Development of gradient centrifugal partition chromatography method and its application for the isolation of 3,5-dimethoxyphenanthrene-2,7-diol and batatasin-I from Dioscorea opposita

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Title
Development of gradient centrifugal partition chromatography method and its application for the isolation of 3,5-dimethoxyphenanthrene-2,7-diol and batatasin-I from Dioscorea opposita
Author(s)
K D Yoon; M H Yang; Young Won Chin; Y Kim; H R Kim; K Choi; J H Park; J Kim
Bibliographic Citation
Natural Products Sciences, vol. 15, no. 3, pp. 144-150
Publication Year
2009
Abstract
Gradient centrifugal partition chromatography (GCPC) method was developed and applied to isolate 3,5-dimethoxyphenanthrene-2,7-diol (DMP) and batatasin-I (BA-I) from the dichloromethane soluble extract of Dioscorea opposita. In this method, the lower phase of n-hexane-methanol-water system (HMW, 10 : 9 : 1, v/v) was used as a mobile phase A (MpA) and water was used as a mobile phase B (MpB). This gradient CPC method is comparable to that of reversed-phase HPLC method in that the stationary upper-phase of HMW (10 : 9 : 1 v/v) works as if it were reversed-phase silica gel due to its hydrophobic property, while the lower phase (MpA) and water (MpB) functioned as hydrophilic mobile phases. The initial condition of the mobile phase was 20% MpA/80% MpB and maintained for 150 min to obtain DMP (1.2 mg), and then MpA was increased up to 50% to elute BA-I (1.7 mg). The purities of DMP and BA-I were 94.1% and 98.3% with the recovery yields of 83% and 86%,respectively. Similar results were obtained by linear-gradient CPC. The CPC peak fractions were identified by comparing their retention time to those of authentic samples of DMP and BA-I and their spectroscopic data (1HNMR and 13C NMR) to those of literature values.
Keyword
3,5-dimethoxyphenanthrene-2,7-diolbatatasin-IDioscorea oppositaGradient centrifugal partition chromatography (GCPC)n-hexane-methanol-water system (HMW, 10 : 9 : 1, v/v)
ISSN
I000-0147
Publisher
Korean Society of Pharmacognosy
Type
Article
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1. Journal Articles > Journal Articles
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