pH 区带精制逆流色谱法在从 Aspidosperma rigidum Rusby 中分离吲哚生物碱中的应用。
Application of pH-zone-refining countercurrent chromatography for the separation of indole alkaloids from Aspidosperma rigidum Rusby.
机构信息
Universidade Federal do Rio de Janeiro, Faculdade de Farmácia, CCS, Bl. A 2(o) andar, Ilha do Fundão 21941-590, RJ, Brazil; Institute of Food Chemistry, Technische Universität Braunschweig, Schleinitzstrasse 20, 38106 Braunschweig, Germany.
出版信息
J Chromatogr A. 2013 Dec 6;1319:166-71. doi: 10.1016/j.chroma.2013.10.044. Epub 2013 Oct 22.
Species of Aspidosperma (Apocynaceae) are characterized by the occurrence of indole alkaloids, but few recent reports on Aspidosperma rigidum Rusby chemical constituents were found. The present work shows the application of pH-zone refining countercurrent chromatography on the separation of alkaloids from the barks of A. rigidum. In this study, the dichloromethane extract was fractionated with the solvent system composed of methyl-tert-butyl ether and water with different concentrations of the retainer triethylamine in the organic stationary phase and formic or hydrochloric acids as eluters in the aqueous mobile phase, in order to evaluate the most suitable condition. In each experiment, from circa 200mg of the dichloromethane extract of A. rigidum, three major alkaloids were isolated and identified as 3α-aricine (circa 17mg), isoreserpiline (ca. 22mg) and 3β-reserpiline (ca. 40mg), with relative purity of 79%, 89% and 82% respectively, in a one-step separation of 2h. Two of them - 3α-aricine and isoreserpiline - were isolated and identified for the first time in this species.
夹竹桃科（Apocynaceae）的Aspidosperma 物种以吲哚生物碱的存在为特征，但最近关于 Aspidosperma rigidum Rusby 的化学成分的报道很少。本工作展示了 pH 区带精制逆流色谱法在分离 A. rigidum 树皮中的生物碱方面的应用。在这项研究中，二氯甲烷提取物用由甲基叔丁基醚和水组成的溶剂系统进行了分级，在有机固定相中含有不同浓度的保留三乙胺，在水相流动相中使用甲酸或盐酸作为洗脱剂，以评估最适合的条件。在每个实验中，从大约 200mg 的 A. rigidum 二氯甲烷提取物中，分离并鉴定出三种主要生物碱，分别为 3α-阿林碱（约 17mg）、异蛇根碱（约 22mg）和 3β-蛇根碱（约 40mg），纯度分别为 79%、89%和 82%，在 2 小时的一步分离中即可得到。其中两种——3α-阿林碱和异蛇根碱——是首次在该物种中分离出来的。
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