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新疆雪莲化学成分的提取分离研究
张 富 昌
学位类型硕士
导师赵文军 ; 高 林
2007-06-20
学位授予单位中国科学院研究生院
学位授予地点北京
学位专业有机化学
关键词雪莲 超临界提取 挥发油 超临界耦合常规溶剂法 总黄酮 大孔树脂
摘要

雪莲花类药材为菊科风毛菊属(Saussurea DC),这类植物的全草或地上部分多用作生药,雪莲类药材主要分布于我国新疆、青海、甘肃、四川、云南和西藏等省区的高寒地区,常被用作生药的雪莲植物有12种和1个变种。其主要次生代谢成分含有黄酮、香豆素,木质素,生物碱、内酯、甾醇、多糖等。药理和临床证明雪莲有抗菌、抗辐射、抗寒、耐高山缺氧、强心、解痉镇静、平喘等功效。本文运用超临界CO2流体萃取技术对新疆雪莲进行了研究,以萃取率为指标,得出新疆雪莲适宜的萃取条件为 :萃取压力20 MPa,萃取温度45 ℃,动态萃取2.5小时。新疆雪莲挥发油的超临界萃出率(2.49%)比水蒸汽法(0.08%)高,并且选择性好。GC-MS分析超临界萃取物主要成分为不饱和脂肪酸,去氢木香内脂,长链烷烃,长链不饱和烯(醇)等。对新疆雪莲乙醇夹带剂超临界萃取部位进行分离纯化,从中分得6个化合物:β-谷甾醇(Ⅰ)、粗毛豚草素(Ⅱ)、4' ,5, 7- 三羟基-3',6-二甲氧基黄酮(Ⅲ)、槲皮素 (Ⅳ)、山奈酚(Ⅴ)、胡萝卜苷(Ⅵ)。提出了一种新的植物有效成分的提取方法——超临界耦合常规溶剂提取法,并用于新疆雪莲总黄酮的提取。试验结果表明此法能高效的萃取出植物中的有效成分,扩展了超临界技术在天然植物化学中的应用。运用大孔吸附树脂对雪莲黄酮粗提物进行富集纯化,优化工艺条件下能将黄酮含量为9.31%雪莲粗提物精制为黄酮含量为47±1%的雪莲提取物。实验表明该工艺简单,溶剂用量小,树脂可重复使用,是一种高效节能的新工艺。

其他摘要
Saussurea in Compositae is a large and polymorphic genus, mainly distributed in southwest and northwest of China (Xinjiang, Yunnan,Sichuan , Tibet,Qinghai) . About 12 species are used in traditional medicine to cure rheumatism disease, gynecological disease, etc. It was reported that flavonoids, maerolides, coumarins, steroids, lignans , alkaloids ,organic acids and sugars were obtained from the plants of Saussurea. Pharmacological activities mainly showed antitumor, anti-inflammatory and antifade. In Saussurea, Saussurea involucrate( Chinese name "XueLianHua") is commonly used. The volatile components of Saussurea involucrate was studied by use using of supercritical CO2 fluid extraction technology. The best results were obtained(pressure 20 MPa , temperature 45℃, time 2.5h)and the yield of volatile components was 2.56%, which also had a better selectivity for active constituents. Volatile constituents of Saussurea involucrate at 10 MPa and 20 MPa were analyzed by GC-MS. There are abundant unsaturated fatty acids, saturated fatty acids, dehydrocostuslactonein in the essential oil extracted from Saussurea involucrate. By utilization of a series of normal column chromatographic steps and filtration through SephadexLH-20, 6 compounds including β-sitosterol(Ⅰ), hispidulin(Ⅱ), 4',5,7-Trihydroxy-3',6-dimethoxy flavone(Ⅲ),quercetin(Ⅳ),kaempferol(Ⅴ) and β- daucosterol(Ⅵ) were isolated from supercritical CO2 fluid with ethanol as an entrainer extracts from whole plant of Saussurea involucrate. The structures of all compounds were elucidated by chemical and spectroscopic methods. It is reported a new method for extracting the active components from natural plants: the Supercritical technology coupled traditional method. By this method, we can enhance the extraction efficiency, lower the extraction temperature, shorten the extraction time, and reduce the losing of effective components. Our study developed a new application of supercritical technology in the extraction of natural resources. Macro-porous resins were used to purify the crude extracts of Saussurea flavonoids. HPD700 resin, with higher adsorption and easier desorption of Saussurea flavonoids was selected from five kinds of macro-porous resins through static adsorption and desorption experiments. the flavonoids content in the product was increased from 9.31% to 47±1% .
文献类型学位论文
条目标识符http://ir.xjipc.cas.cn/handle/365002/3491
专题资源化学研究室
作者单位中国科学院新疆理化技术研究所
推荐引用方式
GB/T 7714
张 富 昌. 新疆雪莲化学成分的提取分离研究[D]. 北京. 中国科学院研究生院,2007.
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