Accelerated solvent extraction and p H ‐zone‐refining counter‐current chromatographic purification of yunaconitine and 8‐deacetylyunaconitine from A conitum vilmorinianum K om

This study aimed to seek an efficient method to extract and purify yunaconitine and 8‐deacetylyunaconitine from A conitum vilmorinianum K om. by accelerated solvent extraction combined with p H ‐zone‐refining counter‐current chromatography. The major extraction parameters for accelerated solvent ext...

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Bibliographic Details
Published in:Journal of separation science 2013-08, Vol.36 (16), p.2680-2685
Main Authors: Shu, Xi‐Kai, Li, Jia, Liu, Feng, Lin, Xiao‐Jing, Wang, Xiao, Song, Chun‐Xia
Format: Article
Language:English
Subjects:
Chromatography
Ethers
Methyl alcohol
NMR spectroscopy
Purification
Separation
Solvent extraction
Solvents
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Summary:This study aimed to seek an efficient method to extract and purify yunaconitine and 8‐deacetylyunaconitine from A conitum vilmorinianum K om. by accelerated solvent extraction combined with p H ‐zone‐refining counter‐current chromatography. The major extraction parameters for accelerated solvent extraction were optimized by an orthogonal test design L 9 (3) 4 . Then a separation and purification method was established using p H ‐zone‐refining counter‐current chromatography with a two‐phase solvent system composed of petroleum ether/ethyl acetate/methanol/water (5:5:2:8, v/v) with 10 mM triethylamine in the upper phase and 10 mM HCl in the lower phase. From 2 g crude extract, 224 mg of 8‐deacetylyunaconitine (I) and 841 mg of yunaconitine (II) were obtained with a purity of over 98.0%. The chemical structures were identified by ESI ‐ MS and 1 H and 13 C NMR spectroscopy.
ISSN:1615-9306
1615-9314
DOI:10.1002/jssc.201300472