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Accelerated solvent extraction and p H ‐zone‐refining counter‐current chromatographic purification of yunaconitine and 8‐deacetylyunaconitine from A conitum vilmorinianum K om
Author(s) -
Shu XiKai,
Li Jia,
Liu Feng,
Lin XiaoJing,
Wang Xiao,
Song ChunXia
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.201300472
Subject(s) - chromatography , chemistry , countercurrent chromatography , extraction (chemistry) , solvent , methanol , triethylamine , ethyl acetate , petroleum ether , column chromatography , analytical chemistry (journal) , organic chemistry
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.