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Industrial production technology for separating rhaponiticin and deoxidized rhaponiticin simultaneously

A technology of deoxyreveredin and rhubarb, which is applied in the field of medicine, can solve the problems of not being able to meet the needs of new drug research and production, not getting deoxyreverin, and prone to safety accidents, so as to ensure health and safety, The effect of low cost and non-toxic solvent

Active Publication Date: 2016-02-17
北京九龙制药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, the patent application number is 201210139975.3, and the title of the invention is "A Method for Rapidly Preparing High-Purity Rhizomatrin and Deoxygenerin". Due to the limitation of equipment and technology, only a few hundred milligrams of samples can be prepared each time. Far from meeting the needs of new drug research and production
Among them, the patent application number is 201110212533.2, and the title of the invention is "The method of extracting rhubarb from Hetao rhubarb". Prepared a compound of rhubarb, but did not get deoxyrhein, resulting in a waste of resources
Among them, the patent application number is 201210166053.1, and the title of the invention is "A Method for High Efficiency and Accurate Separation and Purification of Deoxyrhein". Since it needs to be purified by macroporous resin twice, the process is lengthy, and only one compound, did not get rhizoma glycosides, and also caused a waste of resources

Method used

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  • Industrial production technology for separating rhaponiticin and deoxidized rhaponiticin simultaneously
  • Industrial production technology for separating rhaponiticin and deoxidized rhaponiticin simultaneously
  • Industrial production technology for separating rhaponiticin and deoxidized rhaponiticin simultaneously

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0070] Crush 200 kg of Hetao rhubarb into 40 meshes, add 1,600 kg of 75% alcohol, stir and extract at room temperature for 2 hours, extract once more according to the above method, combine the extracts, concentrate under reduced pressure below 60°C until alcohol-free, add 1,000 kg of water And filtered, adsorbed on the treated polyamide chromatography column, washed with water to remove large polar impurities, then eluted with 30% alcohol for twice the column volume, and then eluted with 50% alcohol until the target molecule was completely eluted, First collect the eluate of ethanol, then collect the eluate of deoxyreveridin, concentrate under reduced pressure below 60°C until just crystallization, cool to room temperature and separate by centrifuge, dry in a hot air oven below 50°C, 15.6 kg of crude product of rhubarb was obtained, with a content of 94.8%, and 3.1 kg of crude product of deoxyrhein, with a content of 96.2%. Put the two kinds of crude products into the reaction...

Embodiment 2

[0072] Crush 200 kg of rhubarb into 80 meshes, add 1800 kg of 60% alcohol, stir and reflux for extraction for 1.5 hours, extract once more according to the above method, combine the extracts, concentrate under reduced pressure below 60°C until there is no alcohol smell, add 1000 kg of water And filtered, adsorbed on the treated polyamide chromatography column, washed with water to remove large polar impurities, then eluted with 20% alcohol for three times the column volume, and then eluted with 60% alcohol until the target molecule was completely eluted, First collect the eluate of ethanol, then collect the eluate of deoxyreveridin, concentrate under reduced pressure below 60°C until just crystallization, cool to room temperature and separate by centrifuge, dry in a hot air oven below 50°C, 14.8 kg of the crude product of rhubarb was obtained, with a content of 95.2%, and 3.8 kg of crude product of deoxyrhubarb, with a content of 95.8%. Put the two crude products into the reac...

Embodiment 3

[0074] Crush 200 kg of Rhubarb Rhubarb into 60 meshes, add 2000 kg of 50% alcohol, stir and reflux for extraction for 1 hour, extract once more according to the above method, combine the extracts, concentrate under reduced pressure below 60°C until alcohol-free, add 1000 kg of water and filtered, adsorbed on the treated polyamide chromatography column, washed with water to remove large polar impurities, then eluted with 40% alcohol for 1.5 times the column volume, and then eluted with 55% alcohol until the target molecule was completely eluted Next, first collect the eluate of ethanol, then collect the eluate of deoxyreverin, respectively concentrate under reduced pressure below 60°C until just crystallization, cool to room temperature and centrifuge to separate, store in a hot air oven below 50°C After drying, 15.3 kg of the crude product of rhubarb was obtained, with a content of 94.1%, and 6.3 kg of crude product of deoxyrhein, with a content of 96.6%. Put the two kinds of ...

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Abstract

The invention relates to an industrial production technology for separating rhaponiticin and deoxidized rhaponiticin simultaneously. A method of the technology comprises the following steps of pulverizing the rhaponiticin, conducting reflux extraction twice with ethyl alcohol with the concentration being 70%, combining extracting solutions, conducting concentration till no ethyl alcohol smell exists, conducting adsorption with a polyamide chromatographic column, washing away large-polarity water soluble impurities with water, then conducting gradient elution with ethyl alcohol, collecting rhaponiticin eluant and deoxidized rhaponiticin eluant separately, conducting concentration till crystals are separated out, conducting filteration and drying, then conducting recrystallization with ethyl alcohol, and obtaining the rhaponiticin with the content being greater than or equal to 98.55 and the deoxidized rhaponiticin with the content being greater than or equal to 98.5%.

Description

technical field [0001] The invention belongs to the field of medicine, and relates to an industrialized production technology capable of simultaneously separating rhubarb and deoxyrhein. Background technique [0002] The molecular structural formula of terraein is as follows: [0003] [0004] CAS: 155-58-8Molecular formula: C21H24O9 [0005] The molecular structural formula of deoxyreveredin is as follows: [0006] [0007] CAS: 30197-14-9Molecular formula: C21H24O8 [0008] Rhubarb is the dry root and rhizome of rhubarb palmatum, rhubarb tangutica or medicinal rhubarb of the Polygonaceae plant. It is a traditional Chinese medicine in my country and has been used for thousands of years. It contains a large amount of anthraquinone compounds, which have the effect of purging It is stipulated in the "Chinese Pharmacopoeia" that rhubarb should not be detected, but research results at home and abroad have shown that stilbene glycosides such as rhubarb and deoxyrhubarb ha...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H15/203C07H1/08
CPCC07H1/08C07H15/203
Inventor 杨喜峰
Owner 北京九龙制药有限公司
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