高速逆流色谱分离纯化连翘中的两对立体异构体

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

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。

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.