Preparative separation and purification of four cis–trans isomers of coumaroylspermidine analogs from safflower by high-speed counter-current chromatography
2013; Elsevier BV; Volume: 938; Linguagem: Inglês
10.1016/j.jchromb.2013.08.012
ISSN1873-376X
AutoresWencong Li, Xiaoyan Wang, Peng‐Cheng Lin, Na Hu, Qiulong Zhang, Yourui Suo, Chenxu Ding,
Tópico(s)Bioactive natural compounds
ResumoHigh-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 1.3 mg of N1, N5, N10-(E)-tri-p-coumaroylspermidine (EEE), 4.4 mg of N1(E)-N5-(Z)-N10-(E)-tri-p-coumaroylspermidine (EZE), 7.2 mg of N1(Z)-N5-(Z)-N10-(E)-tri-p-coumaroylspermidine (ZZE), and 11.5 mg of N1,N5,N10-(Z)-tri-p-coumaroylspermidine (ZZZ) were obtained from 100 mg 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.
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