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Method for separating and preparation of Gelsemium elegans alkaloid monomer by high speed counter current chromatography

A technology of high-speed countercurrent chromatography and hook kiss alkaloids, which is applied in separation methods, chemical instruments and methods, solid adsorbent liquid separation, etc., can solve the problems of unsatisfactory separation effect, long separation cycle, low recovery rate, etc. Effect of separation cycle, long separation cycle, and less sample loss

Active Publication Date: 2010-12-29
FUJIAN MEDICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantages of column chromatography are: long separation period, low recovery rate and unsatisfactory separation effect
In the existing literature, there are no domestic and foreign reports on the separation of Gelnectis alkaloid monomers by high-speed countercurrent chromatography

Method used

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  • Method for separating and preparation of Gelsemium elegans alkaloid monomer by high speed counter current chromatography
  • Method for separating and preparation of Gelsemium elegans alkaloid monomer by high speed counter current chromatography
  • Method for separating and preparation of Gelsemium elegans alkaloid monomer by high speed counter current chromatography

Examples

Experimental program
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Effect test

Embodiment 1

[0032] High-speed counter-current chromatography for the separation of gelzia alkaloids monomer geskinin from the total alkaloids (see figure 1 ).

[0033] 1. Sample: total alkaloids of Gelcyonium, referring to the classic extraction method of Gelkins alkaloids (Chen Zhongliang. Extraction and separation of Gelkins alkaloids, Bulletin of Traditional Chinese Medicine, 1987, 12(5): 41; Xu Jian, Liang Chongzhen. Comparison of extraction methods of total alkaloids of Gelkins, Pharmaceutical Bulletin, 1988, 23(6): 341-342; Chen Jingfeng, Yuan Hui. Extraction, separation, identification and general toxicity of total alkaloids of Gelkins, Journal of Hunan Agricultural University (Natural Science Edition), 2003, 29(5): 422-425) extracted from the rhizome of Ficus genus.

[0034] 2. Instrument: TBE-300A high-speed countercurrent chromatograph, Shanghai Tongtian Biotechnology Co., Ltd.

[0035] 3. Method:

[0036]3.1 Prepare a solvent system, n-hexane: ethyl acetate: absolute ethanol...

Embodiment 2

[0042] High-speed countercurrent chromatography for the separation of kelsinin A and kelsinin, the alkaloid monomers of kiskinin. (See figure 2 )

[0043] This example is an example of the step-by-step separation of the monomers of kinesis alkaloids by high-speed countercurrent chromatography. In the first step, high-speed countercurrent chromatography is used to separate kelkinin, and the specific method is detailed in Example 1; in the second step, the components that cannot be separated by high-speed countercurrent chromatography in the first step are collected and concentrated, and used as a new separated sample. After separation by high-speed countercurrent chromatography again, kelezine A and kelezine can be obtained. This embodiment only describes the second step.

[0044] 2.1 Sample: the two components of kaclelin A and kaclelin I that could not be separated in Example 1 (i.e. figure 1 Components 2 and 3) were combined, evaporated to dryness under reduced pressure...

Embodiment 3

[0053] High-speed counter-current chromatography was used to separate four monomers of kelezin, kelezin A and kelezin. (See image 3 )

[0054] 1. Sample: total alkaloids of Gelcyonium, referring to the classic extraction method of Gelkins alkaloids (Chen Zhongliang. Extraction and separation of Gelkins alkaloids, Bulletin of Traditional Chinese Medicine, 1987, 12(5): 41; Xu Jian, Liang Chongzhen. Comparison of extraction methods of total alkaloids of Gelkins, Pharmaceutical Bulletin, 1988, 23(6): 341-342; Chen Jingfeng, Yuan Hui. Extraction, separation, identification and general toxicity of total alkaloids of Gelkins, Journal of Hunan Agricultural University (Natural Science Edition), 2003, 29(5): 422-425) extracted from the rhizome of Ficus genus.

[0055] 2. Instrument: TBE-300A high-speed countercurrent chromatograph, Shanghai Tongtian Biotechnology Co., Ltd.

[0056] 3. Method:

[0057] 3.1 Prepare a solvent system, 2000ml of chloroform:methanol:0.2mol / l hydrochloric...

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Abstract

The invention discloses a method for separating and preparing a gelsemium alkaloid monomer from gelsemium by adopting high-speed counter current chromatography, which pertains to the separation method of medicinal plant monomers. The invention takes total alkaloids of gelsemium as a raw material and a high-speed counter current chromatograph as a separating device and the method comprises that a solvent system which is composed of stationary phase and mobile phase is prepared; the high-speed counter current chromatograph is filled with the stationary phase and then the mobile phase is pumped in and balanced; and then sampling is conducted by a sample valve; target components are collected according to the map of a detector or in combination of the detection methods of high efficiency liquid chromatography and thin layer chromatography, and distilled under reduced pressure and then recrystallized to obtain the gelsemium alkaloid monomer with high purity. By adjusting the specific proportional parameters of the solvent system, single or multiple target gelsemium alkaloid monomers can be separated by one step or step by step. The method is convenient and efficient, large in preparation amount, less in sample loss, good in separation effect and high in controllability and applicable to automatic production and the obtained gelsemium alkaloid monomer from separation has diverse pharmacological activities and application prospect to be prepared into medicines.

Description

technical field [0001] The invention relates to a method for separating medicinal plant monomers, in particular to a method for separating and preparing the alkaloid monomers from glyphs by using high-speed countercurrent chromatography. Background technique [0002] Gelsemium elegans Benth. (GEB) is the whole plant of Gelsemium elegans Benth., which is divided into Chinese elegans and North American elegans. In my country, it is rich in Zhejiang, Fujian, Guangdong, Guangxi, Hunan, Guizhou, Yunnan and other places. Abroad, in 1887, H Gerrad et al. made it into a Green preparation, which was recorded in some national secondary pharmacopoeias; the American Drug Index and Japan's "World's Folk Medicine" all have records of Gelkin. Our country has a longer history of research on Glycyrrhizae, which is recorded in "Shen Nong's Materia Medica" and "Compendium of Materia Medica". The folks in my country have been using the original plant of Glycyrrhizae to treat various pains, esp...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D491/18B01D15/30
Inventor 俞昌喜许盈刘浩
Owner FUJIAN MEDICAL UNIV
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