Application of high-speed counter-current chromatography for preparative separation of cyclic peptides from Vaccaria segetalis

J Chromatogr B Analyt Technol Biomed Life Sci. 2011 Apr 1;879(11-12):811-4. doi: 10.1016/j.jchromb.2011.02.001.

Abstract

Following an initial clean-up step on silica gel, high-speed counter-current chromatography (HSCCC) was used to separate cyclic peptides from an extract of the seeds of Vaccaria segetalis. The two-phase solvent system used for HSCCC separation was composed of petroleum ether-ethyl acetate-methanol-water at an optimized volume ratio of 0.5:3.5:1:5. From 190 mg of crude extract, 38.0 mg of segetalin B and 28.5 mg of segetalin A were obtained with purities of 98.1% and 95.6% as determined by HPLC, respectively. The chemical structures of the target compounds were confirmed by high resolution electrospray ionization time of flight MS (HRESI-TOF-MS) and (1)H NMR analyses.

Publication types

  • Research Support, Non-U.S. Gov't

MeSH terms

  • Acetates / chemistry
  • Alkanes / chemistry
  • Chromatography, High Pressure Liquid
  • Countercurrent Distribution / methods*
  • Drugs, Chinese Herbal / chemistry*
  • Methanol / chemistry
  • Nuclear Magnetic Resonance, Biomolecular
  • Peptides, Cyclic / isolation & purification*
  • Seeds / chemistry
  • Spectrometry, Mass, Electrospray Ionization
  • Vaccaria / chemistry*

Substances

  • Acetates
  • Alkanes
  • Drugs, Chinese Herbal
  • Peptides, Cyclic
  • segetalin A
  • segetalin B
  • ethyl acetate
  • naphtha
  • Methanol