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PREPARATIVE SEPARATION OF HIGH-PURITY CORDYCEPIN FROMCORDYCEPS MILITARIS(L.) LINK BY HIGH-SPEED COUNTERCURRENT CHROMATOGRAPHY
Journal of Liquid Chromatography & Related Technologies ( IF 1.0 ) Pub Date : 2011-03-26 , DOI: 10.1080/10826076.2011.556965
Licai Zhu 1 , Yong Liang , Deqiang Lao , Tianyou Zhang , Yoichiro Ito
Affiliation  

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, 1H NMR, and 13C NMR.

中文翻译:


高速逆流色谱法从蛹虫草中制备高纯度虫草素



采用制备规模的高速逆流色谱(HSCCC)技术,通过一步分离从北虫草提取物中分离纯化虫草素。通过洗脱较低的流动相,在正己烷-正丁醇-甲醇-水(23:80:30:155,v/v/v/v)两相溶剂系统上实现了高效率的 HSCCC 分离流速为 2 mL/min,转速为 850 rpm。 HSCCC分离216.2mg粗样品(经过732次阳离子交换树脂净化后,含有虫草素,纯度为44.7%),得到64.8mg虫草素,纯度为98.9%,回收率为91.7%。通过UV、IR、MS、1H NMR和13C NMR对目标化合物进行鉴定。
更新日期:2011-03-26
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