Method for preparing celastrine

A technology of shertenin and ultrasound, which is applied in the field of preparation of shertenin from plants, can solve the problems of no disclosure of the industrial production process of shertenin, and achieve the benefits of large-scale production operations, low energy consumption, The effect of little pollution

Inactive Publication Date: 2010-09-15
SUZHOU PAITENG BIOLOGICAL MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In the prior art, there is no disclosure o

Method used

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  • Method for preparing celastrine

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Experimental program
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Example Embodiment

[0016] Example 1

[0017] Take the keratin root bark of Euonymus plant, crush it, add methanol 4 times its mass and volume, put it into an ultrasonic extraction device for ultrasonic extraction once, each time for 0.2 hours, the extraction power is 30KHZ, combine the extracts, filter, reduce Recover methanol under pressure, dissolve the residue by adding 0.05mol / L NaOH aqueous solution, filter, adjust the pH value of the filtrate to 3 with dilute hydrochloric acid solution, let it stand, filter, take the filter residue, add it to the alumina chromatography column, and use volume Elute with methanol-chloroform mixed solvent with a ratio of 3:1, collect 2 times the column volume of the eluate, recover the solvent under reduced pressure and concentrate, add ethanol-n-hexane mixed solvent with a volume ratio of 1:1 for crystallization, and separate the crystallization That is, 5.2 g of shertenin was obtained, and the purity was 98.0% as detected by HPLC.

Example Embodiment

[0018] Example 2

[0019] Take 10Kg of Euonymus plant kerosene root bark, crush it, add methanol with 5 times the volume of its mass, put it into an ultrasonic extraction device for ultrasonic extraction 3 times, each time for 1 hour, the extraction power is 60KHZ, combine the extracts, filter, Recover methanol under reduced pressure, add 0.15mol / L NaOH aqueous solution to the residue to dissolve, filter, adjust the pH value of the filtrate to 5 with dilute hydrochloric acid solution, let it stand, filter, take the filter residue, add it to the alumina chromatography column, use The methanol-chloroform mixed solvent with a volume ratio of 3:1 was eluted, and 4 times the volume of the column volume was collected. Crystallization yielded 9.2 g of shertenin, which was detected by HPLC with a purity of 96.6%.

Example Embodiment

[0020] Example 3

[0021] Take 10Kg of Euonymus plant kerosene root bark, crush it, add methanol with 3 times the volume of its mass, put it into an ultrasonic extraction device for ultrasonic extraction twice, each time for 0.5 hours, the extraction power is 50KHZ, combine the extracts, filter, Recover methanol under reduced pressure, add 1mol / L NaOH aqueous solution to the residue to dissolve, filter, adjust the pH value of the filtrate to 4 with dilute hydrochloric acid solution, let it stand, filter, take the filter residue, add it to an alumina chromatography column, and use volume Elute with a mixed solvent of methanol-chloroform with a ratio of 3:1, collect 3 times the column volume of the eluate, recover the solvent under reduced pressure and concentrate, add a mixed solvent of ethanol-n-hexane with a volume ratio of 1:1 for crystallization, and separate the crystals That is, 8.8 g of shertenin was obtained, and the purity was 98.9% as detected by HPLC.

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Abstract

The invention relates to a method for preparing celastrine with simple and convenient operation, low pollution and low energy consumption. The method comprises the following steps of: taking celastraceae plant celastrus paniculatus root bark, crushing the root bark, adding methanol in an amount which is 4 to 5 times the volume of the root bark into the crushed root bark, putting the mixture into an ultrasonic extraction device to perform ultrasonic extraction for 1 to 3 times for 0.2 to 1 hour each time with the extraction power of 30 to 60KHZ, combining the extract, filtering the extract, reclaiming the methanol under reduced pressure, adding 0.05 to 0.15 mol/L alkali aqueous solution into the residue to dissolve the residue, filtering the solution, adjusting the pH value of the filtrate to between 3 and 5 by using diluted hydrochloric acid solution, standing and filtering the solution, taking the filter residue, adding the filer residue into an aluminum oxide chromatographic column, eluting the filter residue by using a methanol-chloroform mixed solvent in a volume ratio of 3 to 1, collecting eluent in an amount which is 2 to 4 times volume of the aluminum oxide chromatographic column, reclaiming the solvent under reduced pressure, concentrating the eluent, adding the concentrate into an ethanol-n-hexane mixed solvent in a volume ratio of 1 to 1 to perform crystallization, and separating the crystal to obtain the celastrine. The celastrine prepared by adopting the method has high purity, and is easy to realize industrialized amplification.

Description

technical field [0001] The invention relates to a preparation method of shertenin, in particular to a preparation method of extracting shertenin from plants. Background technique [0002] Celastrol, molecular formula: C29H3804, molecular weight: 450.617, CAS registration number: 34157-83-0, mainly exists in a variety of plants, among which the content in the root bark of Celastrus paniculatus Willd. most abundant. Its molecular formula is as follows: [0003] [0004] Modern studies have shown that cerelin has various pharmacological activities such as cytotoxicity, immunosuppression, anti-inflammation, and hypnosis. [0005] In the prior art, there is no disclosure of the industrial production process of cerelin. Contents of the invention [0006] The technical problem to be solved by the present invention is to provide a preparation method of shertenin which is beneficial to large-scale production operation and has high product purity. [0007] In order to solve t...

Claims

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Application Information

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IPC IPC(8): C07J63/00
Inventor 王峰王琳张发成
Owner SUZHOU PAITENG BIOLOGICAL MEDICAL TECH
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