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Isolation and Purification of Three Analogues from Clematis akebioides by Molecularly Imprinted Solid-Phase Extraction and HSCCC

Liu, Hongliu, Gong, Chengcheng, Liao, Zhixin, Chen, Tao, Li, Yulin
Chromatographia 2017 v.80 no.11 pp. 1651-1658
Clematis, acetic acid, acetonitrile, acrylamides, caffeic acid, chloroform, countercurrent chromatography, ferulic acid, molecular imprinting, nuclear magnetic resonance spectroscopy, p-coumaric acid, polymers, solid phase extraction, solvents
An efficient strategy of using molecularly imprinted solid-phase extraction and high-speed counter-current chromatography (HSCCC) were established for separation and purification of three analogues from Clematis akebioides for the first time. The three analogues, including 26.30 mg caffeic acid, 84.20 mg p-coumaric acid, and 44.40 mg ferulic acid, were obtained from 200.00 mg of the crude sample. The molecularly imprinted polymer was prepared with caffeic acid as template molecule and acrylamide as functional monomers. The results showed that the caffeic acid and its analogues could be well enriched. Then, the extract was purified by HSCCC using a two-phase solvent system consisting of chloroform/acetonitrile/water/acetic acid (10:5:4:0.0004, v/v) and a continuous sample introduction system was adopted. The three organic acids were identified by ¹H-NMR and ¹³C-NMR.