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Preparative separation and purification of four cis–trans isomers of coumaroylspermidine analogs from safflower by high-speed counter-current chromatography

Author:
Li, Wen-Cong, Wang, Xiao-Yan, Lin, Peng-Cheng, Hu, Na, Zhang, Qiu-Long, Suo, You-Rui, Ding, Chen-Xu
Source:
Journal of Chromatography B 2013 v.938 pp. 75-79
ISSN:
1570-0232
Subject:
Carthamus tinctorius, carbon, cis-trans isomers, countercurrent chromatography, electrospray ionization mass spectrometry, high performance liquid chromatography, nuclear magnetic resonance spectroscopy, solvents, stable isotopes
Abstract:
High-speed counter-current chromatography (HSCCC) was successfully applied for the first time to isolate and purify four cis–trans isomers of coumaroylspermidine analogs from Safflower. HSCCC separation was achieved with a two-phase solvent system composed of chloroform–methanol–water (1:1:1, v/v/v) with the upper phase as the mobile phase. In a single run, a total of 1.3mg of N1, N5, N10-(E)-tri-p-coumaroylspermidine (EEE), 4.4mg of N1(E)-N5-(Z)-N10-(E)-tri-p-coumaroylspermidine (EZE), 7.2mg of N1(Z)-N5-(Z)-N10-(E)-tri-p-coumaroylspermidine (ZZE), and 11.5mg of N1,N5,N10-(Z)-tri-p-coumaroylspermidine (ZZZ) were obtained from 100mg of crude sample. High Performance Liquid Chromatography (HPLC) analysis showed that the purities of these four components are 95.5%, 98.1%, 97.5% and 96.2%, respectively. The chemical structures were identified by ESI-MS, 1H NMR and 13C NMR.
Agid:
1004730