Published:Journal of Chromatographic Science,
ISSN 0021-9665 Volume
47, Number 5, May/June 2009, pp. 349-353
A High-Speed Counter-Current Chromatography– HPLC–DAD
Method for Preparative Isolation and Purification of Two Polymethoxylated
Flavones From Taraxacum mongolicum
Shuyun Shi1, Honghao Zhou2,
Yuping Zhang1,
Yu Zhao3, Kelong Huang1, and Suqin Liu1 1School of Chemistry and Chemical Engineering, Central South
University, Changsha 410083, China; 2Pharmacogenetics Institute
of Central South University, Changsha 410078, China; and 3College
of Pharmaceutical Sciences, Zhejiang University, Hangzhou 310031,
China
After an initial clean-up step on silica gel,
a preparative high-speed counter-current chromatography coupled
with on-line high-performance liquid chromatography–diode
array detection method (HSCCC–HPLC–DAD) was successfully
developed for the isolation and determination two polymethoxylated
flavones, 3',4',7-trimethoxyquercetin and artemetin, from the
aerial part of Taraxacum mongolicum. The HSCCC separation
was performed with a two-phase solvent system composed of n-hexane–ethyl
acetate–methanol–water (6:5:6:5, v/v/v/v) at a flow
rate of 1.5 mL/min and at 800 rpm. The on-line purity monitoring
of a representative aliquot from each HSCCC fraction was operated
automatically. Using this method, fractions with high purity
were collected. The HSCCC purification step was done in 5 h,
and afforded 84.2 mg of 3',4',7-trimethoxyquercetin and 52.3
mg of artemetin, with purity over 98% from 200 mg of the enriched
extracts of T. mongolicum. The structures were identified
by electorspray ionization mass spectrometry and 1H
NMR experiments. To our best knowledge, 3',4',7-trimethoxyquercetin
was obtained from the plant of genus Taraxacum for the
first time by our group. This hyphenated method could be used
for the preparation of bioactive compounds with higher purity
from natural products.
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