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玉屏风复方有效成分群的提取与分离纯化
Extraction, Separation and Purification of Active Ingredients Group from Yupingfeng Compound
【作者】 李宏;
【导师】 杨克迪;
【作者基本信息】 广西大学 , 化学工艺, 2007, 硕士
【摘要】 玉屏风复方由黄芪、白术、防风组成,始载于元朝朱丹溪的《丹溪心法》,是临床上应用广泛的经典名方。本课题以玉屏风复方为研究对象,以其有效成分群的提取分离为目标,从以下几个方面进行了研究:(1)建立了黄芪甲苷的SPE-HPLC分析方法及复方中黄芪皂苷的含量分光光度法分析方法。(2)利用毛细管气相色谱-质谱联用(GC-MS)方法对玉屏风和白术挥发油化学成分进行分析和鉴定。结果表明,玉屏风复方挥发油以倍半萜类及其衍生物类为主,而白术挥发油中含量较大的赛切烯、α-芹子烯等成分在复方挥发油中未出现,复方中的挥发油组成并不是单味药材挥发油成分的简单加合。(3)以黄芪甲苷的含量及得率为目标,优化了黄芪中黄芪甲苷乙醇回流法提取工艺条件,即以药材质量15倍的55%乙醇在80℃下回流提取4小时;以色原酮苷和黄芪甲苷的含量及得率为目标,应用正交实验和单因素实验优化了玉屏风有效成分群—釜法提取工艺条件。最优工艺条件为:单位药材质量以10倍量80%的乙醇在70℃下回流提取4小时。(4)采用大孔树脂对玉屏风有效成分群进行了分离富集。考察了D101、S-8等七种树脂对玉屏风提取物中黄芪皂苷和色原酮苷的吸附量及解吸率,结果表明,D101、AB-8和X-5树脂对有效成分群吸附效果较好。进一步探讨了AB-8树脂固定床分离富集有效成分群时料液中有效成分群浓度、流速及洗脱剂组成、流速对穿透曲线、洗脱曲线的影响。结果表明,经AB-8树脂固定床分离富集后,提取物中黄芪皂苷含量由2.57%提高到39.27%,回收率为83.71%;升麻苷及5-O-甲基维斯阿米醇苷的含量分别由0.24%、0.31%提高到3.69%和6.34%,回收率分别为82.31%、91.03%,有效成分群得到有效富集。
【Abstract】 Yupingfeng compound composing of Astragali, Atractylodis macrocephala andSanposhnikoviae, is recorded in Dan Xi Xin Fa written by Zhu Dan-xi in dynasty Yuan, whichis a classic famous prescription medicine extensively used in clinical. Separation andpurification of the active ingredients group from Yupingfeng were studied, and the results areas follows:(1) Analysis methods for the determination of astragalosideⅣwith SPE-HPLC anddetermination of astragaloside with ultraviolet-visible absorption spectroscopy wereestablished.(2) Constituents of volatile oil from Yupingfeng compound and Atractylodismacrocephala were analyzed and identified by capillary GC-MS techniques. The resultsshowed that the volatile oil from Yupingfeng mainly contained sesquitrepenes and theirderivatives, The components including seyshellene andα-selinene had high content in volatileoil from Atractylodis macrocephala but were not discovered in volatile oil from Yupingfeng.The composition of volatile oil from compound was not the simple addition of those in singledrugs.(3) On the aim of extraction yield and content of astragalosideⅣ, the extractioncondition of astragalosideⅣextraction in Astragalus membranaceus with ethanol wasoptimized. The optimum condition was 4h of reflux at 80℃with 15 times medicine amountof 55%ethanol. With the aim of extraction yield and content of astragalosideⅣandchromone glycoside, the extraction condition of effective ingredients group extraction in oneautoclave was optimized according to the orthogonal design and single-factor test. Theoptimum condition was 4h of reflux at 70℃with 10 times unit medicine amount of 80%ethanol (4) Active ingredients group of Yupingfeng were separated and enriched with macroporous resin. The adsorption capacity and adsorption ratio of seven kinds of adsorption resinincluding D101 and S-8 for astragaloside and chromone glycoside in extraction of Yupingfengwere investigated. The results showed that the peculiarities of D 101, AB-8 and X-5 were good.Further, the concentration of active ingredients group in solution, flow rate, composition andflow rate of elution reagent affected of leek curves and elution curves were studied. Theresults showed that the purity of astragaloside was raised to 39.27%from 2.57%afterenriched with AB-8 resin bed. Recovery is 83.71%. The purity of prim-O-glucosylcimifuginand 4’-O-β-glucosyl-5-Omethylvisamminol were raised to 3.69%from 0.24%, and 6.34%from 0.31%respectively. Recovery is 82.31%and 91.03%respectively. The active ingredientsgroup was enriched effectively.
【Key words】 Yupingfeng; active ingredients group; extraction; separation and purification; macro porous resin adsorption;
- 【网络出版投稿人】 广西大学 【网络出版年期】2007年 05期
- 【分类号】TQ461
- 【被引频次】2
- 【下载频次】303