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Purifying method for verticillatine

A purification method and extraction technology, which is applied in the field of natural product separation, can solve the problems of long separation period, cumbersome operation, and large amount of preparation, and achieve the effects of reducing sample loss, overcoming cumbersome operation, and large amount of preparation

Inactive Publication Date: 2012-09-12
NANJING ZELANG MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The reason why the present invention adopts cationic resin enrichment is that vitexinlatine is in an ion state under acidic conditions, and can perform ion exchange with cationic resin and be adsorbed on cationic resin to achieve the purpose of effective separation from impurities; adopt high-speed countercurrent Chromatography is used for further separation and purification, because this separation method is easy to operate and avoids the loss of samples. Compared with traditional separation methods, it overcomes the shortcomings of cumbersome operation and long separation cycle, and has the advantages of large preparation volume and high product purity. advantage

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Get the root of 1kg Apocynaceae plant Rauvolwolfia, pulverize, extract by cold soaking with 60% methanol solution of 10LpH2 (formic acid), put the cationic resin column after the extract is concentrated and alcohol-free, and control the adsorption flow rate to be 1.5ml / min. Use 3BV50% ethanol solution to wash away the impurities, then pour the cationic resin from the chromatographic column, add ammonia water to adjust the pH to 9, use ethyl acetate to reflux and extract twice, and the extract is concentrated to dryness to obtain the crude product of Vertinatine;

[0019] Measure chloroform-methanol-0.1M HCl at a volume ratio of 8:5:3, mix ultrasonically and add to a separatory funnel, let stand to separate the upper and lower phases, take the upper phase as the stationary phase, and the lower phase as the mobile phase , dissolve the above-mentioned crude product with the lower phase, then use the upper phase pump to fill the chromatographic column, then pump the mobile p...

Embodiment 2

[0021] Get the root of 1kg Apocynaceae red fruit Rauwolfia, pulverize, and reflux extract 4 times with 60% ethanol solution of 4LpH4 (sulfuric acid), after the extract is concentrated and alcohol-free, put on a cationic resin column, and the adsorption flow rate is controlled to be 2.5ml / min , wash away impurities with 6BV50% ethanol solution, then pour out the cationic resin from the chromatographic column, add ammonia water to adjust to pH10, use ethyl acetate to reflux and extract twice, and the extract is concentrated to dryness to obtain the crude product of vertixinlatine;

[0022] Measure chloroform-methanol-0.1M HCl at a volume ratio of 7:4:3, mix ultrasonically and add to a separatory funnel, let stand to separate the upper and lower phases, take the upper phase as the stationary phase, and the lower phase as the mobile phase , dissolve the above-mentioned crude product with the lower phase, then use the upper phase pump to fill the chromatographic column, then pump th...

Embodiment 3

[0024] Get the root of 5kg Apocynaceae red fruit Rauwolfia, pulverize, and extract twice with 60% ethanol solution cold soaking of 8LpH3 (phosphoric acid), after the extract is concentrated and alcohol-free, put on a cationic resin column, and the adsorption flow rate is controlled to be 3.5ml / Min, wash away impurities with 5BV50% ethanol solution, then pour out the cationic resin from the chromatographic column, add ammonia water to adjust to pH9, use ethyl acetate to reflux and extract twice, and the extract is concentrated to dryness to obtain the crude product of vertixinlatine;

[0025] Measure chloroform-methanol-0.1M HCl at a volume ratio of 6:4:3, mix ultrasonically and add to a separatory funnel, let stand to separate the upper and lower phases, take the upper phase as the stationary phase, and the lower phase as the mobile phase , dissolve the above-mentioned crude product with the lower phase, then use the upper phase pump to fill the chromatographic column, then pu...

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PUM

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Abstract

The invention relates to a purifying method for verticillatine. Process steps include crushing roots of apocynaceae plant rauwolfia varticillata; performing cold-soaking or backflow extraction by acid alcohol solution once to four times; combining extracting solution; concentrating the extracting solution to be alcohol-free and applying the extracting solution onto a cation exchange resin column; removing impurities by neutral alcohol solution; pouring cation exchange resin from a chromatographic column; adding ammonia water to adjust pH (potential of hydrogen) to 9-10; performing backflow extraction by ethyl acetate; concentrating the extracting solution to be dry; finally performing separation and purification by high-speed counter-current chromatography; and drying effluence to obtain the verticillatine. In the method, the utilization quantity of toxic organic reagents is low, preparation quantity is high, loss of samples is low, and the content of products is high.

Description

technical field [0001] The invention belongs to the field of separation of natural products, and in particular relates to a method for extracting high-content vertixinlatine by high-speed countercurrent chromatography. Background technique [0002] Rauwolfia, derived from the plant Rauwolfia in the family Apocynaceae Rauvolfia verticillata (Lour.) Baill. and Yunnan Rauvolwolfia R. yunnanensis Tsiang, the root is used as medicine. Sexual bitterness, cold. It is slightly poisonous. It has the effects of calming down, lowering blood pressure, promoting blood circulation and relieving pain, clearing heat and detoxifying. It can be used for hypertension, headache, dizziness, insomnia, high fever and other diseases; external use can treat bruises, snake bites and other diseases. Red fruit Rauwolfia contains a variety of indole alkaloids. It is currently known that indole alkaloids are the main antihypertensive components of red fruit Rauwolfia. [0003] Vertesinlatine, an i...

Claims

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Application Information

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IPC IPC(8): C07D491/22
Inventor 刘东锋吴艳波
Owner NANJING ZELANG MEDICAL TECH
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