通过pH区带精制逆流色谱法从西伯利亚白刺叶中分离纯化两种新生物碱和两种已知生物碱。
Separation and purification of two new and two known alkaloids from leaves of Nitraria sibirica by pH-zone-refining counter-current chromatography.
作者信息
Bakri Mahinur, Chen Qibin, Ma Qingling, Yang Yi, Abdukadir Abdumijit, Aisa Haji Akber
机构信息
The Key Laboratory of Plant Resources and Chemistry in Arid Regions and Key Laboratory of Xinjiang Indigenous Medicinal Plants Resource Utilization, Xinjiang Technical Institute of Physics and Chemistry, Chinese Academy of Sciences, Urumqi, China.
The Key Laboratory of Plant Resources and Chemistry in Arid Regions and Key Laboratory of Xinjiang Indigenous Medicinal Plants Resource Utilization, Xinjiang Technical Institute of Physics and Chemistry, Chinese Academy of Sciences, Urumqi, China; University of Chinese Academy of Sciences, Beijing, China.
出版信息
J Chromatogr B Analyt Technol Biomed Life Sci. 2015 Dec 1;1006:138-145. doi: 10.1016/j.jchromb.2015.10.038. Epub 2015 Nov 11.
The total alkaloids from Nitraria sibirica leaves have been confirmed to exhibit significant protective effects against inflammatory renal injury, hypertension and albuminuria in angiotensin II-salt hypertension. In the present study, a separation method of pH-zone-refining counter-current chromatography was established for separation of the alkaloids from N. sibirica. The separation was performed with a solvent system of MtBE-n-BuOH-H2O (2:2:5, v/v) at a flow rate of 2.0mL/min. And 15mM triethylamine (TEA) was added to the upper organic phase, while 10mM hydrochloric acid was added to the lower aqueous phase. As a result, a new alkaloid, schobemine (5.6mg), and a known alkaloid, nitraramine (5.0mg), together with fractions A and B were obtained from the total alkaloids of N. sibirica. The fractions A and B were further purified by means of pH-zone-refining counter-current chromatography with solvent systems of n-hexane-n-BuOH-H2O (1.5:3.5:5, v/v) and (2:3:5, v/v), respectively. TEA (10mM) was added to the upper phase, and 10mM of HCl was added to the lower phase in above two solvent systems, respectively. As a result, a known alkaloid, schoberidine (5.0mg), and a new alkaloid, schoberimine (3.0mg) were obtained from fractions A and B, respectively. The purities of the compounds were measured by HPLC-ELSD, and their structures were identified by ESI-MS, 1D and 2D NMR.
西伯利亚白刺叶中的总生物碱已被证实对血管紧张素 II 盐性高血压引起的炎症性肾损伤、高血压和蛋白尿具有显著的保护作用。在本研究中，建立了一种pH区带精制逆流色谱分离方法，用于从西伯利亚白刺中分离生物碱。分离采用甲基叔丁基醚-正丁醇-水（2:2:5，v/v）的溶剂系统，流速为2.0mL/min。在上层有机相中加入15mM三乙胺（TEA），在下层水相中加入10mM盐酸。结果，从西伯利亚白刺总生物碱中得到了一种新生物碱schobemine（5.6mg）、一种已知生物碱nitraramine（5.0mg）以及组分A和B。组分A和B分别通过pH区带精制逆流色谱进一步纯化，溶剂系统分别为正己烷-正丁醇-水（1.5:3.5:5，v/v）和（2:3:5，v/v）。在上述两种溶剂系统中，分别在上层相中加入10mM TEA，在下层相中加入10mM HCl。结果，分别从组分A和B中得到了一种已知生物碱schoberidine（5.0mg）和一种新生物碱schoberimine（3.0mg）。通过HPLC-ELSD测定化合物的纯度，并通过ESI-MS、一维和二维NMR鉴定其结构。
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