Separation and purification of four compounds from Desmodium styracifolium using off-line two-dimensional high-speed counter-current chromatography.
An off-line 2D 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 Desmodium 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 2D high-speed counter-current chromatography is an effective way to isolate compounds in complex samples.
School of Chemistry and Chemical Engineering, Central South University, Changsha, China.
Wen
W
Su
Qi
Q
Liu
Qing
Q
Yang
Jingang
J
Yu
Xiaoqing
X
Chen
D002851:Chromatography, High Pressure Liquid; D003377:Countercurrent Distribution / Q000295:instrumentation / Q000379:methods*; D007887:Fabaceae / Q000737:chemistry*; D009682:Magnetic Resonance Spectroscopy; D010936:Plant Extracts / Q000737:chemistry / Q000302:isolation & purification*
D010936:Plant Extracts
Desmodium styracifolium; High-speed counter-current chromatography; Off-line 2D counter-current chromatography; Recycling counter-current chromatography