高速逆流色谱法从朝鲜乌头中制备分离和纯化两种新的异构二萜生物碱
Preparative isolation and purification of two new isomeric diterpenoid alkaloids from Aconitum coreanum by high-speed counter-current chromatography.
作者信息
Tang Qingfa, Liu Jinghan, Xue Jiao, Ye Wencai, Zhang Zunjian, Yang Chunhua
机构信息
Key Laboratory of Research of Traditional Chinese Medicine and New Drug, Southern Medical University, Guangzhou 510515, China.
出版信息
J Chromatogr B Analyt Technol Biomed Life Sci. 2008 Sep 1;872(1-2):181-5. doi: 10.1016/j.jchromb.2008.07.030. Epub 2008 Jul 30.
Preparative high-speed counter-current chromatography (HSCCC) coupled with evaporative light scattering detection (ELSD) was used to isolate and separate bioactive constituents from the roots of Aconitum coreanum. Two new diterpenoid alkaloid isomers were successfully separated for the first time by HSCCC with an optimized two-phase solvent system composed of ethyl acetate-n-butanol-methanol-2% acetic acid (3.5:1.5:2:4.5, v/v/v/v), 25.4 mg of GFT (1) and 18.3 mg of GFU (2) were isolated form 1 g crude extract in one step HSCCC experiment. The purities of the two new compounds were all over 95% as analyzed by HPLC and their structures were identified by ESI-MS, (1)H NMR, (13)C NMR, and 2D NMR analysis.
采用制备型高速逆流色谱（HSCCC）结合蒸发光散射检测（ELSD）从朝鲜乌头根中分离生物活性成分。通过HSCCC首次成功分离出两种新的二萜生物碱异构体，优化的两相溶剂体系为乙酸乙酯 - 正丁醇 - 甲醇 - 2%乙酸（3.5:1.5:2:4.5，v/v/v/v），在一次HSCCC实验中，从1 g粗提物中一步分离得到25.4 mg的GFT（1）和18.3 mg的GFU（2）。通过HPLC分析，两种新化合物的纯度均超过95%，并通过电喷雾电离质谱（ESI-MS）、氢核磁共振（¹H NMR）、碳核磁共振（¹³C NMR）和二维核磁共振（2D NMR）分析确定了它们的结构。
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