CN1765935A - Method for separating lentinan - Google Patents
Method for separating lentinan Download PDFInfo
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- CN1765935A CN1765935A CN 200510017261 CN200510017261A CN1765935A CN 1765935 A CN1765935 A CN 1765935A CN 200510017261 CN200510017261 CN 200510017261 CN 200510017261 A CN200510017261 A CN 200510017261A CN 1765935 A CN1765935 A CN 1765935A
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- lentinan
- polyoxyethylene glycol
- mushroom
- precipitation
- separation method
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Abstract
The invention discloses a new method to separate lentinan and cartinellin amylose, which comprises: drying and breaking one or more of fruiting body, mycelium, handle and fermentation liquid of mushroom, adding water, heating, extracting; filtering the insolubles, condensing the liquid, adding carbowax, stirring to dissolve the carbowax; placing for a while; cleaning the separated deposition with organic solvent. This method just uses carbowax of 1/4~1/10 to alcohol, cuts process greatly, reduces cost, and the extract content more than 90%.
Description
Technical field
The present invention is the improvement to existing lentinan and Lentinan extraction process, a kind of novel method of separating lentinan and Lentinan is disclosed, with any or any two or more in the mycelium of the sporophore of mushroom, mushroom, champignon stems, the Lentinus Edodes fungus fermented liquid is that raw material extracts, and relates to Chinese medicine extracts active ingredients technical field.
Background technology
Mushroom is the traditional Chinese medicinal materials of China, has the effect of tonifying liver benefit gas.Lentinan is one of main active ingredient of mushroom, has curative effects such as antitumor, antiviral, treatment hepatitis B, is widely used.Japan at first succeeded in developing the lentinan injection in 1985, was used for treating cancer of the stomach.Then there is the people from mushroom submerged fermentation nutrient solution, to extract polysaccharide, the lentinan that called after " Lentinan " extracts from mushroom with difference.
The present more complicated of the extraction process of lentinan and Lentinan, extraction solvent commonly used is an ethanol, if the ethanol that is used for precipitating lentinan and Lentinan 2～4 times of extracting solution usually, so that polysaccharide is separated out.And the purity of polysaccharide of extracting like this is not high, still need just can make the content of polysaccharide reach 90% through a series of subsequent disposal, has improved cost greatly, makes the price of lentinan higher for a long time.In recent years, there are many people that the extracting method of lentinan and Lentinan is improved, in the patent application of the relevant lentinan of Chinese patent nearly 30, but finally all can't break away from this step of ethanol sedimentation, this extraction step has not only expended a large amount of ethanol, and the lentinan content that obtains is not high, and it is complicated to cause subsequent technique to handle.
Summary of the invention
The present invention discloses a kind of novel method of separating lentinan and Lentinan, simplifies and extracts flow process, reduces production costs.
Technical solution of the present invention is as follows: with any or any two or more in the mycelium of the sporophore of mushroom, mushroom, champignon stems, the Lentinus Edodes fungus fermented liquid is raw material, add polyoxyethylene glycol after the extracting solution of above-mentioned raw materials or fermented liquid concentrated, fully stir and make the polyoxyethylene glycol dissolving, leave standstill, separate obtaining precipitation, precipitation promptly gets product of the present invention with organic solvent repetitive scrubbing after drying.
Detailed process may further comprise the steps:
Get the sporophore of mushroom, the mycelium of mushroom, champignon stems, any or multiple above crushed after being dried in the Lentinus Edodes fungus fermented liquid, the water that adds 6～10 times of amounts, 40～100 ℃ are extracted 2～3 times, each 1～2 hour, united extraction liquid, the elimination insolubles, extracting solution is concentrated into solid content 5%～30%, adds polyoxyethylene glycol to concentrated solution weight 1/4～1/10, stirring is dissolved polyoxyethylene glycol fully, placement is waited to precipitate and is separated out, ethanol with 40%～100% carries out refluxing extraction to throw out, and the taking precipitate drying obtains lentinan or Lentinan, yield 3%, content is greater than 90%.
Described molecular weight polyethylene glycol is PEG1000～20000.
The present invention and existing its positively effect of separation method comparison are: replace ethanol as extracting solvent with polyoxyethylene glycol, consumption is an alcoholic acid 1/4～1/10, and whole separating technology only needed for 4 steps can finish, and had shortened technical process greatly, reduce production cost, improved quality product.Because this production technique a large amount of organic solvent of no use carries out separation and Extraction, therefore, has reduced environmental pollution in the production process.Lentinan that extracts with present method and Lentinan content can be used as the raw material of Lentinan sheet and lentinan injection greater than 90%.
Embodiment
By following examples the present invention is described for example further, and do not limit the present invention in any way, under the prerequisite that does not deviate from technical solution of the present invention, any change or change that those of ordinary skills that the present invention did are realized easily all will fall within the claim scope of the present invention.
Embodiment 1
From mushroom fruiting body, extract lentinan
The dried thin mushroom sporophore is pulverized, and crosses sieve No. two.Take by weighing 200 these powder of gram, water 90 degree that add 10 times of amounts extracted 2 times repeatedly 2 hours.Merge 2 times extracting solution, be evaporated to 400 milliliters.Add polyoxyethylene glycol (PEG6000) 80 grams, fully stir and make the polyoxyethylene glycol dissolving fully.Placement is spent the night and is made precipitation fully.Centrifugal must the precipitation, precipitation is with 200 milliliter of 95% alcohol reflux 2 hours, 2 times repeatedly.50 ℃ of cryodryings of precipitation after the extraction get lentinan 6.2 grams, white powder solid, polysaccharide content 94%.
Embodiment 2
From champignon stems, extract lentinan
The dried thin mushroom handle is pulverized, and crosses sieve No. two.Take by weighing 200 these powder of gram, water 90 degree that add 10 times of amounts extracted 2 times repeatedly 2 hours.Merge 2 times extracting solution, use the membrane ultrafiltration of the molecular weight 5000 that dams to be concentrated into 500 milliliters.Add polyoxyethylene glycol (PEG10000) 80 grams, fully stir and make the polyoxyethylene glycol dissolving fully.Placement is spent the night and is made precipitation fully.Centrifugal must the precipitation, precipitation is with 200 milliliter of 60% alcohol reflux 2 hours, 2 times repeatedly.55 ℃ of cryodryings of precipitation after the extraction get lentinan 5.1 grams, white powder solid, polysaccharide content 92%.
Embodiment 3
From the Lentinus Edodes fungus fermented liquid, extract Lentinan
Get 5000 milliliters of Lentinus Edodes fungus fermented liquids, boil, the centrifugal supernatant liquor that gets.Supernatant concentration to 500 milliliter adds polyoxyethylene glycol (PEG20000) 60 grams, fully stirs and makes the polyoxyethylene glycol dissolving fully.Placement is spent the night and is made precipitation fully.Centrifugal must the precipitation, precipitation is with 200 milliliters of dehydrated alcohol refluxing extraction 2 hours, 2 times repeatedly.Precipitation after the extraction adds the hot water dissolving, removes insolubles, and lyophilize gets Lentinan 0.5 gram, white powder solid, polysaccharide content 95%.
Embodiment 4
From mushroom fruiting body and shiitake mushroom hypha mixture, extract lentinan
Dried thin mushroom sporophore and mycelium mix to be pulverized, and crosses sieve No. two.Take by weighing 200 these powder of gram, water 75 degree that add 10 times of amounts extracted 2 times repeatedly 2 hours.Merge 2 times extracting solution, be evaporated to 400 milliliters.Add polyoxyethylene glycol (PEG4000) 80 grams, fully stir and make the polyoxyethylene glycol dissolving fully.Placement is spent the night and is made precipitation fully.Centrifugal must the precipitation, precipitation is with 200 milliliters of acetone refluxing extraction 2 hours, 2 times repeatedly.50 ℃ of cryodryings of precipitation after the extraction get lentinan 6.1 grams, white powder solid, polysaccharide content 96%.
Embodiment 5
From mushroom fruiting body and champignon stems mixture, extract lentinan
Dried thin mushroom sporophore and champignon stems are mixed pulverizing, cross sieve No. two.Take by weighing 200 these powder of gram, water 80 degree that add 9 times of amounts extracted 2 times repeatedly 2 hours.Merge 2 times extracting solution, be evaporated to 400 milliliters.Add polyoxyethylene glycol (PEG4000) 80 grams, made the polyoxyethylene glycol dissolving fully in ultrasonic 1 hour.Placement is spent the night and is made precipitation fully.Centrifugal must the precipitation, precipitation is with 200 ml methanol refluxing extraction 2 hours, 2 times repeatedly.50 ℃ of cryodryings of precipitation after the extraction get lentinan 6.0 grams, white powder solid, polysaccharide content 95%.
Embodiment 6
From champignon stems and shiitake mushroom hypha mixture, extract lentinan
Dried thin mushroom handle and mycelium mix to be pulverized, and crosses sieve No. two.Take by weighing 200 these powder of gram, water 90 degree that add 8 times of amounts extracted 2 times repeatedly 2 hours.Merge 2 times extracting solution, be evaporated to 400 milliliters.Add polyoxyethylene glycol (PEG6000) 80 grams, fully stir and make the polyoxyethylene glycol dissolving fully.Placement is spent the night and is made precipitation fully.Centrifugal must the precipitation, precipitation was extracted 2 hours with 200 milliliters of ethyl acetate backflow, 2 times repeatedly.Precipitation after precipitation after the extraction is extracted adds the hot water dissolving, removes insolubles, and lyophilize gets Lentinan 5.8 grams, white powder solid, polysaccharide content 92%.
Claims (5)
1, a kind of novel method of separating lentinan and Lentinan, it is characterized in that: get any or multiple above crushed after being dried in the mycelium, champignon stems, Lentinus Edodes fungus fermented liquid of sporophore, the mushroom of mushroom, add water, heating is extracted, concentrated extracting solution behind the elimination insolubles adds polyoxyethylene glycol, fully stirs to make the polyoxyethylene glycol dissolving, leave standstill, the throw out after separating is removed residual polyoxyethylene glycol after drying with the organic solvent repetitive scrubbing promptly get product of the present invention.
2, according to the described separation method of claim 1, it is characterized in that: molecular weight polyethylene glycol is PEG1000～20000.
3, according to the described separation method of claim 1, it is characterized in that: the temperature range of extracting lentinan and Lentinan is between 40～100 ℃.
4, according to the described separation method of claim 1, it is characterized in that: being used for the organic solvent of the residual polyoxyethylene glycol of flush away wants to dissolve polyoxyethylene glycol and does not dissolve lentinan and Lentinan: ethanol, acetone, methyl alcohol, ethyl acetate etc.
5, according to the described separation method of claim 1, it is characterized in that: being used for the concentration of organic solvent of the residual polyoxyethylene glycol of flush away is 40%～100%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100172615A CN100453559C (en) | 2005-11-04 | 2005-11-04 | A kind of method of extracting lentinan |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100172615A CN100453559C (en) | 2005-11-04 | 2005-11-04 | A kind of method of extracting lentinan |
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| CN1765935A true CN1765935A (en) | 2006-05-03 |
| CN100453559C CN100453559C (en) | 2009-01-21 |
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| CNB2005100172615A Expired - Fee Related CN100453559C (en) | 2005-11-04 | 2005-11-04 | A kind of method of extracting lentinan |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7514085B2 (en) | 2004-07-16 | 2009-04-07 | Medimush A/S | Immune modulating compounds from fungi |
| CN101921346A (en) * | 2010-08-31 | 2010-12-22 | 浙江省林业科学研究院 | A radial flow chromatographic separation method of polysaccharides from shiitake mushroom mycelium |
| CN101323649B (en) * | 2008-08-04 | 2012-02-29 | 南方李锦记有限公司 | Method for extracting mushroom polysaccharide by using ultra-high pressure |
| CN101775422B (en) * | 2010-02-05 | 2012-04-04 | 武汉迪奥药业有限公司 | A kind of mushroom polysaccharide and preparation method thereof |
| CN101538334B (en) * | 2009-04-24 | 2012-05-30 | 昆明理工大学 | Method for extracting medicinal large leaf moss polysaccharide |
| CN103360505A (en) * | 2013-07-15 | 2013-10-23 | 陕西师范大学 | Method for extracting pomegranate rind polysaccharide with assistance of polyethylene glycol-ultrasonic microwaves |
| US8758768B2 (en) | 2001-09-03 | 2014-06-24 | Glycanova As | Process for production of fungal extracellular immune stimulating compounds |
| US9072776B2 (en) | 2005-06-15 | 2015-07-07 | Glycanova As | Anti-cancer combination treatment and kit-of-parts |
| CN105384840A (en) * | 2015-12-22 | 2016-03-09 | 浙江省林业科学研究院 | Method for extracting lentinula edodes foot polysaccharides |
| CN106478838A (en) * | 2016-12-02 | 2017-03-08 | 湖北省农业科学院农产品加工与核农技术研究所 | A kind of extracting method of high-purity edible fungi polysaccharide |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000159809A (en) * | 1998-11-27 | 2000-06-13 | Kobayashi Pharmaceut Co Ltd | Fraction of lentinula hypha extract and its use |
| CN1178957C (en) * | 1999-12-01 | 2004-12-08 | 上海国宝企业发展中心 | Method of extracting lentinan from lentinus edodes root as material |
| CN1204148C (en) * | 2002-08-22 | 2005-06-01 | 武汉东保科技开发有限责任公司 | Separation and purification process of lentinan |
| KR20040090374A (en) * | 2003-04-16 | 2004-10-22 | 팜텍(주) | Preparation method of water soluble polysaccharide comprising β-glucan from Korean oak mushroom |
| JP2005133069A (en) * | 2003-10-09 | 2005-05-26 | Ichimasa Kamaboko Co Ltd | Process for obtaining β-glucan polysaccharide derived from mushrooms β-glucan polysaccharide derived from mushrooms |
-
2005
- 2005-11-04 CN CNB2005100172615A patent/CN100453559C/en not_active Expired - Fee Related
Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8758768B2 (en) | 2001-09-03 | 2014-06-24 | Glycanova As | Process for production of fungal extracellular immune stimulating compounds |
| US10471135B2 (en) | 2001-09-03 | 2019-11-12 | Glycanova As | Production of fungal extracellular immune stimulating compounds |
| US9249438B2 (en) | 2001-09-03 | 2016-02-02 | Glycanova As | Production of fungal extracellular immune stimulating compounds |
| US7682615B2 (en) | 2004-07-16 | 2010-03-23 | Beka Holding As | Immune modulating compounds from fungi |
| US7514085B2 (en) | 2004-07-16 | 2009-04-07 | Medimush A/S | Immune modulating compounds from fungi |
| US9072776B2 (en) | 2005-06-15 | 2015-07-07 | Glycanova As | Anti-cancer combination treatment and kit-of-parts |
| CN101323649B (en) * | 2008-08-04 | 2012-02-29 | 南方李锦记有限公司 | Method for extracting mushroom polysaccharide by using ultra-high pressure |
| CN101538334B (en) * | 2009-04-24 | 2012-05-30 | 昆明理工大学 | Method for extracting medicinal large leaf moss polysaccharide |
| CN101775422B (en) * | 2010-02-05 | 2012-04-04 | 武汉迪奥药业有限公司 | A kind of mushroom polysaccharide and preparation method thereof |
| CN101921346B (en) * | 2010-08-31 | 2011-12-21 | 浙江省林业科学研究院 | Radial flow chromatography for polysaccharides of mushroom hyphae |
| CN101921346A (en) * | 2010-08-31 | 2010-12-22 | 浙江省林业科学研究院 | A radial flow chromatographic separation method of polysaccharides from shiitake mushroom mycelium |
| CN103360505A (en) * | 2013-07-15 | 2013-10-23 | 陕西师范大学 | Method for extracting pomegranate rind polysaccharide with assistance of polyethylene glycol-ultrasonic microwaves |
| CN103360505B (en) * | 2013-07-15 | 2015-10-28 | 陕西师范大学 | The method of polyoxyethylene glycol-ultrasonic-microwave assisted extraction pomegranate rind polysaccharide |
| CN105384840A (en) * | 2015-12-22 | 2016-03-09 | 浙江省林业科学研究院 | Method for extracting lentinula edodes foot polysaccharides |
| CN106478838A (en) * | 2016-12-02 | 2017-03-08 | 湖北省农业科学院农产品加工与核农技术研究所 | A kind of extracting method of high-purity edible fungi polysaccharide |
| CN106478838B (en) * | 2016-12-02 | 2019-04-23 | 湖北省农业科学院农产品加工与核农技术研究所 | A kind of extracting method of high-purity edible fungi polysaccharide |
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| Publication number | Publication date |
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| CN100453559C (en) | 2009-01-21 |
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Granted publication date: 20090121 Termination date: 20121104 |