title: Accelerated solvent extraction and pH-zone-refining counter-current chromatographic purification of yunaconitine and 8-deacetylyunaconitine from Aconitum vilmorinianum Kom.
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 (1)H and (13)C NMR spectroscopy.
authors.affiliation: Shandong Analysis and Test Center, Shandong Academy of Sciences, Jinan, Shandong, China.
authors.forename: Xi-Kai
authors.initials: XK
authors.lastname: Shu
authors.forename: Jia
authors.initials: J
authors.lastname: Li
authors.forename: Feng
authors.initials: F
authors.lastname: Liu
authors.forename: Xiao-Jing
authors.initials: XJ
authors.lastname: Lin
authors.forename: Xiao
authors.initials: X
authors.lastname: Wang
authors.forename: Chun-Xia
authors.initials: CX
authors.lastname: Song
mesh_terms: D000157:Aconitine / Q000031:analogs & derivatives* / Q000737:chemistry / Q000302:isolation & purification; D031841:Aconitum / Q000737:chemistry*; D003377:Countercurrent Distribution / Q000379:methods*; D015394:Molecular Structure; D010936:Plant Extracts / Q000737:chemistry / Q000302:isolation & purification*; D021241:Spectrometry, Mass, Electrospray Ionization
chemical_list: D010936:Plant Extracts; C069835:yunaconitine; D000157:Aconitine
keywords: Accelerated solvent extraction; Aconitum vilmorinianum Kom.; Counter-current chromatography; Traditional Chinese medicines; Yunaconitine