CN101704787A - Method for preparing allantoin - Google Patents
Method for preparing allantoin Download PDFInfo
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- CN101704787A CN101704787A CN200910233831A CN200910233831A CN101704787A CN 101704787 A CN101704787 A CN 101704787A CN 200910233831 A CN200910233831 A CN 200910233831A CN 200910233831 A CN200910233831 A CN 200910233831A CN 101704787 A CN101704787 A CN 101704787A
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- percolate
- hot water
- wallantoin
- ethanol
- filter
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Abstract
The invention relates to a method for preparing allantoin, which has the advantages of simple operation, light pollution and less equipment investment. The method comprises the following process steps: taking crude powder of dutchmanspipe root, and adding 60 to 90 percent ethanol for percolation; collecting a percolate which is 5 to 10 times of medicinal materials in volume, filtering the percolate, recovering the ethanol at reduced pressure, then concentrating the percolate, and standing overnight; filtering, and taking filter residues; adding hot water to dissolve the filter residues, filtering, and then refrigerating the filtrate; and separating out crystals, separating the crystals, adding the hot water into the crystals to recrystallize, separating, washing and drying the crystals to obtain the allantoin. The allantoin prepared by the method has high purity; and the industrial amplification is easy to implement.
Description
Technical field
The present invention relates to a kind of preparation method of wallantoin, especially a kind of method of from plant, extracting wallantoin.
Background technology
Wallantoin (Allantoin), different name: Dermalex, Cordianin, Actinac, Alphosyl etc.Molecular formula: C
4H
6N
4O
3, molecular weight: 158.116, CAS accession number: 97-59-6, structural formula is as follows:
Wallantoin is a kind of natural compounds, has multiple physiologically actives such as anti-inflammatory, psoriasis, promotion wound healing, extensively is present in the various plants such as Virginia snakeroot.
The Chinese medicine Slender Dutchmanspipe Root is the dry root of aristolochiaceae plant Virginia snakeroot Aristolochia debilis Sieb.et zucc., has Pingyang pain relieving, and the effect of detoxify and promote the subsdence of swelling wherein contains a large amount of wallantoins.
In the prior art, the extraction separation of wallantoin mainly adopts organic solvent method etc., but the content of the wallantoin that these extraction processes obtain is low, and is seriously polluted in the production process, and unfavorable big production operation.
Summary of the invention
Technical problem to be solved by this invention provides a kind of preparation method who is beneficial to big production operation, wallantoin that product purity is high.
For solving the problems of the technologies described above, the present invention adopts following technical proposal:
Get the Slender Dutchmanspipe Root meal, add the 60-90% ethanol percolation, collect the percolate that medicinal material weight 5-10 doubly measures volume, filter, decompression recycling ethanol also concentrates, and placement is spent the night, filter, get filter residue, add the hot water dissolving, filter, filtrate refrigeration is separated out crystallization, fractional crystallization, add the hot water recrystallization, separate, wash, be drying to obtain.
Diacolation is preferably 80% with concentration of ethanol.
The amount of collecting percolate is preferably 8 times of amounts of medicinal material weight volume.
Adopt technique scheme to prepare wallantoin, easy and simple to handle, pollute less, equipment drops into for a short time, is beneficial to big production operation.
Below in conjunction with embodiment the present invention is further elaborated, but the scope of protection of present invention is not limited to following embodiment.
Embodiment
Embodiment 1
Get Slender Dutchmanspipe Root meal 10Kg, add 60% ethanol percolation, collect the percolate of 10 times of amounts of medicinal material weight volume, filter, decompression recycling ethanol also concentrates, and placement is spent the night, filter, get filter residue, add the hot water dissolving, filter, crystallization is separated out in filtrate refrigeration, fractional crystallization, add the hot water recrystallization, separate, wash, be drying to obtain wallantoin 9.2g, detecting purity through HPLC is 98.3%.
Embodiment 2
Get Slender Dutchmanspipe Root meal 10Kg, add 90% ethanol percolation, collect the percolate of 10 times of amounts of medicinal material weight volume, filter, decompression recycling ethanol also concentrates, and placement is spent the night, filter, get filter residue, add the hot water dissolving, filter, crystallization is separated out in filtrate refrigeration, fractional crystallization, add the hot water recrystallization, separate, wash, be drying to obtain wallantoin 10.6g, detecting purity through HPLC is 98.0%.
Embodiment 3
Get Slender Dutchmanspipe Root meal 10Kg, add 80% ethanol percolation, collect the percolate of 8 times of amounts of medicinal material weight volume, filter, decompression recycling ethanol also concentrates, and placement is spent the night, filter, get filter residue, add the hot water dissolving, filter, crystallization is separated out in filtrate refrigeration, fractional crystallization, add the hot water recrystallization, separate, wash, be drying to obtain wallantoin 10.2g, detecting purity through HPLC is 99.6%.
Claims (3)
1. the preparation method of a wallantoin is characterized in that described method comprises the following steps: to get the Slender Dutchmanspipe Root meal, adds the 60-90% ethanol percolation, collect the percolate that medicinal material weight 5-10 doubly measures volume, filter, decompression recycling ethanol also concentrates, placement is spent the night, and filters, and gets filter residue, add the hot water dissolving, filter, filtrate refrigeration, separate out crystallization, fractional crystallization adds the hot water recrystallization, separates, washs, is drying to obtain.
2. according to the preparation method of the described wallantoin of claim 1, it is characterized in that described diacolation concentration of ethanol is 80%.
3. according to the preparation method of the described wallantoin of claim 1, the amount that it is characterized in that described collection percolate is 8 times of amounts of medicinal material weight volume.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
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CN200910233831A CN101704787A (en) | 2009-10-22 | 2009-10-22 | Method for preparing allantoin |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
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CN200910233831A CN101704787A (en) | 2009-10-22 | 2009-10-22 | Method for preparing allantoin |
Publications (1)
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CN101704787A true CN101704787A (en) | 2010-05-12 |
Family
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Family Applications (1)
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CN200910233831A Pending CN101704787A (en) | 2009-10-22 | 2009-10-22 | Method for preparing allantoin |
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CN (1) | CN101704787A (en) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102020611A (en) * | 2010-12-20 | 2011-04-20 | 青海青美生物资源研究开发有限公司 | Method for preparing allantoin from nitraria core residue |
CN106083725A (en) * | 2016-06-12 | 2016-11-09 | 北京梅尔森医药技术开发有限公司 | A kind of preparation method of high-purity allantoin |
-
2009
- 2009-10-22 CN CN200910233831A patent/CN101704787A/en active Pending
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102020611A (en) * | 2010-12-20 | 2011-04-20 | 青海青美生物资源研究开发有限公司 | Method for preparing allantoin from nitraria core residue |
CN102020611B (en) * | 2010-12-20 | 2012-09-12 | 青海青美生物资源研究开发有限公司 | Method for preparing allantoin from nitraria core residue |
CN106083725A (en) * | 2016-06-12 | 2016-11-09 | 北京梅尔森医药技术开发有限公司 | A kind of preparation method of high-purity allantoin |
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PB01 | Publication | ||
C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20100512 |