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Rapid preparative separation of six bioactive compounds from G entiana crassicaulis D uthie ex B urk. using microwave‐assisted extraction coupled with high‐speed counter‐current chromatography
Author(s) -
Liang Jinru,
Ito Yoichiro,
Zhang Xinxin,
He Jiao,
Sun Wenji
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.201300897
Subject(s) - chemistry , chromatography , extraction (chemistry) , gentianaceae , gentiana , countercurrent chromatography , high performance liquid chromatography , elution , acetic acid , organic chemistry , traditional medicine , botany , medicine , biology
A rapid method combining microwave‐assisted extraction ( MAE ) and high‐speed counter‐current chromatography ( HSCCC ) was applied for preparative separation of six bioactive compounds including loganic acid ( I ), isoorientin‐4′‐ O ‐glucoside ( II ), 6′‐ O ‐β‐ d ‐glucopyranosyl gentiopicroside ( III ), swertiamarin ( IV ), gentiopicroside ( V ), sweroside ( VI ) from traditional T ibetan medicine Gentiana crassicaulis D uthie ex B urk. MAE parameters were predicted by central composite design response surface methodology. That is, 5.0 g dried roots of G. crassicaulis were extracted with 50 mL 57.5% aqueous ethanol under 630 W for 3.39 min. The extract (gentian total glycosides) was separated by HSCCC with n ‐butanol/ethyl acetate/methanol/1% acetic acid water (7.5:0.5:0.5:3.5, v/v/v/v) using upper phase mobile in tail‐to‐head elution mode. 16.3, 8.8, 12., 25.1, 40.7, and 21.8 mg of compounds I–VI were obtained with high purities in one run from 500 mg of original sample. The purities and identities of separated components were confirmed using HPLC with photo diode array detection and quadrupole TOF‐MS and NMR spectroscopy. The study reveals that response surface methodology is convenient and highly predictive for optimizing extraction process, MAE coupled with HSCCC could be an expeditious method for extraction and separation of phytochemicals from ethnomedicine.