pH 区带精制逆流色谱法从云南白药中分离异喹啉生物碱。
Preparative separation of isoquinoline alkaloids from Stephania yunnanensis by pH-zone-refining counter-current chromatography.
机构信息
Department of Chemistry, Zhejiang University, 38 Zheda Road, Hangzhou 310027, China.
出版信息
J Chromatogr B Analyt Technol Biomed Life Sci. 2010 Jul 1;878(21):1881-4. doi: 10.1016/j.jchromb.2010.05.005. Epub 2010 May 9.
In this paper, five isoquinoline alkaloids were successfully separated from a crude extract of Stephania yunnanensis using pH-zone-refining counter-current chromatography in single-step. With a two-phase solvent system composed of methyl-tert-butyl ether (MtBE)-acetonitrile-water (2:2:3, v/v) where triethylamine (10 mM) was added to the upper organic phase as a retainer and hydrochloric acid (5 mM) to the aqueous mobile phase as an eluter. From 1.4 g crude extract, 68.7 mg isocorydine, 78.2 mg corydine, 583.4 mg tetrahydropalmatine, 36.3 mg N-methylasimilobine, and 47.3 mg anonaine were separated with purities over 90%. Their structures were identified by (1)H NMR, (13)C NMR, ESI-MS data.
本文采用 pH 区带逆流色谱法，从云南千金藤粗提物中一步法成功分离得到 5 种异喹啉生物碱。两相溶剂系统由甲基叔丁基醚（MtBE）-乙腈-水（2:2:3，v/v）组成，在上相有机相中添加三乙胺（10 mM）作为保留剂，在水相流动相中添加盐酸（5 mM）作为洗脱剂。从 1.4 g 粗提物中，分离得到 68.7 mg 异紫堇定碱、78.2 mg 刻叶紫堇碱、583.4 mg 延胡索乙素、36.3 mg N-甲基原小檗碱和 47.3 mg 蝙蝠葛任碱，纯度均超过 90%。通过（1）H NMR、（13）C NMR、ESI-MS 数据鉴定了它们的结构。
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