title: 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.
abstract: BACKGROUND
  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.
  
  
  CONCLUSIONS
  Three lignans (4'-demethyl podophyllotoxin, podophyllotoxin, deoxypodophyllotoxin) and one flavonol (kaempferol) were successfully isolated by HSCCC and MPLC in one step.
authors.affiliation: Key Laboratory of Adaptation and Evolution of Plateau Biota, Northwest Institute of Plateau Biology, Chinese Academy of Sciences, Xining, 810001, PR China; University of the Chinese Academy of Sciences, Beijing, 100049, PR China.
authors.forename: Ping
authors.initials: P
authors.lastname: Wang
authors.forename: Yongling
authors.initials: Y
authors.lastname: Liu
authors.forename: Tao
authors.initials: T
authors.lastname: Chen
authors.forename: Wenhua
authors.initials: W
authors.lastname: Xu
authors.forename: Jinmao
authors.initials: J
authors.lastname: You
authors.forename: Yongjun
authors.initials: Y
authors.lastname: Liu
authors.forename: Yulin
authors.initials: Y
authors.lastname: Li
mesh_terms: D028141:Berberidaceae / Q000737:chemistry*; D002853:Chromatography, Liquid / Q000295:instrumentation / Q000379:methods*; D003377:Countercurrent Distribution / Q000295:instrumentation / Q000379:methods*; D044948:Flavonols / Q000737:chemistry / Q000302:isolation & purification*; D017705:Lignans / Q000737:chemistry / Q000302:isolation & purification*; D015394:Molecular Structure; D019906:Nuclear Magnetic Resonance, Biomolecular
chemical_list: D044948:Flavonols; D017705:Lignans
keywords: 4′-demethylpodophyllotoxin; Sinopodophyllum emodi; deoxypodophyllotoxin; high-speed counter-current chromatography; kaempferol; medium-pressure liquid chromatography; one-step; podophyllotoxin