CN102432432A - Preparation method of cordycepic acid - Google Patents
Preparation method of cordycepic acid Download PDFInfo
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- CN102432432A CN102432432A CN2010102962559A CN201010296255A CN102432432A CN 102432432 A CN102432432 A CN 102432432A CN 2010102962559 A CN2010102962559 A CN 2010102962559A CN 201010296255 A CN201010296255 A CN 201010296255A CN 102432432 A CN102432432 A CN 102432432A
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Abstract
The invention relates to a preparation method of cordycepic acid. The method comprises technical steps that: cordyceps sinensis is adopted as a raw material; the raw material is extracted 2-3 times by using 15-20 times of deionized water by volume weight (V/W); impurities in the extraction liquid are removed by using an ultrafiltration nano-filtration membrane system; an obtained filtrate is heated and condensed; when a relative density of the filtrate is 1.30-1.32, the filtrate is settled for crystallization; obtained coarse crystals are recrystallized by using absolute ethanol 2-3 times; and the obtained crystals are dried by baking, such that a product is obtained. The method provided by the invention is advantaged in simple operation, relatively low cost, and relatively high purity. With the method, circular economy is realized, such that the method is characterized by low carbon, and environment friendliness.
Description
Technical field
The present invention relates to a kind of preparation method of cordycepic acid, especially a kind of method with membrane separation technique purifying cordycepic acid.
Background technology
Cordycepic acid is claimed D-N.F,USP MANNITOL again
English name: Mannitol
Molecular formula: C
6H
14O
6
Molecular weight: 182.17
Cordycepic acid is not the distinctive material of Chinese caterpillar fungus, has diuresis, gets rid of toxin, and function such as enhance metabolism clinically is used to treat cerebral thrombosis, cerebral embolism, vasospasm, renal failure.Caizhong armies etc. explain that " different places of production entomophyte mannitol content relatively " cordycepic acid content is main relevant with its place of production in the Chinese caterpillar fungus; Chinese caterpillar fungus sample through to 24 different places of production is analyzed; Find cordycepic acid content at 2.87-16.71%, content differs greatly between visible each sample.The employed raw material of this technology originates from Qinghai, the about 8-12% of cordycepic acid content.
In the prior art, cordycepic acid can be synthetic with chemical synthesis, but have a lot of problems: glucose electrolytic process efficient is low, and energy consumption is big, and purity is low; The reduction method product of polyose has the isomery problem, cost height and purity is low; Seminose reduction method raw material sources are a problem etc.Extraction method is raw material with the sea-tangle mainly, and products obtained therefrom is of poor quality, filtration is difficult, and production cost is high, need be further purified.Be that the method extracted of raw material is also few with entomophyte; Disclosed the technology of continuously extracting cordyceps volatile oil, cordycepin, cordycepic acid and Cordyceps polysaccharide " a kind of from Cordyceps militaris (L.) Link. " extracts the multiple product that comprises cordycepic acid with supercritical fluid technology, but processing unit is had relatively high expectations.
Summary of the invention
Technical problem to be solved by this invention provides a kind of simple to operate, and cost is lower, the cordycepic acid preparation method that purity is higher.
For solving the problems of the technologies described above, the present invention adopts following technical proposal:
1) water is carried: get raw material, add deionized water heating and extracting 2-3 time that 15-20 doubly measures (V/W), united extraction liquid must extracting solution;
2) membrane sepn: said extracted liquid sees through liquid again through the further removal of impurities of nf membrane system through ultrafiltration membrane system, nanofiltration night;
3) condensing crystal: when nanofiltration liquid heating is concentrated into specific density and is 1.30-1.32, leave standstill and let alone crystallisation by cooling, coarse crystallization;
4) refining: as coarse crystallization to be dissolved in the absolute ethyl alcohol recrystallization 2-3 time, to dry and promptly get product.
Above-mentioned preparation method is characterized in that raw material is that entomophyte is produced in Qinghai in the said step 1).
Above-mentioned preparation method is characterized in that Heating temperature is 75-80 ℃ in the said step 1), and each extraction time is 1.5-2 hour.
Above-mentioned preparation method is characterized in that said step 2) in ultrafiltration membrane system be the hollow fiber ultrafiltration membrane system of molecular weight cut-off 20000, nf membrane is a HNF-70-4040 type nf membrane.
Above-mentioned preparation method is characterized in that the 2-3 that the each crystal anhydrous amount of ethanol of said step 3) is a coarse crystallization doubly measures (V/W).
In sum, there is following advantage in the present invention:
1, this process using extraction method prepares cordycepic acid, and problems such as isomerizing impurity in the no synthesis method or catalysts are simple to operate;
2, raw material adopts Qinghai to produce entomophyte, and content is high, the simple low-carbon (LC) of production process;
3, the fenestra of nf membrane only allows molecular weight 200 to pass through with interior small molecules; It is linear that cordycepic acid is; Basically can not lose, stop up the nanofiltration fenestra, adopt the ultra-filtration membrane pre-treatment for preventing big impurity because of removal of impurities; Except that performance, also has good decolorizing effect with tangible filtering colloidal impurity;
4, consumption of organic solvent is few, and toxicity is low, and environmental protection is produced safer.
To combine embodiment that the present invention is done further elaboration below, but the scope that the present invention requires to protect is not limited to following embodiment.
Embodiment
Embodiment 1
Get Qinghai and produce entomophyte 100g, add the 1.5L deionized water, 75 ℃ are extracted united extraction liquid 1.5 hours 2 times.Extracting solution is through the hollow fiber ultrafiltration membrane system decolouring of molecular weight cut-off 20000, and the removal of impurities of HNF-70-4040 type nf membrane is collected and seen through liquid.See through the liquid heating and be concentrated into specific density 1.30-1.32, leave standstill crystallisation by cooling, get coarse crystallization 12g.Coarse crystallization adds the 25ml absolute ethyl alcohol, recrystallization 2 times, and oven dry promptly gets cordycepic acid 7.8g, detects through HPLC, and purity is 98.5%.
Embodiment 2
Get Qinghai and produce entomophyte 100g, add the 1.6L deionized water, 80 ℃ are extracted united extraction liquid 1.5 hours 3 times.Extracting solution is through the hollow fiber ultrafiltration membrane system decolouring of molecular weight cut-off 20000, and the removal of impurities of HNF-70-4040 type nf membrane is collected and seen through liquid.See through the liquid heating and be concentrated into specific density 1.30-1.32, leave standstill crystallisation by cooling, get coarse crystallization 14g.Coarse crystallization adds the 30ml absolute ethyl alcohol, recrystallization 2 times, and oven dry promptly gets cordycepic acid 8.9g, detects through HPLC, and purity is 98.6%.
Embodiment 3
Get Qinghai and produce entomophyte 100g, add the 1.8L deionized water, 75 ℃ are extracted united extraction liquid 2 hours 2 times.Extracting solution is through the hollow fiber ultrafiltration membrane system decolouring of molecular weight cut-off 20000, and the removal of impurities of HNF-70-4040 type nf membrane is collected and seen through liquid.See through the liquid heating and be concentrated into specific density 1.30-1.32, leave standstill crystallisation by cooling, get coarse crystallization 13g.Coarse crystallization adds the 35ml absolute ethyl alcohol, recrystallization 2 times, and oven dry promptly gets cordycepic acid 9.8g, detects through HPLC, and purity is 99.2%.
Embodiment 4
Get Qinghai and produce entomophyte 100g, add the 2L deionized water, 80 ℃ are extracted 2 hours 3 times, get extracting solution.Extracting solution is through the hollow fiber ultrafiltration membrane system decolouring of molecular weight cut-off 20000, and the removal of impurities of HNF-70-4040 type nf membrane is collected and seen through liquid.See through the liquid heating and be concentrated into specific density 1.30-1.32, leave standstill crystallisation by cooling, get coarse crystallization 14g.Coarse crystallization adds the 40ml absolute ethyl alcohol, recrystallization 2 times, and oven dry promptly gets cordycepic acid 9.4g, detects through HPLC, and purity is 99.5%.
Claims (5)
1. the preparation method of a cordycepic acid is characterized in that comprising following steps:
1) water is carried: get raw material, add deionized water heating and extracting 2-3 time that 15-20 doubly measures (V/W), united extraction liquid must extracting solution;
2) membrane sepn: said extracted liquid sees through liquid again through the further removal of impurities of nf membrane system through ultrafiltration membrane system, nanofiltration night;
3) condensing crystal: when nanofiltration liquid heating is concentrated into specific density and is 1.30-1.32, leave standstill and let alone crystallisation by cooling, coarse crystallization;
4) refining: as coarse crystallization to be dissolved in the absolute ethyl alcohol recrystallization 2-3 time, to dry and promptly get product.
2. preparation method as claimed in claim 1 is characterized in that raw material is that entomophyte is produced in Qinghai in the said step 1).
3. preparation method as claimed in claim 1 is characterized in that Heating temperature is 75-80 ℃ in the said step 1), and each extraction time is 1.5-2 hour.
4. preparation method as claimed in claim 1 is characterized in that said step 2) in ultrafiltration membrane system be the hollow fiber ultrafiltration membrane system of molecular weight cut-off 20000, nf membrane is a HNF-70-4040 type nf membrane.
5. preparation method as claimed in claim 1 is characterized in that the 2-3 that the each crystal anhydrous amount of ethanol of said step 3) is a coarse crystallization doubly measures (V/W).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010102962559A CN102432432A (en) | 2010-09-29 | 2010-09-29 | Preparation method of cordycepic acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010102962559A CN102432432A (en) | 2010-09-29 | 2010-09-29 | Preparation method of cordycepic acid |
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| CN102432432A true CN102432432A (en) | 2012-05-02 |
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| CN2010102962559A Pending CN102432432A (en) | 2010-09-29 | 2010-09-29 | Preparation method of cordycepic acid |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105341895A (en) * | 2015-09-29 | 2016-02-24 | 上海市农业科学院 | Preparation method of high-purity trehalose |
| CN109265318A (en) * | 2018-11-12 | 2019-01-25 | 湖北葛店人福药用辅料有限责任公司 | A kind of preparation method of sorbierite |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101811934A (en) * | 2010-04-08 | 2010-08-25 | 苏州宝泽堂医药科技有限公司 | Preparation method of mannitol |
-
2010
- 2010-09-29 CN CN2010102962559A patent/CN102432432A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101811934A (en) * | 2010-04-08 | 2010-08-25 | 苏州宝泽堂医药科技有限公司 | Preparation method of mannitol |
Non-Patent Citations (4)
| Title |
|---|
| KUK HYUN SHIN等: "Anti-tumour and Immuno-stimulating Activities of The Fruiting Bodies of Paecilomyces japonica, a New Type of Cordyceps spp.", 《PHYTOTHERAPY RESEARCH》 * |
| 周日尤等: "甘露醇制取的提取法与合成法比较", 《广西轻工业》 * |
| 夏仙兵等: "海带工业中甘露醇的纳滤膜渗滤纯化研究-工艺参数对纳滤提取甘露醇的影响", 《海洋技术》 * |
| 蔡仲军等: "水提取法测定冬虫夏草甘露醇含量", 《重庆教育学院学报》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105341895A (en) * | 2015-09-29 | 2016-02-24 | 上海市农业科学院 | Preparation method of high-purity trehalose |
| CN109265318A (en) * | 2018-11-12 | 2019-01-25 | 湖北葛店人福药用辅料有限责任公司 | A kind of preparation method of sorbierite |
| CN109265318B (en) * | 2018-11-12 | 2021-10-01 | 湖北葛店人福药用辅料有限责任公司 | Preparation method of sorbitol |
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Application publication date: 20120502 |