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Aporphine Alkaloids from Triclisia dictyophylla Diels by pH-Zone Refining Countercurrent Chromatography
Chromatographia ( IF 1.2 ) Pub Date : 2020-10-29 , DOI: 10.1007/s10337-020-03977-x
Eutrophe Le Doux Kamto , Simony C. Mendonça , Auguste Abouem A Zintchem , Eric Robert Tiam , Dieudonné Emmanuel Pegnyemb , Gilda Guimarães Leitão

A new dimeric aporphine alkaloid, biscocsarmine, 2 , together with lirioferine, 1 , and cocsarmine, 3 , were isolated from the ethanol extract of the stems of Triclisia dictyophylla Diels (Menispermaceae) using a preparative pH-zone refining CCC in a single step. The first solvent system family tested for this fractionation was hexane–ethyl acetate–methanol–water (HEMWat) at a series of solvent ratios, and hydrochloric acid and triethylamine at 5 mM as eluter/retainer. None of these HEMWat ratios, however, gave suitable K for the target alkaloids. Ethyl acetate– n -butanol–water (EBuWat) was tested instead and the selected solvent system was composed of ethyl acetate– n -butanol–water 5:5:10 (v/v), where triethylamine (60 mM) was added to the upper organic stationary phase as a retainer and hydrochloric acid (5 mM) to the aqueous mobile phase as an eluter. The chemical structures of the isolated compounds were elucidated based on comprehensive spectroscopic and spectrometric techniques. This is the first report of aporphine alkaloids in this plant species.

中文翻译:

pH-Zone 精制逆流色谱法测定木叶石斛的阿朴啡生物碱

使用制备性 pH 区精制 CCC,从 Triclisia dictyophylla Diels (Menispermaceae) 茎的乙醇提取物中分离出一种新的二聚阿朴啡生物碱 Biscocsarmine, 2,以及 lirioferine, 1 和 cocsarmine, 3。用于该分馏测试的第一个溶剂系统系列是一系列溶剂比的己烷-乙酸乙酯-甲醇-水 (HEMWat),以及 5 mM 的盐酸和三乙胺作为洗脱剂/保留剂。然而,这些 HEMWat 比率都没有为目标生物碱提供合适的 K。改为测试乙酸乙酯-正丁醇-水 (EBuWat),所选溶剂系统由乙酸乙酯-正丁醇-水 5:5:10 (v/v) 组成,其中,将三乙胺 (60 mM) 添加到上层有机固定相中作为保留剂,将盐酸 (5 mM) 添加到水性流动相中作为洗脱剂。基于综合光谱和光谱技术阐明了分离化合物的化学结构。这是该植物物种中阿朴啡生物碱的首次报道。
更新日期:2020-10-29
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