高速逆流色谱分离纯化连翘中的两对立体异构体.docVIP

高速逆流色谱分离纯化连翘中的两对立体异构体 第31卷第5期 2011年1O月 林产化学与工业 ChemistryandIndustryofForestProducts V01.31No.5 0ct.2011 PreparativeIsolationandPurificationofTwoPairsof StereomerfromtheFruitsofForsythiasuspensaby High—-speedCounter?-currentChromatography DUANWen-juan DUANWen-juan,GENGYan—ling,ZHUANGHui—yong, FUMao—run,LIUJian—hua,WANGXiao (ShandongAnalysisandTestCenter;KeylaboratoryforAppliedTechnologyofSophisticated AnalyticalInstrumentofShandongProvince,Jinan250014,China) Abstract:Twopairsofstereomericlignan,namely(+)pinoresinolmonomethylether-fl—D—glucosideand phillyrin,(+)pinoresinol一D—glucosideand(+)epipinoresinol一D—glucoside,weresuccessfullyisolated andpurifiedfromthefruitsofForsythiasue0byhigh—speedcounter—currentchromatography(HSCCC)usingtwo—phasesol- ventsystemswithcomposedofethylacetate-n—butanol—methanol—water(5:0.7:1:5,volumeratio)andethylacetate—n-butanol— methanol—water(5:0.5:1:5,volumeratio),respectively.Thepuritiesoftheisolatedcompoundswereallabove97%deter- minedbyhigh—performanceliquidchromatography(HPLC)andtheirstructureswereconfirmedbyelectrosprayionizationMS (ESI.MS),HNMR,andCNMR. Keywords:high—speedcounter-currentchromatography;Forsythiase瑚n;stereomer CLCnumber:TQ351Documentcode:AArticleID:0253—2417(2011)05—0041—07 高速逆流色谱分离纯化连翘中的两对立体异构体 段文娟,耿岩玲,庄会永,傅茂润,刘建华,王晓 (山东省分析测试中心;山东省大型精密仪器应用技术重点实验室,山东济南250014) 摘要:应用高速逆流色谱法(HSCCC)分离纯化连翘果实中的两对木脂素类立体异构体.分别用乙酸乙酯一正丁醇一甲 醇一水(体积比5:0.7:1:5)和乙酸乙酯一正丁醇一甲醇一水(体积比5:0.5:1:5)为两相溶剂体系,在转速为800r/min, 流速为1.5mL/min,检测波长为254nm的条件下进行分离,所得馏分经高效液相色谱(HPLC)检测纯度,电喷雾电离质 谱(ESI—MS)和碳核磁共振波谱(CNMR)鉴定化合物的结构. 关键词:高速逆流色谱;连翘;立体异构体 Forsythiasuspensa(Thunb.)VahlisanimportantherbforornamentalandmedicinalpurposesinChina. ThefruitsofF.suspensaarewell—knowntraditionalChinesemedicine(TCM),named,LianqiaoinChinese. Accordingtothematuritylevelofthefruits,thecommercialdrugscouldbeclassifiedinto,Qingqiaoand Laoqiao;bothofthemareofficialsourcesofthisTCM.F.suspensa(Thunb).Vahlisaveryimportant antimicrobialmedicinewhichcaninhibittyphoidbacillus,colonbacillusSalmonellaparatyph