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1、天津大學(xué)碩士學(xué)位論文人參皂甙Rb<,3>分離純化的研究姓名:吳懿琳申請(qǐng)學(xué)位級(jí)別:碩士專業(yè):化學(xué)工藝指導(dǎo)教師:韓金玉20040101摘要摘要本文研究了三七葉甙中的特有有效成分人參皂甙Rb,的分離純化工藝,以期得到含量滿足不同新藥要求的產(chǎn)品,為新藥開發(fā)奠定物質(zhì)基礎(chǔ)。以三七葉甙粗提物為原料,在反相半制備液相色譜實(shí)驗(yàn)的基礎(chǔ)上,直接應(yīng)用反相制各液相色譜分離純化單體皂甙Rb,,分別考察了上樣量、流動(dòng)相甲醇一水的組成及流動(dòng)相流速對(duì)分離過程的影響,最終確定了適宜的制備色譜條件,得到Rb3含量為65%~70%的樣品,得率能達(dá)到
2、20%左右,達(dá)到中藥二類原料藥含量要求。為了得到更高含量的Rb3產(chǎn)品,采用二次上樣的方法,所得產(chǎn)品中Rb3含量最高能達(dá)到92.06%??紤]到得率因素,將流動(dòng)相體系改為乙脖一水溶液,選擇粒徑更小的填料,并改變色譜柱的尺寸,從而提高了柱效和分離效果。初步建立了制備色譜條件,所得人參皂甙Rb3含量為86.2%,有望達(dá)到中藥一類原料藥含量要求。同期制得Rc的純度在95%以上。采用多組分普遍化速率模型對(duì)三七葉甙的反相半制各型和制備型高效液相色譜的分離純化過程進(jìn)行了模擬,模擬結(jié)果與實(shí)驗(yàn)數(shù)據(jù)的規(guī)律性吻合較好,對(duì)過程操作具有
3、一定的指導(dǎo)意義。本文所建立的人參皂甙Rb3的分離純化工藝簡(jiǎn)便、高效,對(duì)人參皂甙Rb3單體的藥理研究及新藥開發(fā)具有重要價(jià)值。關(guān)鍵詞:人參皂甙Rb3,液相色譜,分離純化,色譜模型,過程模擬ABSTRACTThispaperdealtwiththeisolationandpurificationofthepharmaceuticalcomponent-ginsenosideRb3fromthetraditionalChinesemedicine—Panaxnotoginseng,hopingtogettheprod
4、uctofwhichthecontentcallmeettheneedofthedifferentnewdrugandsettlingthematerialfoundationforthenewdrugdevelopment.Thenotoginsengfoliumsaponinswereusedasrawmaterialanddirectlyseparatedbyreversedphasepreparativeliquidchromatography.Theeffectsofsamplevolume,con
5、structionandflowrateofthemobilephaseontheseparationprocesswereinvested.Thesuitableconditionsweredeterminedrespectively.ThecontentandthereceiveefficiencyofginsenosideRb3inthecrudeproductwereabout65%~70%and20%respectively.Inordertogettheproduct(content>90%),t
6、hecrudeproductwasusedasrawmaterialandseparatedagain,throughwhichthecontentofRb3intheproductreachedabout92.06%.Toraisetheyield,asemi—preparativechromatographywasusedwhichisconstitutedofthefollowing:themixsolutionofmethlcyanideandwaterasthemobilephase,theCl8o
7、flonmparticlediameteraspacking中40×300mracolumn.Theprimarypreparativeconditionsweredeterminedrespectively.ThecontentoftheproductRb3isabout86.2%,andwhichofReisabove95%.Thegeneralmulti—componentratemodelofpreparativechromatographyWasestablished.Theresultofsimu
8、lationshowedgoodagreementwithexperimentaldatainregularity.Thegeneralmulti·eomponentratmodelisveryusefulforguidingthepreparativeprocess.TheprocessforisolationandpurificationofginsenosideRb3describedhere