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Accelerated solvent extraction and pH‐zone‐refining counter‐current chromatographic purification of yunaconitine and 8‐deacetylyunaconitine from Aconitum vilmorinianum Kom
Authors:Xi‐Kai Shu  Jia Li  Feng Liu  Xiao‐Jing Lin  Xiao Wang  Chun‐Xia Song
Institution:1. Shandong Analysis and Test Center, Shandong Academy of Sciences, , Jinan, Shandong, China;2. College of Pharmacy, Shandong University of Traditional Chinese Medicine, , Jinan, Shandong, China;3. College of Marine, Shandong University at Weihai, , Weihai, Shandong, China
Abstract:This study aimed to seek an efficient method to extract and purify yunaconitine and 8‐deacetylyunaconitine from Aconitum vilmorinianum Kom. by accelerated solvent extraction combined with pH‐zone‐refining counter‐current chromatography. The major extraction parameters for accelerated solvent extraction were optimized by an orthogonal test design L9 (3)4. Then a separation and purification method was established using pH‐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 1H and 13C NMR spectroscopy.
Keywords:Accelerated solvent extraction  Aconitum vilmorinianum Kom    Counter‐current chromatography  Traditional Chinese medicines  Yunaconitine
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