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Method for separating swainsonine by using counter-current chromatography

A technology of swainsonine and countercurrent chromatography, applied in the direction of organic chemistry, etc., to achieve the effect of safe preparation process, high separation efficiency and simple operation

Active Publication Date: 2014-12-24
LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There is no report on the application of countercurrent chromatography to separate swainsonine monomeric compounds in the existing literature. Therefore, the present invention discloses a method for separating swainsonine monomeric compounds in the total alkaloid extract of Oxytropis chinensis by using countercurrent chromatography. method

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Embodiment 1

[0026] Separation of swainsonine monomers in the total alkaloid extract of Oxytropis gansuensis by high-speed countercurrent chromatography.

[0027] 1. Sample: total alkaloids of Oxytropis gansu, extracted from Oxytropis gansu with reference to the patent preparation process for extracting total alkaloids from Oxytropis gansu (application number: 200910117752.5).

[0028] 2. Instrument: TBE-300B countercurrent chromatograph, Shanghai Tongtian Biotechnology Co., Ltd., China.

[0029] 3. Preparation method: Mix methyl tert-butyl ether: n-butanol: water in a ratio of 1:3:4 (v:v), mix well, add ammonia water dropwise to adjust the pH to 9-10, and place it in a separatory funnel Set aside for stratification. Release the upper and lower phases respectively and degas them by ultrasonication for 20 minutes. The upper phase is the stationary phase and the lower phase is the mobile phase. First, pump the stationary phase into the spiral tube of the countercurrent chromatograph at a f...

Embodiment 2

[0031] 1. Sample: total alkaloids of Oxytropis gansu, extracted from Oxytropis gansu with reference to the patent preparation process for extracting total alkaloids from Oxytropis gansu (application number: 200910117752.5).

[0032] 2. Instrument: DE HPCCC Spectrum countercurrent chromatograph, British DE company.

[0033] 3. Preparation method: Mix methyl tert-butyl ether: n-butanol: water according to the ratio of 1:3:4 (v:v), mix well, add ammonia water to it to adjust the pH to 9-10, then place it in the liquid separation Let stand overnight in the funnel. Release the upper and lower phases respectively and degas them by ultrasonication for 20 minutes. The upper phase is the stationary phase and the lower phase is the mobile phase. First, pump the stationary phase into the spiral tube of the countercurrent chromatograph at a flow rate of 6mL / min. After the spiral tube is completely filled with the stationary phase, turn on the main engine of the countercurrent chromatogra...

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Abstract

The invention discloses a method for separating swainsonine by using counter-current chromatography. According to the invention, methyl tert-butyl ether, n-butanol and water are mixed and then stood for layering so as to form a solvent system for a counter-current chromatographic stationary phase and a counter-current chromatographic mobile phase; the stationary phase is pumped into a separation column of a counter-current chromatographic instrument at a great flow velocity; after the separation column is full of the stationary phase, the instrument is started, the main engine of the counter-current chromatographic instrument is allowed to rotate at a set rotating speed, and then the mobile phase is pumped into the separation column at a certain flow velocity; after the two phases reach dynamic balance in the separation column, sample introduction is carried out through a sample introduction valve; fractions are collected by an automatic fraction collector; and thin layer chromatography and high performance liquid chromatography are used for detection, fractions containing a swainsonine component are combined together, then a solvent is recovered, and recrystallization is carried out so as to obtain swainsonine with a purity greater than 90%. The method provided by the invention has the advantages of easiness, convenience, fastness, a good separation effect, a great preparation quantity, small loss of a sample, low separation cost, high product purity and suitability for industrial production.

Description

technical field [0001] The invention belongs to the field of natural product chemistry and relates to a method for separating swainsonine by countercurrent chromatography. Background technique [0002] Swainsonine (SW) is a highly polar indolizidine alkaloid. Studies have shown that swainsonine not only inhibits the growth and metastasis of tumor cells, but also stimulates the growth and development of bone marrow cells in the body. Proliferation, enhance the body's immunity (Lu Hao, et al. Research progress on the anti-tumor effect of swainsonine, Advances in Veterinary Medicine, 2009, 30(9): 87-90). Therefore, in recent years, as a brand-new anticancer drug, swainsonine has attracted the attention of researchers at home and abroad. Abroad, the research on swainsonine has entered the stage of clinical research for the treatment of tumors, while domestically, its antitumor activity research is still in its infancy. [0003] Due to the special anti-tumor activity and bidire...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D471/04
Inventor 邸多隆黄新异陈小芬
Owner LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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