Tang Qingfa, Yang Chunhua, Ye Wencai, Liu Jinghan, Zhao Shouxun
Department of Natural Medicinal Chemistry, China Pharmaceutical University, Nanjing 210009, China.
J Chromatogr A. 2007 Mar 16;1144(2):203-7. doi: 10.1016/j.chroma.2007.01.058. Epub 2007 Jan 25.
Preparative high-speed counter-current chromatography (HSCCC) coupled with evaporative light scattering detection (ELSD) was employed for the isolation and purification of alkaloids from the roots of Aconitum coreanum (Lèvl.) Rapaics. The two-phase solvent system used in HSCCC was n-hexane-ethyl acetate-methanol-0.2M HCl (1:3.5:2:4.5, v/v/v/v). Six alkaloids were obtained and yielded 10.4 mg of Guanfu base P, 9.2 mg of Guanfu base G, 9.5 mg of Guanfu base F, 8.9 mg of atisine, 11.9 mg of Guanfu base A and 25.7 mg of Guanfu base I from 2 g of crude extracts. The purity of these compounds was 96.9%, 95.7%, 91.5%, 98.9%, 95.8% and 95.5%, respectively, as determined by high-performance liquid chromatography (HPLC). Their chemical structures were identified by MS, (1)H NMR and (13)C NMR.
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（Aconitum coreanum (Lèvl.) Rapaics）根中分离纯化生物碱。HSCCC中使用的两相溶剂体系为正己烷 - 乙酸乙酯 - 甲醇 - 0.2M盐酸（1:3.5:2:4.5，v/v/v/v）。从2 g粗提物中获得了6种生物碱，分别得到10.4 mg关附碱P、9.2 mg关附碱G、9.5 mg关附碱F、8.9 mg阿替生、11.9 mg关附碱A和25.7 mg关附碱I。通过高效液相色谱（HPLC）测定，这些化合物的纯度分别为96.9%、95.7%、91.5%、98.9%、95.8%和95.5%。它们的化学结构通过质谱、氢核磁共振（¹H NMR）和碳核磁共振（¹³C NMR）进行鉴定。
