Method for separating evodiamine and rutaecarpin from fructus evodiae

A technology of evodiamine and evodiamine, which is applied in the direction of organic chemistry, can solve the problems of not doing separation and purification process, and achieve the effect of easy operation, simple production process and low cost

Active Publication Date: 2018-08-07
NANCHANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In the literature or patents, there have been many reports on methods for preparing and synthesizing evodiamine and rutadiamine, such as the Chinese patent "Application No. 200810046164.2", which uses column chromatography and efficient liquid phase separation to prepare evodiamine and rutadiam

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] (1) Take an appropriate amount of dried and pulverized traditional Chinese medicine Evodia rutaecarpa powder, add 1 times the amount of 75% ethanol and ultrasonically (400W, 20°C) stir and extract 3 times, each time for 2h, combine the extracts and recover the solvent to obtain the extract.

[0021] (2) Degrease the above extract with 10 times the amount of petroleum ether for 3 times. Then soak and wash with 10 times the amount of 1% hydrochloric acid solution for 1 hour, filter, take the solid, and repeat 3 times.

[0022] (3) Soak the above solid in 10 times the amount of 20% sodium hydroxide solution, react for 1 h, filter, take the residual solid and add 10% hydrochloric acid for 1 h, filter to obtain a solid.

[0023] (4) Dissolve the solid with 10 times the amount of chloroform, filter, take the liquid and the solid, adjust the reaction with 10 times the amount of 10% sodium hydroxide and the solution for 1 hour, filter, wash, and take the solid, The crude produ...

Embodiment 2

[0026] (1) Take an appropriate amount of Evodia rutaecarpa, add 4 times the amount of absolute ethanol, stir, reflux at 60°C for 5 times, 1 hour each time, combine the extracts and recover the solvent to obtain the extract.

[0027] (2) Degrease the above extract five times with 1 times the amount of n-hexane. Then soak and wash with 100 times the amount of 2% sulfuric acid solution for 1 hour, filter, and take the solid, and repeat this operation 3 times.

[0028] (3) Soak the above solid in 20 times the amount of 1% potassium hydroxide solution, react for 1 h, filter, take the residual solid and add sulfuric acid to adjust the reaction for 48 h, filter to obtain a solid.

[0029] (4) Dissolve the above-mentioned solid with 10% acetone, filter, take the liquid and the solid two parts, adjust the reaction with 10 times the amount of 30% potassium hydroxide solution for 1 h, centrifuge, wash, take the solid, and get the crude product of evodiamine and Evodia rutaecarpine crude...

Embodiment 3

[0032] (1) Take an appropriate amount of dry powder of Chinese medicine Evodia rutaecarpa, add 15 times the amount of 75% methanol and ultrasonically (300W, 20°C) stir and extract 4 times, each time for 1h, combine the extracts and recover the solvent to obtain the extract.

[0033] (2) Degrease the above extract with 20 times the amount of cyclohexane 5 times. Then soak and wash with 30 times the amount of 10% hydrochloric acid solution for 10 h, filter, take the solid, and repeat 3 times.

[0034] (3) The above-mentioned washed solid was added to 20 times the amount of 1% ammonia solution, fully dissolved for 10 h, filtered, and the residual solid was added with sulfuric acid to adjust the reaction for 1 h, centrifuged to obtain a solid.

[0035] (4) Dissolve the above solid with 30 times the amount of dichloromethane, filter, take the liquid and solid two parts, adjust the reaction with 10 times the amount of 1% ammonia solution for 6 hours, filter, wash, and take the solid...

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PUM

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Abstract

The invention relates to a method for separating evodiamine and rutaecarpin from fructus evodiae. The method provided by the invention takes fructus evodiae as a raw material. The method for preparingthe evodiamine and rutaecarpin comprises the following steps: taking the raw material, adding a certain amount of solvent, extracting, and recycling the solvent, so that fructus evodiae extract is obtained; degreasing the extract with a low polarity solvent and a mixture, and then washing with diluted hydrochloric acid or sulfuric acid, nitric acid or phosphoric acid solution; taking residual solids, namely obtaining the residual solids by filtering or centrifuging; carrying out adjustment reaction on the residual solids, and filtering or centrifuging; dissolving the solids with dichloromethane, chloroform, acetone or ethyl acetate again, filtering or centrifuging, obtaining two parts, namely solids and a liquid, taking the solid and liquid parts, reacting respectively, obtaining a evodiamine crude product and a rutaecarpin crude product, and then carrying out crystallization and recrystallization so as to finally obtain high-purity evodiamine and rutaecarpin crystals.

Description

technical field [0001] The invention mainly relates to a method for large-scale preparation of evodiamine and evodiamine from evodia rutaecarpa, and belongs to the field of extraction and separation of traditional Chinese medicines. Background technique [0002] Evodiamine and Rutaecarpa are mainly found in the seeds or fruits of Rutaceae (Rutaceae), such as the fruits of Evodiamine, the fruit of Shihu, and the fruits of Evodia spp. content of evodiamine and evodiamine. Pharmacological studies have shown that evodiamine and evodiamine have strong physiological activities, such as anti-oxidation, anti-inflammatory, anti-fungal, analgesic, anti-tumor, anti-viral and other activities. So evodiamine and evodiamine are a class of active ingredients with very high development value. [0003] The invention proposes a new method for efficiently separating and purifying evodiamine and evodiamine. The raw materials used in the method are widely available and easy to obtain, the prep...

Claims

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Application Information

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IPC IPC(8): C07D471/14
CPCC07D471/14
Inventor 范杰平郑兵
Owner NANCHANG UNIV
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