CN100453559C - Method for separating lentinan - Google Patents

Method for separating lentinan Download PDF

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Publication number
CN100453559C
CN100453559C CNB2005100172615A CN200510017261A CN100453559C CN 100453559 C CN100453559 C CN 100453559C CN B2005100172615 A CNB2005100172615 A CN B2005100172615A CN 200510017261 A CN200510017261 A CN 200510017261A CN 100453559 C CN100453559 C CN 100453559C
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China
Prior art keywords
lentinan
mushroom
cartinellin
polysaccharide
polyethyleneglycol
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CNB2005100172615A
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CN1765935A (en
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杨勇杰
张萍
姜瑞芝
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  • Preparation Of Compounds By Using Micro-Organisms (AREA)
  • Polysaccharides And Polysaccharide Derivatives (AREA)

Abstract

The present invention discloses a new method for separating lentinan and cartinellin polysaccharide. The method comprises: one or more kinds of mushroom fruit bodies, mushroom mycelium, mushroom stems, cartinellin fermentation liquor are dried and are then pulverized; water is added to the materials, and is heated and extracted; after insoluble substances are filtered off, extract liquor is concentrated; polyethyleneglycol is added to the concentrated extract liquor, and is sufficiently stirred so as to dissolve the polyethyleneglycol; the extract liquor is made to stand; separated precipitates are repeatedly washed by organic solvents, and are then dried. The present invention replaces ethanol with polyethyleneglycol as extraction solvents, and the use amount of the polyethyleneglycol is only 1/4 to 1/10 of that of ethanol. The whole separation technology can be finished in four steps, so the present invention greatly shortens technological processes, reduces production cost, and improves product quality. The content of lentinan and cartinellin polysaccharide extracted by the method is larger than 90%. The lentinan and the cartinellin polysaccharide can be used as raw materials of various preparations of lentinan and cartinellin polysaccharide.

Description

A kind of method of extracting lentinan
Technical field
The present invention is the improvement to existing lentinan extraction process, a kind of method of extracting 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, extraction solvent commonly used is an ethanol, if the ethanol that is used for precipitating 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 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 method of extracting 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, 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.The lentinan content that extracts with present method 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 (2)

1, a kind of method of extracting lentinan, it is characterized in that: with the sporophore of mushroom, the mycelium of mushroom, any or multiple crushed after being dried in the champignon stems, add water, heating is extracted, behind the elimination insolubles extracting solution, get and add polyoxyethylene glycol after extracting solution concentrates, fully stir and 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.
2, according to the described extracting method of claim 1, it is characterized in that: molecular weight polyethylene glycol is 1000~20000.
CNB2005100172615A 2005-11-04 2005-11-04 Method for separating lentinan Expired - Fee Related CN100453559C (en)

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Families Citing this family (10)

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NO20014256D0 (en) 2001-09-03 2001-09-03 Bjoern Kristiansen Preparation of immunostimulatory compound
US7514085B2 (en) 2004-07-16 2009-04-07 Medimush A/S Immune modulating compounds from fungi
EP1896600A2 (en) 2005-06-15 2008-03-12 Medimush A/S Anti-cancer combination treatment and kit-of-part
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 Lentinus Edodes Mycelia 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
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
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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