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Application of high-speed counter-current chromatography for preparative separation of cyclic peptides from Vaccaria segetalis
- Wang, Xiao, Dong, Hongjing, Liu, Yuqin, Yang, Bin, Wang, Xia, Huang, Luqi
- Journal of chromatography 2011 v.879 no.11-12 pp. 811-814
- Vaccaria hispanica subsp. hispanica, chemical structure, countercurrent chromatography, cyclic peptides, high performance liquid chromatography, ionization, nuclear magnetic resonance spectroscopy, petroleum, seeds, silica gel, solvents
- 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 190mg of crude extract, 38.0mg of segetalin B and 28.5mg 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 ¹H NMR analyses.