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 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.