CN103601812B - Utilize the method that macroporous adsorbent resin extracts cordycepin and Cordyceps polysaccharide from Cordyceps militaris (L.) Link. - Google Patents
Utilize the method that macroporous adsorbent resin extracts cordycepin and Cordyceps polysaccharide from Cordyceps militaris (L.) Link. Download PDFInfo
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- CN103601812B CN103601812B CN201310592568.2A CN201310592568A CN103601812B CN 103601812 B CN103601812 B CN 103601812B CN 201310592568 A CN201310592568 A CN 201310592568A CN 103601812 B CN103601812 B CN 103601812B
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Abstract
The present invention relates to a kind of method utilizing macroporous adsorbent resin to extract cordycepin and Cordyceps polysaccharide from Cordyceps militaris (L.) Link., including Cordyceps militaris (L.) Link.sporophore being pulverized, using water extraction, extracting solution is concentrated, it is subsequently adding ethanol stand precipitation Cordyceps polysaccharide and obtain supernatant, supernatant is crossed macroporous adsorptive resins and obtains eluent, eluent concentrate drying is obtained cordycepin extractum.The inventive method products obtained therefrom hazardous solvent residual is few, and the method step is simple, and low cost can realize industrialized production.
Description
Technical field
The invention belongs to the field of deep of edible medicinal fungi, be specifically related to a kind of extraction cordycepin and method of Cordyceps polysaccharide from Cordyceps militaris (L.) Link..
Background technology
Cordycepin content in wild cordyceps is atomic, and the cordycepin of present institute generally individually extracts from Cordyceps militaris (L.) Link..There are antiviral, antitumor action.Cordycepin, as a kind of novel broad-spectrum antibiotic, with its distinctive antimicrobial antiviral activity, has caused the great attention of whole world science and technology developed country.It can suppress DNA and RNA of tumor cell to synthesize；Bacillus subtilis and mycobacterium tuberculosis avium all there is inhibitory action；HIV-I type virus also there is lethal effect；Especially multiple solid malignant there is the strongest inhibitory action.Therefore, developing as a kind of broad-spectrum new drug is inexorable trend.
The method extracting cordycepin has macroporous resin extraction method, supercritical methanol technology, anion-cation exchange resin extraction method etc..But supercritical methanol technology is huge for the investment of equipment, cation and anion exchange method needs to regulate pH value with HCl and ammonia etc., easily remains, is unfavorable for food safety, and yield is the lowest simultaneously；It addition, existing method synthesis steps is complicated, cost is high, raw material causes the biggest waste, it is impossible to for industrialized production.
Summary of the invention
It is an object of the invention to provide a kind of step simple, low cost, industrialized production can be realized, without extraction cordycepin and the method for Cordyceps polysaccharide from Cordyceps militaris (L.) Link. of hazardous solvent residual.
What the present invention provided utilizes the method that macroporous adsorbent resin extracts cordycepin and Cordyceps polysaccharide from Cordyceps militaris (L.) Link., including Cordyceps militaris (L.) Link.sporophore being pulverized, using water extraction, extracting solution is concentrated, it is subsequently adding ethanol stand precipitation Cordyceps polysaccharide and obtain supernatant, supernatant is crossed macroporous adsorptive resins and obtains eluent, eluent concentrate drying is obtained cordycepin extractum.
As improvement, above-mentioned grinding particle size is 10-30 mesh.
As improvement, above-mentioned water extraction material-water ratio is 1:5-20, Extracting temperature 50-70 DEG C.
As improvement, above-mentioned by extracting solution concentration, temperature controls at 50-70 DEG C, concentrates extracting solution for proportion 1.1-1.5g/cm3Thick paste.
As improvement, above-mentioned macroporous adsorptive resins excessively, eluting solvent is the ethanol water of 20-50%, elution flow rate 2-5BV/h.
As improvement, above-mentioned by eluent concentration, control temperature and be 50-70 DEG C, eluent is concentrated as thick paste.
As improvement, above-mentioned by eluent concentrate drying, obtain cordycepin content extractum more than 15%.
The dry cream of cordycepin that the present invention obtains can be fabricated directly into product, and in addition to cordycepin content is greatly improved, other effective ingredient such as protein, aminoacid and trace element are also retained；If the dry cream of the cordycepin obtained refines again, although can obtain the cordycepin of purity more than 98%, but yield is extremely low, only about 10%, raw material is caused waste.
The present invention, with Cordyceps militaris (L.) Link.sporophore as raw material, utilizes the effective of macroporous resin adsorption cordycepin, decreases the loss of cordycepin, improves yield；Do not use the chemical reagent such as HCl, ammonia, it is ensured that the green of put forward cordycepin product, health；Can produce the cordycepin product with physiologically active cordycepin, products obtained therefrom hazardous solvent residual is few；The method has the clear and definite process conditions of applicable industrialized production, and step is simple, and low cost can realize industrialized production.
Accompanying drawing explanation
Accompanying drawing 1 is the cordycepin eluent HPLC detection figure of embodiment 1.
Detailed description of the invention
Cordyceps militaris (L.) Link.sporophore (cordycepin content is at 0.2-0.5%) is dried the water content to less than 5% by the inventive method, pulverizes with the screen cloth of 10-30 mesh, and wherein grinding particle size is optimal with 20 mesh.
Raw material after pulverizing, with water as Extraction solvent, material-water ratio is 1:5-20, Extracting temperature 50-70 DEG C, and each extraction time is 2-10h.
It is 1.1-1.5g/cm by the extracting solution obtained with being concentrated to proportion3Thick paste, wherein thickening temperature controls at 50-70 DEG C, and vacuum, at-0.005 to-0.009 Mpa, adds the ethanol of 2-5 times of thick paste volume, stands overnight that to take supernatant standby, obtains alcohol hypostasis, is dried i.e. thick Cordyceps polysaccharide.
It is diluted supernatant processing, in case carrying out purification with macroreticular resin.During upper prop control load solution cordycepin mass concentration be 0.6-2.0mg/mL, loading volume 2-10BV, loading flow velocity 1-3BV/h；Desorption solvent is 20-50% ethanol water (preferably 25%), elution flow rate 2-5BV/h, desorption solvent volume 4-10BV used.
It is-0.005Mpa by the eluent eluted at pressure to concentrate when being 50-70 DEG C to-0.009Mpa, temperature, is concentrated into thick paste state, after being then dried, obtains the dry cream of cordycepin of cordycepin content more than 15%.It is described in detail with specific embodiment below:
Embodiment one
Extraction cordycepin and Cordyceps polysaccharide from Cordyceps militaris (L.) Link. in the steps below:
(1) pulverize: artificial cordyceps militaris fruiting body is dried to moisture below 5% at 50 DEG C, cross 10 eye mesh screens pulverizing；
(2) with water extraction: being thrown into by the Cordyceps militaris (L.) Link.sporophore that 150kg pulverizes in the extraction pot of 3 tons, inject purified water 3000kg, solid-liquid ratio 1:20, and open stirring, temperature controls at 65-70 DEG C, and each soak extraction time is 2 hours, repeats soak extraction three times；
(3) concentrate precipitate with ethanol: the extracting solution of three times mixed also, squeeze into vacuum concentration pot and be evaporated to the thick paste of 160kg (proportion is 1.5g/cm3), wherein thickening temperature 50-70 DEG C, concentration pressure-0.005 to-0.009Mpa.In thick paste, add 95% ethanol of 5 times of thick paste volumes, stand overnight that to take supernatant standby, obtain alcohol hypostasis, be dried i.e. thick Cordyceps polysaccharide；
(4) macroporous adsorbent resin eluting: take supernatant and be diluted processing, control load solution cordycepin mass concentration 0.6mg/mL, loading volume 10BV, loading flow velocity 3BV/h；Eluting solvent is 50% ethanol water, elution flow rate 2BV/h, elution volume 4BV.Eluent sampling HPLC detects, and wavelength 260nm is shown in accompanying drawing 1.
(5) concentrate drying: the eluent eluted is squeezed into vacuum concentration pot, is that-0.005Mpa extremely-0.009Mpa, temperature concentrate when being 50-70 DEG C at pressure, is concentrated into thick paste.Then being proceeded to microwave drying oven, temperature and pressure is all the same with when concentrating, and obtains the dry cream of cordycepin that content is 17%, yield 63% after drying.
Embodiment two
Extraction cordycepin and Cordyceps polysaccharide from Cordyceps militaris (L.) Link. in the steps below:
(1) pulverize: artificial cordyceps militaris fruiting body is dried to moisture below 5% at 50 DEG C, cross 30 eye mesh screens pulverizing；
(2) with water extraction: being thrown into by the Cordyceps militaris (L.) Link.sporophore that 150kg pulverizes in the extraction pot of 3 tons, inject purified water 750kg, solid-liquid ratio 1:5, and open stirring, temperature controls at 50-55 DEG C, and each soak extraction time is 10 hours, repeats soak extraction three times；
(3) concentrate precipitate with ethanol: the extracting solution of three times mixed also, squeeze into vacuum concentration pot and be evaporated to the thick paste of 150 kg (proportion is 1.1g/cm3), wherein thickening temperature 50-70 DEG C, concentration pressure-0.005 to-0.009Mpa.In thick paste, add 95% ethanol of 2 times of thick paste volumes, stand overnight that to take supernatant standby, obtain alcohol hypostasis, be dried i.e. thick Cordyceps polysaccharide；
(4) macroporous adsorbent resin eluting: take supernatant and be diluted processing, control load solution cordycepin mass concentration 2.0mg/mL, loading volume 2BV, loading flow velocity 1BV/h；Eluting solvent is 20% ethanol water, elution flow rate 5BV/h, elution volume 10BV.
(5) concentrate drying: the eluent eluted is squeezed into vacuum concentration pot, is that-0.005Mpa extremely-0.009Mpa, temperature concentrate when being 50-70 DEG C at pressure, is concentrated into thick paste.Then being proceeded to microwave drying oven, temperature and pressure is all the same with when concentrating, and obtains the dry cream of cordycepin that content is 15.3%, yield 65% after drying.
Claims (3)
1. one kind utilizes the method that macroporous adsorbent resin extracts cordycepin and Cordyceps polysaccharide from Cordyceps militaris (L.) Link., including Cordyceps militaris (L.) Link.sporophore being pulverized, using water extraction, extracting solution is concentrated, it is subsequently adding ethanol stand precipitation Cordyceps polysaccharide and obtain supernatant, supernatant is crossed macroporous adsorptive resins and obtains eluent, eluent concentrate drying is obtained cordycepin extractum；Described water extraction material-water ratio is 1:5-20, Extracting temperature 50-70 DEG C；Described by extracting solution concentration, temperature controls at 50-70 DEG C, concentrates extracting solution for proportion 1.1-1.5g/cm3Thick paste；Described amount of alcohol added is 2-5 times of thick paste volume；Described macroporous adsorptive resins excessively, eluting solvent is the ethanol water of 20-50%, elution flow rate 2-5BV/h；Described by eluent concentration, control temperature and be 50-70 DEG C, eluent is concentrated as thick paste.
The method utilizing macroporous adsorbent resin to extract cordycepin and Cordyceps polysaccharide from Cordyceps militaris (L.) Link. the most according to claim 1, it is characterised in that described grinding particle size is 10-30 mesh.
The method utilizing macroporous adsorbent resin to extract cordycepin and Cordyceps polysaccharide from Cordyceps militaris (L.) Link. the most according to claim 1 and 2, it is characterised in that described by eluent concentrate drying, obtains cordycepin content extractum more than 15%.
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| CN201310592568.2A CN103601812B (en) | 2013-11-22 | 2013-11-22 | Utilize the method that macroporous adsorbent resin extracts cordycepin and Cordyceps polysaccharide from Cordyceps militaris (L.) Link. |
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| CN201310592568.2A CN103601812B (en) | 2013-11-22 | 2013-11-22 | Utilize the method that macroporous adsorbent resin extracts cordycepin and Cordyceps polysaccharide from Cordyceps militaris (L.) Link. |
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| CN103601812B true CN103601812B (en) | 2016-08-17 |
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| CN103966064A (en) * | 2014-04-30 | 2014-08-06 | 湖南生有虫草生物科技有限公司 | Cordyceps militaris nucleic acid nutritive wine and producing method thereof |
| CN105801718A (en) * | 2016-04-21 | 2016-07-27 | 浙江工业大学 | Extraction method of cordyceps sinensis flower polysaccharide |
| CN105996022A (en) * | 2016-07-12 | 2016-10-12 | 江苏大学 | Method for producing functional foods by simultaneously converting Chinese yam from cordyceps taishanensis |
| CN111574570B (en) * | 2020-04-30 | 2023-06-30 | 烟台金草王生物科技有限公司 | Comprehensive utilization method of cordyceps militaris culture residues |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| KR20010054264A (en) * | 1999-12-04 | 2001-07-02 | 안용준 | Cordycepin separated from Cordyceps spp. for an anti-cancer medicine and its production |
| CN101157712A (en) * | 2007-11-16 | 2008-04-09 | 上海市农业科学院 | Method for separating and purifying cordycepin |
| CN101716196A (en) * | 2009-12-04 | 2010-06-02 | 华南师范大学 | Cordycepin extractive and application thereof in preparing hypoglycemic drugs or health-care foods |
| CN101906127A (en) * | 2010-07-23 | 2010-12-08 | 上海国宝企业发展中心 | Method for extracting cordycepin and cordyceps polysaccharides from residue of cordyceps militaris culture medium |
| CN102558264A (en) * | 2012-01-18 | 2012-07-11 | 辽宁仙榆湾北冬虫夏草（集团）有限公司 | Method for extracting cordycepin and cordyceps polysaccharide from cordyceps militaris |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102432656B (en) * | 2011-12-23 | 2014-07-02 | 辽宁省农业科学院大连生物技术研究所 | Method for extracting and purifying cordycepin from Cordyceps militaris sporophore |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20010054264A (en) * | 1999-12-04 | 2001-07-02 | 안용준 | Cordycepin separated from Cordyceps spp. for an anti-cancer medicine and its production |
| CN101157712A (en) * | 2007-11-16 | 2008-04-09 | 上海市农业科学院 | Method for separating and purifying cordycepin |
| CN101716196A (en) * | 2009-12-04 | 2010-06-02 | 华南师范大学 | Cordycepin extractive and application thereof in preparing hypoglycemic drugs or health-care foods |
| CN101906127A (en) * | 2010-07-23 | 2010-12-08 | 上海国宝企业发展中心 | Method for extracting cordycepin and cordyceps polysaccharides from residue of cordyceps militaris culture medium |
| CN102558264A (en) * | 2012-01-18 | 2012-07-11 | 辽宁仙榆湾北冬虫夏草（集团）有限公司 | Method for extracting cordycepin and cordyceps polysaccharide from cordyceps militaris |
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