高速逆流色谱法从紫花前胡根中分离纯化香豆素类化合物

Isolation and purification of coumarin compounds from the root of Peucedanum decursivum (Miq.) Maxim by high-speed counter-current chromatography.

作者信息

Liu Renmin, Sun Qinghua, Shi Yunrong, Kong Lingyi

机构信息

Department of Natural Medicinal Chemistry, China Pharmaceutical University, Nanjing 210009, China.

出版信息

J Chromatogr A. 2005 May 27;1076(1-2):127-32. doi: 10.1016/j.chroma.2005.04.041.

DOI:10.1016/j.chroma.2005.04.041

PMID:15974078

Abstract

A preparative high-speed counter-current chromatography (HSCCC) method for isolation and purification of coumarin compounds from the Chinese medicinal plant Peucedanum decursivum (Miq.) Maxim (Zihuaqianhu in Chinese) was successfully established by using light petroleum-ethyl acetate-methanol-water (5:5:7:4, v/v) as the two-phase solvent system. The upper phase of light petroleum-ethyl acetate-methanol-water (5:5:7:4, v/v) was used as the stationary phase of HSCCC. Nodakenetin (2.8 mg), 6.1 mg of Pd-C-IV, 7.3 mg of Pd-D-V, 4.7 mg of ostruthin, 7.8 mg of decursidin and 11.2 mg of decursitin C with the purity of 88.3%, 98.0%, 94.2%, 97.1%, 97.8% and 98.4%, respectively, were separated successfully in one-step separation from 150 mg of crude sample from P. decursivum (Miq.) Maxim. After purified by HSCCC again with light petroleum-ethyl acetate-methanol-water (5:5:4:5, v/v) as the two-phase solvent system, the purity of (I) can reach 99.4%. The structures of all the compounds were identified by 1H NMR and 13C NMR.

摘要

以石油醚 - 乙酸乙酯 - 甲醇 - 水（5:5:7:4，v/v）为两相溶剂体系，成功建立了一种从中药紫花前胡（Peucedanum decursivum (Miq.) Maxim）中分离纯化香豆素类化合物的制备型高速逆流色谱（HSCCC）方法。石油醚 - 乙酸乙酯 - 甲醇 - 水（5:5:7:4，v/v）的上相用作HSCCC的固定相。从150 mg紫花前胡粗样品中一步分离得到了纯度分别为88.3%、98.0%、94.2%、97.1%、97.8%和98.4%的紫花前胡苷元（2.8 mg）、Pd - C - IV（6.1 mg）、Pd - D - V（7.3 mg）、蛇床子素（4.7 mg）、前胡素（7.8 mg）和前胡丙素（11.2 mg）。以石油醚 - 乙酸乙酯 - 甲醇 - 水（5:5:4:5，v/v）为两相溶剂体系再次通过HSCCC纯化后，（I）的纯度可达99.4%。所有化合物的结构均通过1H NMR和13C NMR进行了鉴定。