Milato Jonatas Vicente, Silva Raphael Salles Ferreira, Figueiredo Fabiana de Souza, Azevedo Debora de Almeida, Ribeiro Carlos Alexandre Bulchi, Leitão Gilda Guimarães
Universidade Federal do Rio de Janeiro, Instituto de Pesquisas de Produtos Naturais, CCS, Bl. H, Ilha do Fundão, Rio de Janeiro, RJ, Brazil.
Instituto Federal de Educação, Ciência e Tecnologia do Rio de Janeiro, Campus Rio de Janeiro, Maracanã, Rio de Janeiro, RJ, Brazil.
J Chromatogr A. 2018 Feb 16;1537:135-140. doi: 10.1016/j.chroma.2018.01.020. Epub 2018 Jan 9.
A solvent system was developed for selective isolation by high-speed counter-current chromatography (HSCCC) of the benzoquinone 7α-hydroxyroileanone, 1, a bioactive diterpene from a dichloromethane extract of Tetradenia riparia leaves. Several solvent systems were initially studied, including hexane-ethyl acetate-methanol-water in several ratios, hexane-acetone-methanol-water, hexane-ethanol-water and hexane-acetonitrile-methanol, which gave recovery rates for the target compound between 13.4 and 35.9%. The new solvent system hexane-5% aqueous NaCO (1:1) was developed based on the chemical ionization reaction of the benzoquinone hydroxyl group in the basic pH of the carbonate solution, prompted by the extraction procedure used for the extraction of lapachol (a natural naphtoquinone) from a Tabebuia species wood. By using the HSCCC chromatograph as a liquid-liquid extractor with the above mentioned solvent system the recovery rate of 1 increased to 81.8%, affording the quinone with 97% purity.
开发了一种溶剂系统，用于通过高速逆流色谱法（HSCCC）从河岸四棱豆叶二氯甲烷提取物中选择性分离生物活性二萜苯醌7α-羟基罗勒烯酮（1）。最初研究了几种溶剂系统，包括不同比例的己烷-乙酸乙酯-甲醇-水、己烷-丙酮-甲醇-水、己烷-乙醇-水和己烷-乙腈-甲醇，目标化合物的回收率在13.4%至35.9%之间。基于在碳酸盐溶液碱性pH条件下苯醌羟基的化学电离反应，开发了新的溶剂系统己烷-5%碳酸钠水溶液（1:1），这是受从Tabebuia属木材中提取拉帕醇（一种天然萘醌）的提取程序启发。通过使用HSCCC色谱仪作为液-液萃取器，采用上述溶剂系统，1的回收率提高到81.8%，得到纯度为97%的醌。
