延胡索中生物碱类化合物的分离纯化及指纹图谱研究

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1、大连理工大学博士学位论文延胡索中生物碱类化合物的分离纯化及指纹图谱研究姓名：张少君申请学位级别：博士专业：生物化工指导教师：王长海20090401延胡索中生物碱类化合物的分离纯化及指纹图谱研究SeparationandPurificationAlkaloidsFromyanhusuoW．T．WangandtheFingerprintingStudy一AbstractThispapertookalkaloidsofCorydalisyahusuoW．T．Wang(Cyanhusuo)astheresearchmode．Accordingtotheproblemsneedtobc

2、solvedinseparationandqualitycontrolofalkaloids，wedevelopedanewprocessforproducingalkloidswithhighpurityusingion-exchangeresinsseparationandhigh-speedcounter-currentchromatography(HSCCC)purification．Furthermore，thedigitizedfingerprintswereconstructedforqualitycontrolofalkaloids-containingpro

3、ducts．Themainresultsarelistedasfollows：AfterexaminedtheextractionmethodsofCyanhusuo，ion·exchangerresinD152wasselectedfordl-tetrahydropalmatine(dl—THP)separationfromcrudeextractofCyanhusuo．Undertheoptimizedsorption-desorptionconditions，theareapercentofdl-THPincrudeextreactincreasedfrom4．11％t

4、o21．13％witharecoveryof65．S口％usingD152packedcolumn．Comparedwithliquid／1iquidextractionanddepositionmethod，ion-exchangeresinshowedobviousadvantagesofhighrecovery，hightreatmentcapability，easyoperationandeasyregeneration．Inthehigh·speedcounter-currentchromatography(HSCCC)technique，solventscreen

5、ingtookover90％worktime．WeestablishedafastsolventscreeningmethodnamedaveragepolaritypJ)．Usingthenewmethod，aHSCCCseparationwasfurtherconstructedtopurifydl-THPwith刀-hexane-ethylacetate-methanol-water(4：6：5：5，v／v)assolventsystems，andthepurityofdl-THPreached92．7％witharecoveryof95．1％afteronerunHS

6、CCCpurification．Fingerprintbecomesapopularandauthoritativemethodforthequalitycontrolofnaturealproduct，whichwasrecommendedbyauthoritiesincludingSFDA,FDA,WHOandtheEuropeanAgency．AHPLCfingerprinthasbeendevelopedforthepurposeofqualitycontrolofTCMproduct．Inordertoeliminatetheeffectofoperationand

7、reducethefluctuationofchromatographyinformation，adigitizedfingerprintwasfurtherconstructedusingRRTasnaturedeterminationcriterion，RPAasquantificationcriterion，nmainpeaks，differenceratio，superposeratioandcorrelationcoefficientasparameters，andcharactercurve