高速逆流色谱法从狭叶松果菊（DC.）Hell.根中分离烷基酰胺。

Purification of alkylamides from Echinacea angustifolia (DC.) Hell. Roots by high-speed countercurrent chromatography.

机构信息

Department of Agricultural, Food and Nutritional Science, 4-10 Agriculture/Forestry Centre, University of Alberta, Edmonton, Alberta T6G 2P5, Canada.

出版信息

J Agric Food Chem. 2011 Jan 26;59(2):491-4. doi: 10.1021/jf103436p. Epub 2010 Dec 29.

DOI:10.1021/jf103436p

PMID:21190380

Abstract

High-speed countercurrent chromatography (HSCCC) was used for the separation of alkylamides from the roots of Echinacea angustifolia (DC.) Hell. For this purpose, the alkylamides were extracted with hexane and subjected to semipreparative HSCCC using a two-phase solvent system consisting of n-hexane, ethyl acetate, methanol, and water (4:1:2:1). The lower aqueous phase was used as the mobile phase at a flow rate of 3 mL/min and a rotary speed of 1000 rpm. This procedure led to the isolation of four pure alkylamides, that is, dodeca-2E,4E,8Z,10E/Z-tetraenoic acid isobutylamide (38.9 mg, 97% purity), dodeca-2E,4E,8Z-trienoic acid isobutylamide (4.4 mg, 92% purity), dodeca-2E,4E-dienoic acid isobutylamide (3.2 mg, 99% purity), and dodeca-2E,4E-dienoic acid 2-methylbutylamide (0.3 mg, 92% purity). The identity and purity of the isolated alkylamides were confirmed by LC-ESI-MS and (1)H NMR and (13)C NMR data. To the best of the authors' knowledge, this is the first report of dodeca-2E,4E-dienoic acid 2-methylbutylamide in E. angustifolia roots.

摘要

高速逆流色谱（HSCCC）用于从狭叶紫锥菊（Echinacea angustifolia（DC.）Hell）的根部分离烷基酰胺。为此，用正己烷提取烷基酰胺，并使用由正己烷、乙酸乙酯、甲醇和水（4:1:2:1）组成的两相溶剂系统进行半制备 HSCCC。较低的水相用作流动相，流速为 3 mL/min，转速为 1000 rpm。该程序导致分离出四种纯烷基酰胺，即十二碳-2E、4E、8Z、10E/Z-四烯酸异丁酰胺（38.9 mg，97%纯度）、十二碳-2E、4E、8Z-三烯酸异丁酰胺（4.4 mg，92%纯度）、十二碳-2E、4E-二烯酸异丁酰胺（3.2 mg，99%纯度）和十二碳-2E、4E-二烯酸 2-甲基丁酰胺（0.3 mg，92%纯度）。通过 LC-ESI-MS 和（1）H NMR 和（13）C NMR 数据确认分离的烷基酰胺的身份和纯度。据作者所知，这是首次在狭叶紫锥菊根中报道十二碳-2E、4E-二烯酸 2-甲基丁酰胺。