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Method for preparing brucea javanica picrol

A technology of brucepharoside and brucei, which is applied in the field of natural medicinal chemistry, can solve the problems of high production cost, complicated operation, small preparation amount, etc., and achieves the effects of low production cost and simple operation of the method.

Inactive Publication Date: 2013-12-04
NANJING ZELANG MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This type of method is complicated to operate, the preparation amount is small, the production cost is high, and it is difficult to industrialize production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Take 10 kg of defatted bruce chinensis raw material, add 10 times the amount of 70% methanol solution for 10 hours, extract 3 times, the extract is filtered and concentrated to no alcohol, the concentrated solution is diluted with an appropriate amount of water and then added to D101 macroporous resin for adsorption, first use 7 times The impurities were eluted with 20% ethanol solution by column volume, and the active ingredients were eluted with 5 times the column volume of 70% ethanol. The eluate was concentrated to a density of 1.05, extracted with ethyl acetate for 3 times, the extract was concentrated under reduced pressure, and an appropriate amount of concentrated solution was added. Dissolve in 30% ethanol solution, add it to AB-8 macroporous resin for adsorption, use 20 times the column volume of 50% ethanol solution to elute the impurities, and then use 20 times the column volume of 60% ethanol to elute, collect the eluate and concentrate under reduced pressure...

Embodiment 2

[0019] Take 10 kg of defatted bruceus raw material, add 5 times the amount of 90% methanol solution to soak for 10 hours, extract 3 times, the extract is filtered and concentrated to no alcohol, the concentrated solution is diluted with an appropriate amount of water, and then added to AB-8 macroporous resin for adsorption. 5 times the column volume of 30% ethanol solution to elute the impurities, and then use 10 times the column volume of 75% ethanol to elute the active ingredient, the eluent is concentrated to a density of 1.03, and ethyl acetate is added for extraction 3 times, the extract is concentrated under reduced pressure, and the concentrated solution Add an appropriate amount of 20% ethanol solution to dissolve, add it to AB-8 macroporous resin for adsorption, use 20 times the column volume of 50% ethanol solution to elute the impurities, and then use 20 times the column volume of 60% ethanol to elute, collect the eluate and concentrate under reduced pressure The cr...

Embodiment 3

[0021] Take 10kg of defatted Brucea javanica raw material, add 7 times the amount of 80% methanol solution to soak for 10 hours, extract 3 times, the extract is filtered and concentrated to no alcohol, the concentrate is diluted with an appropriate amount of water, and then added to HZ816 macroporous resin for adsorption, first use 7 times The impurities were eluted with 40% ethanol solution by column volume, and the active ingredients were eluted with 8 times the column volume of 70% ethanol. The eluate was concentrated to a density of 1.04, extracted with ethyl acetate for 3 times, the extract was concentrated under reduced pressure, and an appropriate amount of concentrated solution was added. Dissolved in 30% ethanol solution, added to HZ816 macroporous resin for adsorption, eluted impurities with 20 times the column volume of 50% ethanol solution, and then eluted with 20 times the column volume of 60% ethanol, collected the eluate and concentrated to anhydrous under reduced...

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PUM

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Abstract

The invention discloses a method for preparing brucea javanica picrol. The method for preparing the brucea javanica picrol includes the following steps that firstly, a degreased brucea javanica raw material is taken, soaked into a 70%-90% methanol solution with the volume which is 5-10 times the volume of the raw material for 10-20 hours and extracted for three times, the extracted liquid is filtered and concentrated, the concentrated liquid is filled with proper water, diluted and absorbed by macroporous resin and undergoes gradient elution with an ethanol solution, the eluted liquid is concentrated and extracted with ethyl acetate, the extracted liquid is decompressed and concentrated and the concentrated liquid is obtained; secondly, a 30%-50% ethanol solution is added into the concentrated liquid for dissolution and then, the concentrated liquid is added into the macroporous resin for being absorbed and a 50% ethanol solution with the column volume which is 20 times that of the concentrated liquid is used for eluting impurities. A 60% ethanol solution with the column volume which is 20 times that of the concentrated liquid is used for carrying out elution, and the eluted liquid is collected, decompressed and concentrated into anhydrous crystals. The crystals undergo recrystallization with ethyl acetate and are dried at a low temperature. The brucea javanica picrol produced with the method is simple in technological operation, low in production cost and easy to be produced in an industrialized mode.

Description

technical field [0001] The invention belongs to the field of natural medicine chemistry, and in particular relates to a preparation method of Brucea Brucea. Background technique [0002] Brucea Brucea, CAS No. 14907-98-3, molecular weight C26H32O11, molecular weight 520.528, molecular structure formula: [0003] [0004] Brucea brucea has anti-tumor and anti-amoeba activities. Brucelipidol is an effective inhibitory drug. It is a triterpenoid compound in Brucea javanica. It has been proved to have Nrf2 inhibitory effect and can cooperate with a variety of chemotherapy drugs to improve the cure rate of tumors. . [0005] Brucea javanica is the dry and mature fruit of the plant Bructus javanica in the family Bitterwoodaceae. In recent years, it has been reported that it has various biological activities such as anthelmintic, antimalarial, antiviral, and antitumor. The main components of Brucea javanica are Brucea brucein A, B, C, D, E, F, G, H, I, Bruceolide, Brusatol; i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D493/10
Inventor 刘东锋万冬梅
Owner NANJING ZELANG MEDICAL TECH
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