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王萍,刘永玲,陈涛,徐文华,尤进茂,刘永军,李玉林*.One-step Separation and Purification of Three Lignans and One Flavonol from Sinopodophyllum emodi by Medium-pressure Liquid Chromatography and High-speed Counter-current Chromatography, Phytochemical Analysis,2013,24:603-607.IF=2.48
Abstract:
Introduction – Lignans and flavonols are the primary constituents of Sinopodophyllum emodi and have been used as cathartic,anthelmintic,chemotherapeutic and anti-hypertensive compounds. Although these compounds have been isolated, there have been no reports on the separation of 40-demethyl podophyllotoxin, podophyllotoxin, deoxypodophyllotoxin and kaempferol in one step by medium-pressure liquid chromatography (MPLC) and high-speed counter-current chromatography (HSCCC).
Objective – Development of an efficient method for the preparative separation and purification of three lignans and one flavonol from S. emodi.
Methods – The precipitate of crude extracts was first separated by MPLC into four parts, numbered GJ-1, GJ-2, GJ-3 and GJ-4.GJ-1 was separated and purified by HSCCC using a solvent system composed of n-hexane:ethyl acetate:methanol:water (1.75:1.5:1:0.75, v/v/v/v). The purities of the target compounds were assessed using high-performance liquid chromatography (HPLC) and chemical structures were identified by 1H-NMR and 13C-NMR.
Results – The HSCCC and MPLC methods were successfully used for the preparative separation and purification of 40-demethyl podophyllotoxin (8.5 mg, 92.4%), podophyllotoxin (40.1 mg, 92.1%), deoxypodophyllotoxin (4.6 mg, 98.1%), and kaempferol (1.6 mg, 96.7%) from a 100 mg sample.
