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Separation and purification of four compounds from D esmodium styracifolium using off‐line two‐dimensional high‐speed counter‐current chromatography
Author(s) -
Su Wen,
Liu Qi,
Yang Qing,
Yu Jingang,
Chen Xiaoqing
Publication year - 2013
Publication title -
journal of separation science
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.72
H-Index - 102
eISSN - 1615-9314
pISSN - 1615-9306
DOI - 10.1002/jssc.201300653
Subject(s) - countercurrent chromatography , chromatography , chemistry , ethyl acetate , elution , high performance liquid chromatography , solvent , analytical chemistry (journal) , two dimensional chromatography , phase (matter) , column chromatography , organic chemistry
An off‐line 2 D high‐speed counter‐current chromatography technique in preparative scale has been successfully applied to separate and purify the main compounds from the ethyl acetate extract of D esmodium styracifolium . A two‐phase solvent system composed of n ‐hexane/ethyl acetate/methanol/water at an optimized volume ratio of 1:2:1:2 v/v/v/v was used. Conventional high‐speed counter‐current chromatography was used as the first dimension, and the upper phase of the solvent system was used as the stationary phase in the head‐to‐tail elution mode at a flow rate of 2.0 mL/min and a rotation speed of 900 rpm. Recycling high‐speed counter‐current chromatography served as the second dimension to separate an impure fraction of the first dimension. A total of four well‐separated substances including vanillic acid ( 1 ), β‐sitosterol ( 2 ), formononetin ( 3 ), and aromadendrin ( 4 ) were obtained, and their purities and structures were identified by HPLC – MS and 1 H NMR spectroscopy. The results illustrated that off‐line 2 D high‐speed counter‐current chromatography is an effective way to isolate compounds in complex samples.