CN101434662B - Method for preparing fungal polysaccharide - Google Patents
Method for preparing fungal polysaccharide Download PDFInfo
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- CN101434662B CN101434662B CN2008102315405A CN200810231540A CN101434662B CN 101434662 B CN101434662 B CN 101434662B CN 2008102315405 A CN2008102315405 A CN 2008102315405A CN 200810231540 A CN200810231540 A CN 200810231540A CN 101434662 B CN101434662 B CN 101434662B
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Abstract
The invention discloses a method for preparing fungi polysaccharide, namely a multi-stage dissolvent-cycle dynamic-thermal-reflux extraction condensation method. The method comprises the technological steps of raw material crushing, mixing with a solvent, extraction, condensation, deposition in alcohol, filtering and drying so as to obtain a finished product. The method for preparing fungi polysaccharide integrates extraction, condensation, solvent recovery and the like together, and is completely carried out in an enclosed system, without any bad occurrence of escaping, steaming, leakage and dripping, etc. The production practice shows that the method can shorten the extraction cycle by 50 percent to 85 percent so as to improve the production rate; the ration between raw material to solvent can be reduced to 1:3-8 (as the traditional method has a ration between raw material and solvent higher than 1:20), and the amount of an extractant used can also be saved by 25 percent to 80 percent; primary/secondary steam can be put into fullplay and cooling water is saved so that the effect of energy conservation is very significant. Compared with the traditional method, the method can save 30 percent to 70 percent of steam amount; and the medical material does not need to be crushed finely, which is favorable to the further operation. The method can be largely applied to the development and production of the fungi polysaccharide and other related polysaccharides or natural medical materials.
Description
Technical field
The present invention relates to a kind of method for preparing fungus polysaccharide.
Background technology
In the world, food, medicinal fungi glycocalix are called " biological response modifier " (Biological ResponseModifier is called for short BRM), and it is the biologically active substance that a class can strengthen immune function of human body, has physiology and pharmacological function widely.In recent years, the continuous appearance along with biological chemistry, biotechnology, biopolymer research new technology, novel method makes both at home and abroad food, medicinal fungi STUDY ON POLYSACHAROSE to be developed rapidly.At present, food, medicinal fungi polysaccharide have become one of the research focus in fields such as biological chemistry, molecular biology, medical science, pharmacy, Food science.Though people have carried out comparatively extensive research to aspects such as the structure of fungus polysaccharide, biological activity, pharmacological functions, how the efficient production fungus polysaccharide does not also cause people's great attention.At present, the preparation method of natural fungus polysaccharide class medicine mainly contains hot water, acid, alkali lixiviate and method, these methods such as gets, no matter be hot cooking's extraction method, still acid, alkali extraction, employed equipment all be basically can't be airtight steam cooker or jar, and all be periodical operation in batches.In process of production, can cause the waste of the great energy and fund, for example, when using the hot water lixiviate, hot water constantly steams in jar in the process of heating, and this just requires us otherwise a large amount of solvents and the energy have consequently been wasted in moisturizing that stops and heating; When (as alcohol, acetone) extracted when with an organic solvent for another example, the continuous volatilization along with organic solvent can cause the huger wasting of resources and environmental pollution.Shortcomings such as in a word, these method ubiquities and can not be realized digestion and spissated continuous operation, and energy utilization rate is low, and solvent load is big, loss is many, and production cycle length and production efficiency are low, and also may cause environmental pollution in some cases; Be difficult to satisfy national GMP standard-required.
Summary of the invention
Technical problem to be solved by this invention provides a kind of extracting cycle and shortens, the production efficiency height, and solvent load is few, and is energy-saving and cost-reducing, reaches a kind of novel method for preparing fungus polysaccharide that national GMP requires easily.
The technical solution used in the present invention is:
The method that this prepares fungus polysaccharide comprises following processing step:
(1) raw material pulverizing is mixed with extraction agent
The raw material that extracts the preparation fungus polysaccharide is cleaned, after the cryodrying, is ground into the particle of 60-7000 μ m, itself and extraction agent were mixed by mass ratio in 1: 2.5～1: 12;
(2) extract
Above-mentioned raw materials and extraction agent mixed solution are carried out the dynamic thermal backflow that circulates of multistage solvent extract in multi-functional extractor, extract 35-100 ℃ of temperature, pH=4-8, under the condition of solvent refluxing rate 5-30% refluxing extraction 40-90 minute;
(3) filter and concentrate
With the extracting solution of said extracted certain hour by secondary wire gauzee filter or centrifuging after directly vacuum be transported in the outer circulation heating-type economic benefits and social benefits vacuum concentrator, at vacuum tightness 0.01-0.08MPa, concentrate 1-3 hour under the temperature 35-80 ℃ of condition, make the density of concentrated solution reach 1.1-1.40g/cm
3
(4) alcohol precipitation
Above-mentioned concentrated solution is pumped into Alcohol-settling tank, add by volume and left standstill 30-120 minute after 2-5 times of 95% alcohol stirs, used alcohol is more than the food grade;
(5) drying
Above-mentioned pure hypostasis is added 3-15 distilled water or other stirring solvent doubly by mass ratio make its dissolving, then, in inlet temperature is 160-220 ℃, temperature out is under the 80-95 ℃ of condition after spraying drying or vacuum freezedrying or the vacuum-drying, can obtain yield and reach 8.92-19.85%, sugar degree reaches the polysaccharide product of 12.90-25.68%.
The raw material that the present invention extracts the preparation fungus polysaccharide means that mushroom, Hericium erinaceus (Bull. Ex Fr.) Pers., glossy ganoderma, black fungus, Grifola frondosa, white fungus, needle mushroom etc. contain any or several in the food of compound of polysaccharide, the medicinal fungi.
Extraction agent of the present invention is meant all any materials that can be used to extract the preparation fungus polysaccharide such as water, ethanol, acetone, ether, alkali, acid, salt.
The dynamic thermal backflow that circulates of multistage solvent is extracted as that the 1-3 level is adjustable arbitrarily as required in described (2) step, both can when extracting, carry out the dynamic thermal backflow that circulates of 1 grade of solvent separately, can when single-action concentrates, carry out the dynamic thermal backflow that circulates of 2 grades of solvents again, also can when economic benefits and social benefits concentrate, carry out the dynamic thermal backflow that circulates of 3 grades of solvents.
Filtration during the step of described (3) is filtered and concentrated is that employing order number is 60-200 purpose secondary Stainless Steel Wire net filtration or tubular type or link-suspended basket centrifuge filtration.
Vacuum freezedrying is at vacuum tightness 25-100Pa in described (5) drying step, vacuum freezedrying under the temperature 20-40 ℃ of condition; Or vacuum-drying is at vacuum tightness 0.01-0.085MPa, the vacuum-drying under temperature 45-75 ℃ of condition.
A kind of beneficial effect for preparing the fungus polysaccharide novel method disclosed in this invention is:
This prepares the method for fungus polysaccharide, and method of enrichment is extracted in the circulate dynamic thermal backflow of promptly multistage solvent, is that collection extracts, concentrates and solvent recuperation etc. is one, and whole process is to carry out in a closed system, can not produce bad phenomenon such as run, drip, leak; Production practice show that this method can shorten extracting cycle 50-85%, enhances productivity; The feed liquid specific energy reduces to 1: 3-8 (and the solid-liquid ratio of traditional method is many more than 1: 20), and can save and extract quantity of solvent 25-80%; Once/and secondary steam both was fully used, and saved cooling water again, and energy-saving effect is very remarkable, and the two compares the steam consumption that can save 30-70%; Do not need very little with pulverizing medicinal materials, increase concentration difference, just guaranteed extraction yield by continuous reflux solvent, so more help follow-up centrifugal with operation such as separate; Easily reach the requirement of national GMP.
Embodiment
Below introduce embodiments of the invention.All material rates are all by mass ratio in these embodiments.
Embodiment 1:
A kind of method for preparing fungus polysaccharide comprises following processing step:
(1) raw material pulverizing is mixed with extraction agent
The raw material (lotus flower bacterium, mushroom, Hericium erinaceus (Bull. Ex Fr.) Pers.) that extracts the preparation fungus polysaccharide is cleaned, after low temperature (30 ℃) drying, is ground into the particle of 60-100 μ m, itself and extraction agent water are mixed by mass ratio at 1: 3.5;
(2) extract
Above-mentioned raw materials and extraction agent mixed solution are carried out the dynamic thermal backflow of the multistage circulation of solvent extract in multi-functional extractor, extract 35 ℃ of temperature, pH=4.5, (adopts 1 grade of solvent circulate dynamic thermal backflow) extraction 40 minutes refluxes under the condition of solvent refluxing rate 5%;
(3) filter and concentrate
With the extracting solution of said extracted certain hour by secondary wire gauzee filter or tubular type centrifuging after directly vacuum be transported in the outer circulation heating-type economic benefits and social benefits vacuum concentrator, at vacuum tightness 0.01MPa, concentrate 1.5 hours under 40 ℃ of conditions of temperature;
(4) alcohol precipitation
Above-mentioned concentrated solution is pumped into Alcohol-settling tank, add by volume and left standstill 30 minutes after 2 times of 95% above alcohol of food grade stirs;
(5) drying
Above-mentioned pure hypostasis is added 3 times distilled water or other stirring solvent by mass ratio make its dissolving, then, at vacuum tightness 0.01-0.085MPa, after the vacuum-drying, can obtain yield and reach 8.95%, 8.92% under 55 ℃ of conditions of temperature, 8.98%, sugar degree reaches 12.90%, 13.29%, 13.18% polysaccharide product.
Embodiment 2:
Identical with the step of embodiment 1, different is:
(1) after the raw material (lotus flower bacterium, mushroom, Hericium erinaceus (Bull. Ex Fr.) Pers.) that will extract the preparation fungus polysaccharide places 50 ℃ of dryings, is ground into the particle of 2500-3000 μ m, itself and extraction agent water are mixed by mass ratio at 1: 8;
(2) extraction conditions is: extract 100 ℃ of temperature, and pH=6.5, (adopts 2 grades of solvents circulate dynamic thermal backflow) extraction 70 minutes refluxes under the condition of solvent refluxing rate 15%;
(3) concentrate:, concentrate 3 hours under 65 ℃ of conditions of temperature at vacuum tightness 0.05MPa;
(4) alcohol precipitation: add by volume and left standstill 80 minutes after 3 times of 95% above alcohol of food grade stirs;
(5) drying: above-mentioned pure hypostasis is added 8 times distilled water or other stirring solvent by mass ratio make its dissolving, then, in inlet temperature is 160-220 ℃, temperature out is a spraying drying under the 80-95 ℃ of condition, can obtain yield and reach 18.85%, 19.68%, 17.15%, sugar degree reaches 23.67%, 24.29%, 25.68% polysaccharide product.
Embodiment 3:
Identical with the step of embodiment 1, different is:
(1) after the raw material (lotus flower bacterium, mushroom, Hericium erinaceus (Bull. Ex Fr.) Pers.) that will extract the preparation fungus polysaccharide places 65 ℃ of dryings, is ground into the particle of 6500-7000 μ m, itself and extraction agent water are mixed by mass ratio at 1: 12;
(2) extraction conditions is: extract 80 ℃ of temperature, and pH=8.5, (adopts 3 grades of solvents circulate dynamic thermal backflow) extraction 90 minutes refluxes under the condition of solvent refluxing rate 28%;
(3) concentrate:, concentrate 2 hours under 80 ℃ of conditions of temperature at vacuum tightness 0.065MPa;
(4) alcohol precipitation: add by volume and left standstill 120 minutes after 5 times of 95% above alcohol of food grade stirs;
(5) drying: above-mentioned pure hypostasis is added 15 times distilled water or other stirring solvent by mass ratio make its dissolving, then, be at vacuum tightness 25-100Pa, vacuum lyophilization under the temperature 20-40 ℃ of condition can obtain yield and reach 18.35%, 19.85%, 17.62%, sugar degree reaches 22.16%, 24.72%, 23.96% polysaccharide product.
Claims (3)
1. method for preparing fungus polysaccharide comprises following processing step:
(1) raw material pulverizing is mixed with extraction agent
The raw material that extracts the preparation fungus polysaccharide is cleaned, after the cryodrying, is ground into the particle of 60-7000 μ m, itself and extraction agent were mixed by mass ratio in 1: 2.5～1: 12;
(2) extract
Above-mentioned raw materials and extraction agent mixed solution are carried out the dynamic thermal backflow that circulates of multistage solvent extract in multi-functional extractor, extract 35-100 ℃ of temperature, pH=4-8, under the condition of solvent refluxing rate 5-30% refluxing extraction 40-90 minute; The dynamic thermal backflow that circulates of multistage solvent is extracted as and carries out the dynamic thermal backflow that circulates of 1 grade of solvent when extracting separately, carries out the dynamic thermal backflow that circulates of 2 grades of solvents when perhaps single-action concentrates, and perhaps carries out the dynamic thermal backflow that circulates of 3 grades of solvents when economic benefits and social benefits concentrate;
(3) filter and concentrate
With the extracting solution of said extracted certain hour by secondary wire gauzee filter or centrifuging after directly vacuum be transported in the outer circulation heating-type economic benefits and social benefits vacuum concentrator, at vacuum tightness 0.01-0.08MPa, concentrate 1-3 hour under the temperature 35-80 ℃ of condition, make the density of concentrated solution reach 1.1-1.40g/cm
3Filtration is that employing order number is 60-200 purpose secondary Stainless Steel Wire net filtration or tubular type or link-suspended basket centrifuge filtration;
(4) alcohol precipitation
Above-mentioned concentrated solution is pumped into Alcohol-settling tank, add by volume and left standstill 30-120 minute after 2-5 times of 95% alcohol stirs; Used alcohol is food grade;
(5) drying
Above-mentioned pure hypostasis is added 3-15 distilled water stirring doubly by mass ratio make its dissolving, then, be 160-220 ℃ in inlet temperature, temperature out is under the 80-95 ℃ of condition after the spraying drying, can obtain yield and reach 8.92-19.85%, sugar degree reaches the polysaccharide product of 12.90-25.68%.
2. the method for preparing fungus polysaccharide according to claim 1 is characterized in that: the raw material of preparation fungus polysaccharide means any in mushroom, Hericium erinaceus (Bull. Ex Fr.) Pers., glossy ganoderma, black fungus, Grifola frondosa, white fungus, the needle mushroom in described (1) step.
3. the method for preparing fungus polysaccharide according to claim 1 and 2 is characterized in that: the extraction agent in described (1) step is meant water, ethanol, acetone, ether.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN2008102315405A CN101434662B (en) | 2008-12-29 | 2008-12-29 | Method for preparing fungal polysaccharide |
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| CN2008102315405A CN101434662B (en) | 2008-12-29 | 2008-12-29 | Method for preparing fungal polysaccharide |
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| CN101434662A CN101434662A (en) | 2009-05-20 |
| CN101434662B true CN101434662B (en) | 2011-06-22 |
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| CN2008102315405A Expired - Fee Related CN101434662B (en) | 2008-12-29 | 2008-12-29 | Method for preparing fungal polysaccharide |
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| CN102093598B (en) * | 2010-09-06 | 2013-09-11 | 山东好当家海洋发展股份有限公司 | Composite edible fungi polysaccharides and preparation method thereof |
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| CN103549405A (en) * | 2013-11-01 | 2014-02-05 | 王颖 | Method for extracting agaric essences |
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| CN103819571B (en) * | 2013-12-20 | 2016-08-17 | 中华全国供销合作总社南京野生植物综合利用研究所 | A kind of Tremella fructification polysaccharide technology of preparing |
| CN104059160B (en) * | 2014-06-25 | 2016-08-24 | 上海市农业科学院 | A kind of Hericium erinaceus (Bull. Ex Fr.) Pers. cell wall polysaccharides and preparation method thereof |
| CN104045731A (en) * | 2014-06-26 | 2014-09-17 | 河南中烟工业有限责任公司 | Flammulina velutipes polysaccharide and extracting and purifying method thereof as well as application of flammulina velutipes polysaccharide as tobacco humectant |
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| CN104231103B (en) * | 2014-09-17 | 2017-05-24 | 上海交通大学 | Flammulina velutipes polysaccharide as well as preparation method and application thereof |
| CN104480022A (en) * | 2014-11-24 | 2015-04-01 | 广东省微生物研究所 | Collecting method of liquid-cultured fungus mycelia |
| CN104403021A (en) * | 2014-11-28 | 2015-03-11 | 哈尔滨墨医生物技术有限公司 | Method for extracting high-activity hericium erinaceus polysaccharide |
| CN105831773A (en) * | 2016-03-23 | 2016-08-10 | 北京东方兴企食品工业技术有限公司 | Functional food of compound fungal polysaccharide and composition |
| CN105906731A (en) * | 2016-04-25 | 2016-08-31 | 百朗德生物化学海门有限公司 | Production method and use of natural tremella polysaccharide |
| CN105754002B (en) * | 2016-04-29 | 2018-06-12 | 江苏耐雀生物工程技术有限公司 | A kind of preparation method of high content silver fungus polysaccharides |
| CN107223937A (en) * | 2017-06-08 | 2017-10-03 | 安徽真心食品有限公司 | A kind of stomach-nourishing type water boils peanut rice processing method |
| CN107630055A (en) * | 2017-11-16 | 2018-01-26 | 天津北洋百川生物技术有限公司 | The method for adding serine production pulullan polysaccharide |
| CN109456416B (en) * | 2018-12-17 | 2021-03-23 | 河北科技大学 | Extraction method of tremella polysaccharide |
| CN109504725B (en) * | 2018-12-26 | 2021-07-02 | 华熙生物科技股份有限公司 | Method for preparing high-purity hericium erinaceus polysaccharide by fermenting hericium erinaceus and fermentation culture medium |
| CN111378053A (en) * | 2020-05-09 | 2020-07-07 | 福州康来生物科技有限公司 | Extraction method of hericium erinaceus polysaccharide |
| CN112690336A (en) * | 2021-01-29 | 2021-04-23 | 刘刚 | Milk containing edible fungus polysaccharide extract and preparation method thereof |
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| CN2221441Y (en) * | 1995-06-12 | 1996-03-06 | 周希勤 | External-heating multi-stage multi-energy extraction device |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2221441Y (en) * | 1995-06-12 | 1996-03-06 | 周希勤 | External-heating multi-stage multi-energy extraction device |
Non-Patent Citations (1)
| Title |
|---|
| 王卫国等.香菇多糖分离纯化技术研究.《中国食用菌》.2002,第21卷(第2期),第31页第1小节. * |
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