Preparative separation and purification of four cis-trans isomers of coumaroylspermidine analogs from safflower by high-speed counter-current chromatography.
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 N(1), N(5), N(10)-(E)-tri-p-coumaroylspermidine (EEE), 4.4mg of N(1)(E)-N(5)-(Z)-N(10)-(E)-tri-p-coumaroylspermidine (EZE), 7.2mg of N(1)(Z)-N(5)-(Z)-N(10)-(E)-tri-p-coumaroylspermidine (ZZE), and 11.5mg of N(1),N(5),N(10)-(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, (1)H NMR and (13)C NMR.
Key Laboratory of Tibetan Medicine Research, Northwest Institute of Plateau Biology, Chinese Academy of Sciences, Xining 810001, China; Graduate University of the Chinese Academy of Sciences, Beijing 100049, China.
Wen-Cong
WC
Li
Xiao-Yan
XY
Wang
Peng-Cheng
PC
Lin
Na
N
Hu
Qiu-Long
QL
Zhang
You-Rui
YR
Suo
Chen-Xu
CX
Ding
D031187:Carthamus tinctorius / Q000737:chemistry*; D003373:Coumaric Acids / Q000032:analysis / Q000737:chemistry / Q000302:isolation & purification*; D003377:Countercurrent Distribution / Q000379:methods*; D007536:Isomerism; D008958:Models, Molecular; D010936:Plant Extracts / Q000737:chemistry; D013095:Spermidine / Q000031:analogs & derivatives* / Q000032:analysis / Q000737:chemistry / Q000302:isolation & purification*
D003373:Coumaric Acids; D010936:Plant Extracts; D013095:Spermidine
HSCCC; Safflower; Tri-p-coumaroylspermidine