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1、高速逆流色譜分離制備蒲公英中的黃酮苷施樹云1,張宇平1,趙昱2,黃可龍1,劉素琴1(1.中南大學化學化工學院長沙410083;2.浙江大學藥學院杭州310058)’摘要:目的:采用高速逆流色譜(nsccC)分離純化蒲公英中的芫花素_4’一0一B—D一蘆丁糖苷和橙皮苷。方法:采用C.。反相色譜對蒲公英的正丁醇部位進行預處理,再利用正丁醇一正己烷一水(體積比為1:1:2)為溶劑系統(tǒng)對其進行分離,上相為固定相,下相為流動相,流速為1.5mL/min,檢測波長為254llln。所得產品經過高效液相色譜進行檢測,通過面積歸一化法檢測純度。經過紫外,質譜,一維以及二維核磁共振等方法進行結
2、構分析鑒定。結果:經過一步HSCCC可以從600mg富集物中分離純化得到84.6rag芫花素.4’一O—B—D一蘆丁糖苷和45.1rag橙皮苷,純度分別為98.8%和98.1%。結論:化合物芫花素-4‘一O—B—D一蘆丁糖苷和橙皮苷均為首次從蒲公英屬植物中分離得到。利用該技術,可以對中草藥中的活性成分進行快速的分離純化以及進行相應的結構鑒定。關鍵詞:高速逆流色譜;蒲公英;黃酮苷;核磁共振PreparativeisolationandpurificationoftwoflavonoidglycosidesfromTaraxacumgolicumbyhigh-speediro1a
3、raxacamongoilcumDy11il巨h-scounter-currentchromatographySHIShu—yunl,ZHANGYu-pin91,ZHAOYu2,HUANGKe-lon91,LIUSu—qinl('SchoolofChemistryandChemicalEngineering,CentralSouthUniversity,Changsha410083,China;2InstituteofMateriaMedica,CollegeofPharmaceuticalSciences,ZhejiangUniversity,Hangzhou310031,
4、China)ABSTRACT:OBJEC。In噬:Twoflavonoidglycosides,genkwanin--4LO-B-D-lutinosideandhesperidinwereisolatedandpurifiedfromtheaerialpartofTaraxacummongolicum,atraditionalChinesemedicineffCM)byhigh-speedcounter-currentchromatography(HSCCC).蛐咖ODS:AfterC,sopencolurmichromatographyservedasenrichments
5、tep,high-speedcounter-currentchromatography(HSCCC)wasusedforthefinalpurification.Thetargetcompoundswerefinallyisolatedandpurifiedwithasolventsystemcomposedofn-hexane-n-butanol-water(hl:2,v/v/v).TheHSCCCfractionswereanalyzedbyhigh-performanceliquidchromatography(HPLC)andthechemicalstructures
6、ofthetwoflavonoidglycosideswereidentifiedbyUV,ESI—Ms,1HNMR,”CNMRandHMBCanalysis.I也SULl晦:Inasingleoperation,600mgoftheenrichedextractsofT.mongolicumWasseparatedtoyield84.6mgofgenkwanin-4’-O-B—D—lutinosideand45.1mgofhesperidinwiththepurityof98.8%and98.1%,respectively.CONCLUSION:Genkwanin-4’-O
7、-B-D-lutinosideandhesperidinwereobtainedfromtheplantofgenusTaraxacumforthefirsttime.whichmaybeusedforinvitroandinvivostudiesandreferencesubstancesforanalyticalpurpose.Thistechniqueshouldalsobeapplicabletothepreparationofunknownbioactivecompoundsfromtradi