取效果的影响，从而确定适宜的萃取范围。 3. 以单因素试验结果为依据，通过四因素三水平正交试验对超临界CO2萃取工艺进行了优化。最佳工艺条件为：萃取压力20 MPa；萃取温度40 ℃；分离釜Ⅰ压力：6.5 MPa；分离釜Ⅰ温度50 ℃；分离釜Ⅱ压力：4.5 MPa；分离釜Ⅱ温度55 ℃；CO2流量40 L/h；萃取时间45 min；原料粒度：40目。在此条件下萃取，萃取物得率达5.45 %，萃取物中土木香内酯和异土木香内酯两种主要活性成分的含量达65.12 %。 4. 对超临界萃取物进行了GC/MS组分分析，鉴定出了12个组分，占总出峰面积的96.81 %，并用面积的归一法确定了各组分的相对百分含量，其中土木香内酯和异土木香内酯的含量最高，分别占49.31 %，44.12 %。两者总含量达93.44 %，说明藏木香超临界萃取物中主要活性成分含量高，杂质少。藏木香超临界CO2萃取物通过硅胶柱色谱，薄层色谱进行分离纯化，分离得到化合物1，经薄层色谱、HPLC、NMR等鉴定为异土木香内酯。 5. 为规范藏木香提取物的质量标准研究，制订了藏木香提取物标准草案。 6. 以提取时间、料液比、提取温度为主要影响因素，菊糖含量和浸膏得率为评价指标，通过星点设计-效应面法优化超声波提取藏木香残渣中菊糖的工艺条件，最佳工艺条件为：藏木香粉末加14倍水，60 ℃下，超声提取20 min。浸膏得率达12.9 %，菊糖含量为81.4 %。用星点设计-效应面法优化藏木香菊糖的提取工艺方法简便，预测性好。
其他摘要	Inula racemosa belongs Compositae, Inulae, is one of the traditional herb remedies in Tiben and Mongolian medicine, roots of which can be used as medicine and possess many pharmacologica effects, such as promoting circulation and analgesic effect, invigorating spleen and helping digestion effect and so on. Modern pharmacological study indicates that inulin, alantolactone and isoalantolactone were considered the main active constituents, and ting live, regulating heart, antivirus and anti-cancer. anti-inflammation, bacteriostasis, protec- Inula racemosa was mainly used as crude drug. Although there were some extract, it was extracted by organic solvent, and complicated process, low yield, low purity, and residual organic solvent. The supercritical CO2 extraction method was an advanced bioseparation technology, which can extract active constituents from animals and plants. Consulting document, there were no report about the extract craft of Inula racemosa. So the thesis used Inula racemosa which cultivated in Qinghai provice as raw material. Factors which based on arrange orthogonal experiments were selected to extract sesquiterpenes active constituents by supercritical CO2 technology. This thesis also study on component analysis, purification, and quality specification formulation of extract, and the condition of inulin in the residue after extracting by supercritical CO2 technology. The following conclusions was arrived at: ⑴ Traditional solvent methods were researched and compared with the supercritical CO2 extraction. The results showed that supercritical CO2 extraction method has higher rate of yield and content of active compenent, no pollution. Considering the inlfluence of every aspect, the erxtract of Inula racemosa by supercritical CO2 is of the industrial value. ⑵ In order to find the best extraction conditions, the single experiments of extraction pressure, extraction temperature, extraction time, dioxide flux, particle size were respectively carried out to determine suitable extraction range. ⑶ Based on the results of single factors experiment, extraction pressure, extraction temperature, extraction time and dioxide flux were selected as influencing factors to arrange orthogonal experiments. The suitable extraction conditions obtained as follows: extraction temperature 20 MPa; extraction temperature 40 ℃; separation pressureⅠ6.5 MPa; separation temperature Ⅰ50 ℃; separation pressureⅡ 4.5 MPa; separation temperature Ⅱ55 ℃; extraction time 45min; particle size 40 order. Under the condition, the overall yield of the extraction attained 5.45 %, and the content of alantolactone and isoalantolactone attained 65.12 %. ⑷ Thirteen compounds in the extraction of Inula racemosa have been identified by GC-MS, and the relative content of is totally higher than 89 %, and the total content of main active components attained 93.4 %. Using silica gel chromatogram and thin-layer chromatography to purificate the extract, compound 1 was obtained, which was identificated to be isoalantolactone by thin-layer, HPLC, and NMR. ⑸ In oder to specify extract of Inula racemosa, formulated ground-plan of extract of Inula racemosa. ⑹ The main influencing factors of extraction effect included the quantity of extraction time, extraction temperature and the ration of solvent to solid, the extraction conditions were evaluated by the extract yield and the contents of inulin. The optimal extraction of inulin was selected by central composite design-response surface methodology. The result showed that the optimal conditions consisted of the ration of solvent to solid 14 times, extraction temperature 60 ℃,and extraction time 20 min. under this condition, the yied was 12.9 %, and the content of the inulin is 81.4 %.
学科领域	植物学
语种	中文
文献类型	学位论文
条目标识符	http://210.75.249.4/handle/363003/3388
专题	中国科学院西北高原生物研究所
推荐引用方式 GB/T 7714	续艳丽. 藏木香活性成分提取及质量标准研究[D]. 北京. 中国科学院研究生院,2010.

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