Case Ryan J, Wang Yuehong, Franzblau Scott G, Soejarto D Doel, Matainaho Lohi, Piskaut Pius, Pauli Guido F
Institute for Tuberculosis Research, University of Illinois at Chicago, Chicago, IL 60612, USA.
J Chromatogr A. 2007 Jun 1;1151(1-2):169-74. doi: 10.1016/j.chroma.2007.01.022. Epub 2007 Jan 11.
Through several steps of in vitro based bioassay-guided fractionation, three highly potent anti-mycobacterial constituents (1-2 microg/mL minimum inhibitory concentrations) were isolated from Dracaena angustifolia Roxb. (Dracaenaceae). Isolation was expedited due to the application of new techniques in counter-current chromatography (CCC). The first of these applications, gradient-array CCC, enables the expansion of the high-resolution window (sweet spot) by applying successive CCC separations in different solvent systems to a crude extract. Further fractionation was also performed using the recently designed 1L fast-centrifugal partition chromatography (FCPC) rotor with the solvent system hexane:methyl-tert butylether:acetonitrile (10:1:10). Results indicated that gradient-array CCC and high-capacity FCPC can facilitate drug discovery efforts from complex natural products, increase reproducibility of separation schemes, and provide more rigid dereplication of previously isolated bioactive compounds.
通过基于体外生物测定指导的分级分离的几个步骤,从狭叶龙血树(龙舌兰科)中分离出三种高效抗分枝杆菌成分(最低抑菌浓度为1-2微克/毫升)。由于在逆流色谱(CCC)中应用了新技术,分离过程得以加快。这些应用中的第一个,梯度阵列CCC,通过在不同溶剂系统中对粗提物进行连续的CCC分离,能够扩大高分辨率窗口(最佳点)。还使用最近设计的1L快速离心分配色谱(FCPC)转子,以正己烷:甲基叔丁基醚:乙腈(10:1:10)的溶剂系统进行了进一步分级分离。结果表明,梯度阵列CCC和高容量FCPC可以促进从复杂天然产物中发现药物,提高分离方案的重现性,并对先前分离的生物活性化合物进行更严格的去重复。