Ping Wang1,2, Yongling Liu1,2, Tao Chen1, Wenhua Xu1, Jinmao You1, Yongjun Liu1, Yulin Li1
1Key Laboratory of Adaptation and Evolution of Plateau Biota, Northwest Institute of Plateau Biology, Chinese Academy of Sciences, Xining 810001, PR China
2University of the Chinese Academy of Sciences, Beijing 100049, PR China
Tóm tắt
ABSTRACTIntroductionLignans 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).ObjectiveDevelopment of an efficient method for the preparative separation and purification of three lignans and one flavonol from S. emodi.MethodsThe 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.ResultsThe 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.ConclusionThree 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.
