Preparative separation of high-purity cordycepin from Cordyceps militaris (L.) Link by high-speed countercurrent chromatography

Zhu, L.; Liang, Y.; Lao, D.; Zhang, T.; Ito, Y.

Journal of Liquid Chromatography and Related Technologies 37(7): 491-499

2011


ISSN/ISBN: 1082-6076
PMID: 21643461
DOI: 10.1080/10826076.2011.556965
Accession: 055137995

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Abstract
A high-speed counter-current chromatography (HSCCC) technique in a preparative scale has been applied to separate and purify cordycepin from the extract of Cordyceps militaris(L.) Link by a one-step separation. A high efficiency of HSCCC separation was achieved on a two-phase solvent system of n-hexane-n-butanol-methanol-water (23:80:30:155, v/v/v/v) by eluting the lower mobile phase at a flow rate of 2 ml/min under a revolution speed of 850 rpm. HSCCC separation of 216.2 mg crude sample (contained cordycepin at 44.7% purity after 732 cation-exchange resin clean-up) yielded 64.8 mg cordycepin with purity of 98.9% and 91.7% recovery. Identification of the target compound was performed by UV, IR, MS, (1)H NMR and (13)C NMR.