高速逆流色谱分离纯化连翘中的两对立体异构体

林产化学与工业 ›› 2011, Vol. 31 ›› Issue (5): 41-47.

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

收稿日期:2010-12-31 修回日期:1900-01-01 出版日期:2011-10-30 发布日期:2011-10-30
通讯作者: 王晓,博士,研究员,从事天然产物化学方面的研究;E-mail:Wangx@keylab.net。

Preparative Isolation and Purification of Two Pairs of Stereomer from the Fruits of Forsythia suspensa by High-speed Counter-current Chromatography

DUAN Wen-juan DUAN Wen-juan, GENG Yan-ling, ZHUANG Hui-yong, FU Mao-run, LIU Jian-hua, WANG Xiao

Shandong Analysis and Test Center; Key laboratory for Applied Technology of Sophisticated Analytical Instrument of Shandong Province, Jinan 250014, China

Received:2010-12-31 Revised:1900-01-01 Online:2011-10-30 Published:2011-10-30

摘要/Abstract

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-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 800 r/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。

关键词: 高速逆流色谱, 连翘, 立体异构体

Abstract: 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-butanol-methanol-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), ¹H NMR, and ¹³C NMR.

Key words: high-speed counter-current chromatography, Forsythia suspensa, stereomer CLC number:TQ351

中图分类号:

TQ351

段文娟;耿岩玲;庄会永;傅茂润;刘建华;王晓. 高速逆流色谱分离纯化连翘中的两对立体异构体[J]. 林产化学与工业, 2011, 31(5): 41-47.

DUAN Wen-juan DUAN Wen-juan;GENG Yan-ling;ZHUANG Hui-yong;FU Mao-run;LIU Jian-hua;WANG Xiao. Preparative Isolation and Purification of Two Pairs of Stereomer from the Fruits of Forsythia suspensa by High-speed Counter-current Chromatography[J]. , 2011, 31(5): 41-47.

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