采用常规逆流色谱法和pH区带精制逆流色谱法从苦木（Picrasma quassioides (D. Don) Benn.）中制备分离生物碱。
Preparative separation of alkaloids from Picrasma quassioides (D. Don) Benn. by conventional and pH-zone-refining countercurrent chromatography.
作者信息
Zhang Qinghai, Shu Xikai, Jing Feng, Wang Xiao, Lin Changhu, Luo Aiqin
机构信息
Department of Biochemical Engineering, School of Life Science, Beijing Institute of Technology, Beijing 100081, China.
TCM Process Control Research Center, Shandong Analysis and Test Center, Shandong Academy of Sciences, 19 Keyuan Street, Jinan 250014, China.
出版信息
Molecules. 2014 Jun 25;19(7):8752-61. doi: 10.3390/molecules19078752.
Two high-speed countercurrent chromatography (HSCCC) modes were compared by separation of major alkaloids from crude extract of Picrasma quassioides. The conventional HSCCC separation was performed with a two-phase solvent system composed of petroleum ether-ethyl acetate-methanol-water (5:5:4.5:5.5, v/v/v/v) with 200 mg loading. pH-Zone-refining CCC was performed with two-phase solvent system composed of petroleum ether-ethyl acetate-n-butanol-water (3:2:7:9, v/v/v/v) where triethylamine (10 mM) was added to the upper organic stationary phase and hydrochloric acid (5 mM) was added to the lower aqueous phase with 2 g loading. From 2 g of crude extract, 87 mg of 5-methoxycanthin-6-one (a), 38 mg of 1-methoxy-β-carboline (b), 134 mg of 1-ethyl-4,8-dimethoxy-β-carboline (c), 74 mg of 1-ethoxycarbonyl-β-carboline (d), 56 mg of 1-vinyl-4,8-dimethoxy-β-carboline (e) and 26 mg of 1-vinyl-4-dimethoxy-β-carboline (f) were obtained with purities of over 97.0%. The results indicated that pH-zone-refining CCC is an excellent separations tool at the multigram level.
通过从苦木粗提物中分离主要生物碱，比较了两种高速逆流色谱（HSCCC）模式。传统的HSCCC分离是在由石油醚 - 乙酸乙酯 - 甲醇 - 水（5:5:4.5:5.5，v/v/v/v）组成的两相溶剂系统中进行，上样量为200 mg。pH区带精制CCC是在由石油醚 - 乙酸乙酯 - 正丁醇 - 水（3:2:7:9，v/v/v/v）组成的两相溶剂系统中进行，其中向上层有机固定相中加入三乙胺（10 mM），向下层水相中加入盐酸（5 mM），上样量为2 g。从2 g粗提物中，得到了87 mg的5 - 甲氧基坎替 - 6 - 酮（a）、38 mg的1 - 甲氧基 - β - 咔啉（b）、134 mg的1 - 乙基 - 4,8 - 二甲氧基 - β - 咔啉（c）、74 mg的1 - 乙氧羰基 - β - 咔啉（d）、56 mg的1 - 乙烯基 - 4,8 - 二甲氧基 - β - 咔啉（e）和26 mg的1 - 乙烯基 - 4 - 二甲氧基 - β - 咔啉（f），纯度均超过97.0%。结果表明，pH区带精制CCC是一种毫克级的优秀分离工具。
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