利用高速逆流色谱法从一种中药中分离出四种苯丙素苷类化合物。

Separation of Four Phenylpropanoid Glycosides from a Chinese Herb by HSCCC.

作者信息

Zhang Lin, Yue Hui-Lan, Zhao Xiao-Hui, Li Jing, Shao Yun

机构信息

Northwest Institute of Plateau Biology, Chinese Academy of Sciences, Xining 810001, China.

Northwest Institute of Plateau Biology, Chinese Academy of Sciences, Xining 810001, China Key Laboratory of Adaptation and Evolution of Plateau Biota, Northwest Institute of Plateau Biology, Chinese Academy of Sciences, Xining 810001, China.

出版信息

J Chromatogr Sci. 2015 Jul;53(6):860-5. doi: 10.1093/chromsci/bmu130. Epub 2014 Nov 19.

DOI:10.1093/chromsci/bmu130

PMID:25410625

Abstract

Four phenylpropanoid glycosides (PPGs), such as echinacoside, wiedemannioside C, forsythoside B and verbascoside, were isolated and purified from the Tibetan medicinal herb Pedicularis longiflora Rudolph. var. tubiformis (Klotz) Tsoong by high-speed counter-current chromatography (HSCCC) combined with macroporous resin (MR) column separation for the first time. In the present study, the two-phase solvent system composed of ethyl acetate-n-butanol-water (10 : 6:15, v/v/v) was used for HSCCC separation. A total of 3.5 mg of echinacoside, 12.6 mg of wiedemannioside C, 22.7 mg of forsythoside B and 48.7 mg of verbascoside with the purity of 93.6, 97.9, 97.8 and 98.1%, respectively, were obtained from 120 mg of crude sample. The HSCCC fractions were analyzed by HPLC, and the chemical structures were identified by (1)H NMR and (13)C NMR. The results demonstrate that MR coupled with HSCCC is a powerful technique for separation of PPGs from natural products.

摘要

首次采用高速逆流色谱（HSCCC）结合大孔树脂（MR）柱分离法，从藏药长管马先蒿（Pedicularis longiflora Rudolph. var. tubiformis (Klotz) Tsoong）中分离并纯化出4种苯丙素苷（PPGs），即松果菊苷、魏德曼苷C、连翘酯苷B和毛蕊花糖苷。在本研究中，采用乙酸乙酯 - 正丁醇 - 水（10 : 6 : 15，v/v/v）组成的两相溶剂体系进行HSCCC分离。从120 mg粗样品中分别获得了3.5 mg松果菊苷、12.6 mg魏德曼苷C、22.7 mg连翘酯苷B和48.7 mg毛蕊花糖苷，纯度分别为93.6%、97.9%、97.8%和98.1%。通过高效液相色谱（HPLC）分析HSCCC馏分，并通过氢核磁共振（¹H NMR）和碳核磁共振（¹³C NMR）鉴定化学结构。结果表明，MR与HSCCC联用是从天然产物中分离PPGs的有效技术。