pH 区带精制逆流色谱法从延胡索中大规模分离生物碱。

Large-scale separation of alkaloids from Corydalis bungeana Turcz. by pH-zone-refining counter-current chromatography.

机构信息

Shandong Analysis and Test Center, Shandong Academy of Sciences, 19 Keyuan Street, Jinan 250014, Shandong, China.

出版信息

Molecules. 2012 Dec 17;17(12):14968-74. doi: 10.3390/molecules171214968.

DOI:10.3390/molecules171214968

PMID:23247369

原文链接:https://pmc.ncbi.nlm.nih.gov/articles/PMC6268814/

Abstract

pH-Zone-refining counter-current chromatography (pH-zone-refining CCC) was successfully applied for the large-scale separation of alkaloids from Corydalis bungeana. The crude extract was separated by a two-phase solvent system composed of petroleum ether-ethyl acetate-methanol-water (5:5:2:8, v/v) where triethylamine (10 mM) was added to the upper organic stationary phase as a retainer and hydrochloric acid (5 mM) to the aqueous mobile phase as a displacer. As a result, 285 mg of protopine, 86 mg of corynoloxine, 430 mg of coryno1ine, and 115 mg of acetylcorynoline were obtained from 3.0 g of crude extract in a one-step separation. The purities of these compounds were 99.1%, 98.3%, 99.0% and 98.5%, respectively, as determined by HPLC. The chemical structures of these isolated compounds were confirmed by ESI-MS, ¹H-NMR and ¹³C-NMR.

摘要

pH 区域精制逆流色谱（pH-zone-refining CCC）成功应用于从延胡索中大规模分离生物碱。粗提取物通过两相溶剂系统分离，该系统由石油醚-乙酸乙酯-甲醇-水（5:5:2:8，v/v）组成，在上有机固定相中加入三乙胺（10 mM）作为保留剂，在上有机固定相中加入盐酸（5 mM）作为置换剂。结果，从 3.0 g 粗提取物中一步分离得到 285 mg 原阿片碱、86 mg 山姜诺林碱、430 mg 山姜诺林碱和 115 mg 乙酰山姜诺林碱。这些化合物的纯度分别通过 HPLC 确定为 99.1%、98.3%、99.0%和 98.5%。通过 ESI-MS、1H-NMR 和 13C-NMR 确证了这些分离化合物的化学结构。