CN104231108A - Production method for extracting tremella polysaccharide by subcritical water extraction-hot water digestion two-step method - Google Patents
Production method for extracting tremella polysaccharide by subcritical water extraction-hot water digestion two-step method Download PDFInfo
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- CN104231108A CN104231108A CN201410546381.3A CN201410546381A CN104231108A CN 104231108 A CN104231108 A CN 104231108A CN 201410546381 A CN201410546381 A CN 201410546381A CN 104231108 A CN104231108 A CN 104231108A
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- 150000004676 glycans Chemical class 0.000 title claims abstract description 86
- 229920001282 polysaccharide Polymers 0.000 title claims abstract description 85
- 239000005017 polysaccharide Substances 0.000 title claims abstract description 85
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 73
- 241001506047 Tremella Species 0.000 title claims abstract description 53
- 238000000034 method Methods 0.000 title claims abstract description 24
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 16
- 230000029087 digestion Effects 0.000 title abstract 3
- 238000000605 extraction Methods 0.000 claims abstract description 54
- 239000008367 deionised water Substances 0.000 claims abstract description 29
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 29
- 239000007788 liquid Substances 0.000 claims abstract description 25
- 238000003809 water extraction Methods 0.000 claims abstract description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000001914 filtration Methods 0.000 claims abstract description 8
- 239000003957 anion exchange resin Substances 0.000 claims abstract description 4
- 241000233866 Fungi Species 0.000 claims description 18
- 238000003756 stirring Methods 0.000 claims description 11
- 239000000284 extract Substances 0.000 claims description 10
- 239000012528 membrane Substances 0.000 claims description 10
- 239000000843 powder Substances 0.000 claims description 10
- 238000000108 ultra-filtration Methods 0.000 claims description 10
- 239000000243 solution Substances 0.000 claims description 7
- 239000006228 supernatant Substances 0.000 claims description 7
- 239000000706 filtrate Substances 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 4
- 239000012535 impurity Substances 0.000 claims description 3
- 239000000049 pigment Substances 0.000 claims description 3
- 102000004169 proteins and genes Human genes 0.000 claims description 3
- 108090000623 proteins and genes Proteins 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 238000005265 energy consumption Methods 0.000 abstract description 5
- 239000012141 concentrate Substances 0.000 abstract 2
- 238000001035 drying Methods 0.000 abstract 2
- 238000002156 mixing Methods 0.000 abstract 2
- 239000002244 precipitate Substances 0.000 abstract 2
- 230000001376 precipitating effect Effects 0.000 abstract 2
- 235000001674 Agaricus brunnescens Nutrition 0.000 description 5
- 229920001491 Lentinan Polymers 0.000 description 4
- 210000002421 cell wall Anatomy 0.000 description 4
- 238000009413 insulation Methods 0.000 description 4
- 229940115286 lentinan Drugs 0.000 description 4
- 238000001816 cooling Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 229960004756 ethanol Drugs 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 230000008595 infiltration Effects 0.000 description 3
- 238000001764 infiltration Methods 0.000 description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000002255 enzymatic effect Effects 0.000 description 2
- 238000002386 leaching Methods 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 239000004332 silver Substances 0.000 description 2
- 238000002137 ultrasound extraction Methods 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- 244000252132 Pleurotus eryngii Species 0.000 description 1
- 235000001681 Pleurotus eryngii Nutrition 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 102000011759 adducin Human genes 0.000 description 1
- 108010076723 adducin Proteins 0.000 description 1
- 230000003712 anti-aging effect Effects 0.000 description 1
- 230000002019 anti-mutation Effects 0.000 description 1
- 239000003699 antiulcer agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 210000001124 body fluid Anatomy 0.000 description 1
- 239000010839 body fluid Substances 0.000 description 1
- 238000004737 colorimetric analysis Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 229960000935 dehydrated alcohol Drugs 0.000 description 1
- 238000000855 fermentation Methods 0.000 description 1
- 230000004151 fermentation Effects 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 230000002518 glial effect Effects 0.000 description 1
- 230000002218 hypoglycaemic effect Effects 0.000 description 1
- 230000036039 immunity Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 210000004072 lung Anatomy 0.000 description 1
- 235000008935 nutritious Nutrition 0.000 description 1
- 230000036961 partial effect Effects 0.000 description 1
- OQUKIQWCVTZJAF-UHFFFAOYSA-N phenol;sulfuric acid Chemical compound OS(O)(=O)=O.OC1=CC=CC=C1 OQUKIQWCVTZJAF-UHFFFAOYSA-N 0.000 description 1
- 150000004804 polysaccharides Polymers 0.000 description 1
- 238000011403 purification operation Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000001603 reducing effect Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 210000002784 stomach Anatomy 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
Landscapes
- Polysaccharides And Polysaccharide Derivatives (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention discloses a production method for extracting tremella polysaccharide by the subcritical water extraction-hot water digestion two-step method. The production method comprises the following steps: adding tremella to a subcritical extraction kettle; adding deionized water based on solid-to-liquid ratio of 1: 10-20kg/L to perform subcritical water extraction; directly transferring subcritical water extraction liquid into a mixing tank in which deionized water is added based on the solid-to-liquid ratio of 1: 20-30kg/L; mixing to dissolve; performing rough filtering, centrifuging and concentrating to obtain tremella polysaccharide concentrate; or precipitating concentrate through alcohol, and drying the alcohol precipitate to obtain tremella polysaccharide; or adding deionized water to alcohol precipitate; adding anion exchange resin column; performing purifying, concentrating, precipitating with alcohol, and drying to obtain the refined tremella polysaccharide. According to the production method, the tremella polysaccharide is processed by subcritical water extraction based on relatively small solid-to-liquid ratio, then the tremella polysaccharide is processed by deionized water digestion based on relatively high solid-to-liquid ratio, and therefore, the space utilization rate of an extraction kettle used is raised, and the consumption of subcritical water and energy consumption can be reduced.
Description
Technical field
The present invention relates to a kind of extracting method of edible fungi polysaccharide, especially utilize the industrialized preparing process of Subcritical water chromotagraphy tremella polysaccharide, belong to edible mushrooms field of deep.
Background technology
White fungus (Tremella fuciformls) is that a kind of economic worth is high, nutritious medicine-food two-purpose bacterium, has that nourishing is promoted the production of body fluid, effect of moistening lung nourishing the stomach.Tremella polysaccharide is the main active ingredient of white fungus, has and improves the effect such as body immunity, hypoglycemic, reducing blood-fat, anti-ageing, antiulcer agent, antithrombus formation, anti-mutation.At present, the conventional extraction of tremella polysaccharide is Hot water extraction, but this traditional extracting method also exist extraction yield low, consuming time, cause the problems such as the wasting of resources.Tremella polysaccharide is divided into exocellular polysaccharide and cell wall polysaccharide, and cell wall polysaccharide use water is difficult to extract completely, even diluted acid or diluted alkaline extraction method, again because par-tial polysaccharide is easily hydrolyzed, destroys the active structure of polysaccharide, causes polysaccharide loss and extraction yield to reduce.
In recent years, researchist adopts the emerging technologies such as zymohydrolysis extracting method, ultrasonic extraction, microwave loss mechanisms and Subcritical Water Extraction method, improves the extraction yield of tremella polysaccharide all to a certain extent.Zymohydrolysis extracting method has that polysaccharide extract rate is high, reaction conditions is gentle, destroy little advantage to polysaccharide structures, but due to the price of enzyme more expensive, production cost is relatively high, is not suitable for being applied to large batch of industrial production.Ultrasonic extraction and microwave loss mechanisms can improve the extraction yield of polysaccharide, shorten extraction time, but cause the component of polyoses extract more complicated sometimes, bring certain difficulty to follow-up separation and purification operation.
With regard to Subcritical Water Extraction method, because subcritical water has good infiltration and dissolving power, be conducive to the extraction yield improving edible fungi polysaccharide.As Lou Guanqun etc. adopts Subcritical water chromotagraphy lentinan, optimum extraction condition is subcritical water temperature 150 DEG C, solid-to-liquid ratio 1:30, extraction time is 5min, and extraction time is 2 times, lentinan yield can reach 15.7% under this condition, compared with Hot water extraction, obviously can reduce extraction time and improve lentinan yield (technical study of Subcritical water chromotagraphy lentinan, " Northeast Agricultural University's journal ", 2010,41 (2): 138-142).But white fungus is a kind of special glial mushroom, is different from the edible mushrooms that mushroom, needle mushroom, Pleurotus eryngii etc. are common, a large amount of moisture can be absorbed, the rate of expansion of dried tremella can reach more than 10 times, and the solid-to-liquid ratio of extraction wants large, otherwise abundant for polysaccharide stripping and cannot extract completely.As: Lin Yuye etc. adopt Enzymatic Extraction tremella polysaccharide, and solid-to-liquid ratio is 1:80 (research of Enzymatic Extraction tremella polysaccharide, " food and fermentation industries ", 1995,1:13-17); Carrying out lucky grade adopts hot-water process to extract tremella polysaccharide, and solid-to-liquid ratio is 1:100 (tremella polysaccharide industrialization optimal extraction technology and skin-care effect are studied, " daily chemical industry ", 2010,40 (4): 259-262).Therefore, Subcritical Water Extraction method is utilized to extract tremella polysaccharide, one is the restriction by high-temperature and high-pressure conditions, it is too large that the volume of subcritical abstraction still can not do, two is that the solid-to-liquid ratio extracted is too high, and the space availability ratio of subcritical abstraction still is extremely low, and too much subcritical water also needs to consume a large amount of heat, consider from economy and efficiency, be also difficult to the requirement adapting to suitability for industrialized production.
Summary of the invention
The object of the invention is the deficiency in order to overcome current tremella polysaccharide extractive technique, a kind of production method adopting Subcritical Water Extraction-hot water extraction's two-step approach to extract tremella polysaccharide is provided.The method the first step adopts the Subcritical Water Extraction tremella polysaccharide of lower solid-to-liquid ratio, subcritical water is utilized to have good infiltration and dissolving power, cell wall polysaccharides and subcritical water are fully contacted and stripping, second step adopts and fully dissolves and Leaching of Silver fungus polysaccharides compared with the deionized water of high solid-liquid ratio, utilize subcritical water to have very high heat energy simultaneously, the extraction temperature of heating deionized water, improves the extraction yield of tremella polysaccharide.Adopt Subcritical Water Extraction-hot water extraction's two-step approach extraction process, not only increase the space availability ratio that extraction kettle uses, and reduce consumption and the energy consumption of subcritical water, the extraction yield of tremella polysaccharide, also higher than traditional hot water extraction's method, makes the technique of Subcritical water chromotagraphy tremella polysaccharide, equipment, economy and efficiency can meet the requirement of suitability for industrialized production.
Technical scheme of the present invention is: a kind of production method adopting Subcritical Water Extraction-hot water extraction's two-step approach to extract tremella polysaccharide, and it is as follows that the method comprising the steps of:
1) low solid-to-liquid ratio Subcritical Water Extraction: being dropped in subcritical abstraction still by the white fungus dry powder pulverized, is that 1:10-20kg/L adds deionized water by solid-to-liquid ratio, Extracting temperature 100-150 DEG C, extraction time 10-120min.
2) deionized water stripping tremella polysaccharide: stirred pot drops into quality for benchmark with white fungus dry powder in advance, be that 1:20-30kg/L adds deionized water by solid-to-liquid ratio, until step 1) extraction terminate after, open extraction kettle bottom valve, subcritical water extract is directly put into stirred pot, after stirring and dissolving is abundant, coarse filtration;
3) by step 2) filtrate of stirred pot is concentrated into the 1/2-1/20 of original volume with the ultra-filtration membrane of the centrifugal 10-20min of rotating speed 3000-5000r/min, supernatant liquor 3-50kD molecular weight cut-off, and obtain tremella polysaccharide and slightly carry concentrated solution.
4) by step 3) tremella polysaccharide slightly carries concentrated solution and adds 95-100%vt ethanol, make ultimate density be 70%wt, after stirring, staticly settle 6-12h, and throw out absolute ethanol washing 1-3 time, vacuum or lyophilize, obtain white fungus Crude polysaccharides.
5) by step 4) throw out adds deionized water to be mixed with polysaccharide content is the 5-10%kg/L aqueous solution, upper anion-exchange resin column, remove the impurity such as protein and pigment, collect polysaccharide effluent liquid, the 1/2-1/20 of original volume is concentrated into the ultra-filtration membrane of 3-50kD molecular weight cut-off, repeating step 4), obtain the tremella polysaccharide refined.
Beneficial effect:
1, the method adopts Subcritical Water Extraction-hot water extraction's two-step approach to extract tremella polysaccharide, the first step adopts the Subcritical Water Extraction tremella polysaccharide of lower solid-to-liquid ratio, subcritical water is utilized to have good infiltration and dissolving power, cell wall polysaccharides and subcritical water are fully contacted and stripping, second step adopts and fully dissolves and Leaching of Silver fungus polysaccharides compared with the deionized water of high solid-liquid ratio, utilize subcritical water to have very high heat energy simultaneously, the extraction temperature of heating deionized water, improves the extraction yield of tremella polysaccharide.
2, the present invention adopts the Subcritical water chromotagraphy tremella polysaccharide of lower solid-to-liquid ratio, not only increase the space availability ratio that extraction kettle uses, and the volume of extraction kettle is too large without the need to design, also reduce consumption and the energy consumption of subcritical water, equipment manufacturing cost and running cost are all lower.
3, the valve bottom extraction kettle of the present invention is connected with the opening for feed of stirred pot, subcritical water extract is without the need to cooling the stirred pot directly put into and deionized water is housed in advance, subcritical water is utilized to have very high heat energy, the deionized water of heating and stirring tank, both the extraction temperature of deionized water had been improved, reclaim subcritical water heat energy again, reach energy-saving and cost-reducing object.
4, the present invention not only increases the space availability ratio that extraction kettle uses, reduce consumption and the energy consumption of subcritical water, and the extraction yield of tremella polysaccharide is also higher than traditional extracting method, use the technique of Subcritical water chromotagraphy tremella polysaccharide, equipment, economy and efficiency can both meet the requirement of suitability for industrialized production.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail, but they are not limitation of the present invention.
Determination of polysaccharide of the present invention adopts phenol-sulfuric acid and colorimetric method, polysaccharide yield (%)=polysaccharide quality/raw material dry mass × 100%.
Embodiment 1
Get 20 object white fungus dry powder 50kg and be placed in extraction kettle, add 1000L and add deionized water, be heated to 120 DEG C, after insulation 60min, open extraction kettle bottom valve, subcritical water extract is put into the stirred pot that 1500L deionized water is housed in advance, after stirring and dissolving 1h, coarse filtration, filtrate is with the centrifugal 10min of 4000r/min, the ultra-filtration membrane of supernatant liquor 10kD molecular weight cut-off is concentrated into 300L, add 95% ethanol, its final concentration is made to be 70%, after stirring, staticly settle 10h, throw out is with after 300L deionized water dissolving, on the anion-exchange resin column of anticipating, add 1800L deionized water wash-out, remove the impurity such as protein and pigment, collect polysaccharide effluent liquid, 300L is concentrated into the ultra-filtration membrane of 10kD molecular weight cut-off, add 98% ethanol, its final concentration is made to be 70%, after stirring, staticly settle 10h, throw out absolute ethanol washing 2 times, lyophilize, obtain the tremella polysaccharide of 19.5kg white powder, polysaccharide content is 74.2%, polysaccharide yield is 28.9%.
Embodiment 2
Get 60 object white fungus dry powder 100kg and be placed in extraction kettle, add 1500L and add deionized water, be heated to 140 DEG C, after insulation 10min, open extraction kettle bottom valve, subcritical water extract is put into the stirred pot that 3000L deionized water is housed in advance, after stirring and dissolving 1.5h, coarse filtration, filtrate is with the centrifugal 10min of 3000r/min, the ultra-filtration membrane of supernatant liquor 50kD molecular weight cut-off is concentrated into 400L, add dehydrated alcohol, its final concentration is made to be 70%, after stirring, staticly settle 8h, throw out absolute ethanol washing 2 times, vacuum-drying, obtain 54.8kg gray powdery tremella polysaccharide, polysaccharide content is 61.7%, polysaccharide yield is 33.8%.
Embodiment 3
Get 40 object white fungus dry powder 50kg and be placed in extraction kettle, add 1000L and add deionized water, be heated to 130 DEG C, after insulation 20min, open extraction kettle bottom valve, subcritical water extract is put into the stirred pot that 1500L deionized water is housed in advance, after stirring and dissolving 1h, coarse filtration, filtrate is concentrated into original volume 1/15 with the ultra-filtration membrane of the centrifugal 10min of 4000r/min, supernatant liquor 5kD molecular weight cut-off, obtains 241L tremella polysaccharide concentrated solution, polysaccharide content is 84.6g/L, and polysaccharide yield is 40.8%.
Comparative example 4
Get 40 object white fungus dry powder 10kg and be placed in extraction kettle, add 600L and add deionized water, be heated to 130 DEG C, after insulation 20min, open extraction kettle bottom valve, cooling and coarse filtration after, be concentrated into original volume 1/15 with the ultra-filtration membrane of the centrifugal 10min of 4000r/min, supernatant liquor 5kD molecular weight cut-off, obtain the milky tremella polysaccharide concentrated solution of 31L, polysaccharide content is 80.5g/L, and polysaccharide yield is 41.1%.
Comparative example 5
Get 40 object white fungus dry powder 10kg and be placed in extractor, add 800L and add deionized water, be heated to 90 DEG C, after backflow 6h, open extractor bottom valve, cooling and coarse filtration after, be concentrated into original volume 1/15 with the ultra-filtration membrane of the centrifugal 10min of 4000r/min, supernatant liquor 5kD molecular weight cut-off, obtain 47L tremella polysaccharide concentrated solution, polysaccharide content is 57.0g/L, and polysaccharide yield is 26.8%.
Table 1: several Different Extraction Method tremella polysaccharide extracts yield and compares
From table 1, Subcritical Water Extraction of the present invention-hot water extraction's two-step approach extraction process and Subcritical Water Extraction method extraction process are compared with atmospheric hot-water restricted-access media technique, not only obviously shorten the extraction time of tremella polysaccharide, and significantly improve the extraction yield of tremella polysaccharide.And Subcritical Water Extraction-hot water extraction's two-step approach extraction process is compared with Subcritical Water Extraction method extraction process, the extraction yield of tremella polysaccharide is close, but due to have employed lower solid-to-liquid ratio subcritical water, not only increase the space availability ratio that extraction kettle uses, and reduce consumption and the energy consumption of subcritical water, equipment manufacturing cost and running cost obviously reduce, and make the technique of Subcritical water chromotagraphy tremella polysaccharide, equipment, economy and efficiency can meet the requirement of suitability for industrialized production.
Claims (1)
1. adopt Subcritical Water Extraction-hot water extraction's two-step approach to extract a production method for tremella polysaccharide, it is characterized in that, it is as follows that the method comprising the steps of:
1) low solid-to-liquid ratio Subcritical Water Extraction: being dropped in subcritical abstraction still by the white fungus dry powder pulverized, is that 1:10-20 kg/L adds deionized water by solid-to-liquid ratio, Extracting temperature 100-150 DEG C, extraction time 10-120 min;
2) deionized water stripping tremella polysaccharide: stirred pot drops into quality for benchmark with white fungus dry powder in advance, be that 1:20-30 kg/L adds deionized water by solid-to-liquid ratio, after step 1) extraction terminates, open extraction kettle bottom valve, subcritical water extract is directly put into stirred pot, after stirring and dissolving is abundant, coarse filtration;
3) by step 2) filtrate of stirred pot is concentrated into the 1/2-1/20 of original volume with the ultra-filtration membrane of the centrifugal 10-20 min of rotating speed 3000-5000 r/min, supernatant liquor 3-50 kD molecular weight cut-off, and obtain tremella polysaccharide and slightly carry concentrated solution;
4) step 3) tremella polysaccharide is slightly carried concentrated solution and add 95-100 %vt ethanol, make ultimate density be 70 %wt, after stirring, staticly settle 6-12 h, throw out absolute ethanol washing 1-3 time, vacuum or lyophilize, obtain white fungus Crude polysaccharides;
5) step 4) throw out being added deionized water, to be mixed with polysaccharide content be the 5-10% kg/L aqueous solution, upper anion-exchange resin column, remove the impurity such as protein and pigment, collect polysaccharide effluent liquid, the 1/2-1/20 of original volume is concentrated into the ultra-filtration membrane of 3-50 kD molecular weight cut-off, repeating step 4), obtain the tremella polysaccharide refined.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107759706A (en) * | 2016-08-15 | 2018-03-06 | 黄祖威 | A kind of technology that ground method extraction tremella polysaccharides is boiled with physical heating |
| TWI750084B (en) * | 2021-04-23 | 2021-12-11 | 樂活生技開發股份有限公司 | Method of extracting active ingredients in mushrooms |
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| TWI750084B (en) * | 2021-04-23 | 2021-12-11 | 樂活生技開發股份有限公司 | Method of extracting active ingredients in mushrooms |
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