林产化学与工业
林產化學與工業
림산화학여공업
CHEMISTRY AND INDUSTRY OF FOREST PRODUCTS
2011年
5期
41-47
,共7页
段文娟%耿岩玲%庄会永%傅茂润%刘建华%王晓
段文娟%耿巖玲%莊會永%傅茂潤%劉建華%王曉
단문연%경암령%장회영%부무윤%류건화%왕효
高速逆流色谱%连翘%立体异构体
高速逆流色譜%連翹%立體異構體
고속역류색보%련교%입체이구체
high-speed counter-current chromatography%Forsythia suspensa%stereomer
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-正丁醇-甲醇-水(体积比5∶0.7∶1∶5)和乙酸乙酯-正丁醇-甲醇-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1.5 mL/min、检测波长为254 nm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(13C NMR)鉴定化合物的结构.
應用高速逆流色譜法(HSCCC)分離純化連翹果實中的兩對木脂素類立體異構體.分彆用乙痠乙酯-正丁醇-甲醇-水(體積比5∶0.7∶1∶5)和乙痠乙酯-正丁醇-甲醇-水(體積比5∶0.5∶1∶5)為兩相溶劑體繫,在轉速為800r/min、流速為1.5 mL/min、檢測波長為254 nm的條件下進行分離,所得餾分經高效液相色譜(HPLC)檢測純度,電噴霧電離質譜(ESI-MS)和碳覈磁共振波譜(13C NMR)鑒定化閤物的結構.
응용고속역류색보법(HSCCC)분리순화련교과실중적량대목지소류입체이구체.분별용을산을지-정정순-갑순-수(체적비5∶0.7∶1∶5)화을산을지-정정순-갑순-수(체적비5∶0.5∶1∶5)위량상용제체계,재전속위800r/min、류속위1.5 mL/min、검측파장위254 nm적조건하진행분리,소득류분경고효액상색보(HPLC)검측순도,전분무전리질보(ESI-MS)화탄핵자공진파보(13C NMR)감정화합물적결구.
Two pairs of stereomeric lignan,namely (+) pinoresinol monomethyl ether-,β-D-glucoside and phillyrin,(+) pinoresinol-β-D-glucoside and (+) epipinoresinol-β-D-glucoside,were successfully isolated and purified from the fruits of Forsythia suspensa by high-speed counter-current chromatography (HSCCC) using two-phase solvent systems with composed of ethyl acetate-n-butanol-methanol-water (5 ∶ 0.7 ∶ 1 ∶ 5,volume ratio) and ethyl acetate-n-butanolmethanol-water (5 ∶ 0.5 ∶ 1 ∶ 5,volume ratio ),respectively.The purities of the isolated compounds were all above 97 ％ determined by high-performance liquid chromatography (HPLC) and their structures were confirmed by electrospray ionization MS (ESI-MS),1HNMR,and 13CNMR.
