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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
Author(s) -
Wang Ping,
Liu Yongling,
Chen Tao,
Xu Wenhua,
You Jinmao,
Liu Yongjun,
Li Yulin
Publication year - 2013
Publication title -
phytochemical analysis
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.574
H-Index - 72
eISSN - 1099-1565
pISSN - 0958-0344
DOI - 10.1002/pca.2438
Subject(s) - chemistry , chromatography , podophyllotoxin , kaempferol , countercurrent chromatography , high performance liquid chromatography , column chromatography , quercetin , organic chemistry , antioxidant
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 4′‐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 1 H‐NMR and 13 C‐NMR. Results The HSCCC and MPLC methods were successfully used for the preparative separation and purification of 4 ′‐ 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 . Conclusion Three lignans (4′‐demethyl podophyllotoxin, podophyllotoxin, deoxypodophyllotoxin) and one flavonol (kaempferol) were successfully isolated by HSCCC and MPLC in one step. Copyright © 2013 John Wiley & Sons, Ltd.