利用高速逆流色谱法从苦木中制备分离和纯化生物碱
Preparative isolation and purification of alkaloids from Picrasma quassiodes (D. Don) Benn. by high-speed countercurrent chromatography.
作者信息
Zhao Wenna, He Jiao, Zhang Yongmin, Ito Yoichiro, Su Qi, Sun Wenji
机构信息
Biomedicine Key Laboratory of Shaanxi Province, Northwest University, Xi'an 710069, P.R. China.
出版信息
J Liq Chromatogr Relat Technol. 2012;35(11):1597-1606. doi: 10.1080/10826076.2011.621150. Epub 2012 Jun 22.
Abstract
By using a two-phase solvent system composed of n-hexane-ethyl acetate-methanol-water (2:2:2:2, v/v/v/v), a high-speed counter-current chromatography technique was successfully used for isolation and purification of three alkaloids from Picrasma quassiodes (D. Don) Benn. for the first time. A total of 22.1 mg of 3-methylcanthin-2,6-dione, 4.9 mg of 4-methoxy-5-hydroxycanthin-6-one and 1.2 mg of 1-mthoxycarbonyl-β-carboline were obtained from 100 mg of crude extract of Picrasma quassiodes (D. Don) Benn. in less than 5 h, with purities of 89.30%, 98.32% and 98.19%, respectively. The target compounds were identified by ESI-MS, (1)H NMR and (13)C NMR.
摘要
通过使用由正己烷 - 乙酸乙酯 - 甲醇 - 水（2:2:2:2，v/v/v/v）组成的两相溶剂系统，首次成功地运用高速逆流色谱技术从苦木（Picrasma quassiodes (D. Don) Benn.）中分离纯化出三种生物碱。从100 mg苦木（Picrasma quassiodes (D. Don) Benn.）粗提取物中，在不到5小时内获得了总共22.1 mg的3 - 甲基 - 2,6 - 二氧代坎替啶、4.9 mg的4 - 甲氧基 - 5 - 羟基 - 6 - 氧代坎替啶和1.2 mg的1 - 甲氧基羰基 - β - 咔啉，纯度分别为89.30%、98.32%和98.19%。通过电喷雾电离质谱（ESI - MS）、氢核磁共振（¹H NMR）和碳核磁共振（¹³C NMR）对目标化合物进行了鉴定。
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