CN101780118A - Method for extracting active ingredients of artificially cultured cordceps militaris waste liquor by flocculation - Google Patents
Method for extracting active ingredients of artificially cultured cordceps militaris waste liquor by flocculation Download PDFInfo
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- CN101780118A CN101780118A CN200910045487A CN200910045487A CN101780118A CN 101780118 A CN101780118 A CN 101780118A CN 200910045487 A CN200910045487 A CN 200910045487A CN 200910045487 A CN200910045487 A CN 200910045487A CN 101780118 A CN101780118 A CN 101780118A
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Abstract
The invention relates to a method for extracting active ingredients of artificially cultured cordceps militaris waste liquor by flocculation, which comprises the following steps: dissolving a flocculating agent in water, wherein the mass concentration of the flocculating agent is 0.5 to 5 percent; and adjusting the pH value of the solution with acetic acid or sodium hydroxide to 3 to 9; adding the cordceps militaris waste liquor in a container at the temperature of 20 to 30 DEG C, adding the prepared flocculating agent solution into the container, and stirring at the stirring speed of 40 to 80r/min for 10 to 60min; stopping stirring, and standing the solution for 2 to 4 hours to completely settle the flocculation; removing the supernatant, centrifugalizing the flocculation, taking out a sediment containing relatively little water, and further processing the sediment; and processing the sediment to obtain a polysaccharide product. The method of the invention has the following advantages that: the processing step is simple and quick; the reclaimed products are rich and diversified; the flocculating property of the flocculating agent is strong; and the flocculation is easily separated.
Description
[technical field]
The present invention relates to Cordyceps waste liquid technical field, specifically, is the flocculation extracting method of effective ingredient in a kind of artificial culture Cordyceps militaris (L.) Link. waste liquid.
[background technology]
Contain abundant Cordycepin, protein, aminoacid, D～mannitol, Cordyceps polysaccharide etc. in the Cordyceps fermentation liquid, Cordyceps polysaccharide biological activity wherein is strong, adapts to widely, has very high value of exploiting and utilizing.Owing to contain a large amount of Organic substances, thus the Cordyceps waste liquid COD value up to 25000, this has increased the difficulty that disposes waste liquid.Therefore seek a kind of can high efficiency extraction Cordyceps waste liquid in the method for effective ingredient, not only can improve economic benefit of enterprises, and environmental conservation is also had positive effect.
Utilize the effective ingredient in the flocculating agent extraction Cordyceps waste liquid, comprise acrylamide series flocculating agent, microbial flocculant, organic many living polymers flocculating agent, aluminium porcelain enamelling flocculating agent, iron preparation flocculating agent, natural organic high-molecular flocculant.They all have certain sedimentation capacity to the Organic substance in the waste liquid, and wherein the iron preparation flocculating agent has edibility, can replenish the trace iron that human body needs; Chitosan has strong biological activity in the natural macromolecule flocculating agent, and is on probation wide, has excellent application value.
Chinese patent publication number 200710067315.8 discloses macroporous adsorbent resin reclaims adenosine from low concentration Chinese caterpillar fungus fermentation waste water method, and method step is as follows: the Cordyceps waste liquid is removed by filter insoluble granule; Pack in chromatographic column through pretreated macroporous adsorbent resin, the resin column ratio of height to diameter is 2～10; Chinese caterpillar fungus fermentation waste liquid after the filtration is crossed chromatographic column with the flow velocity of 0.5～3 bed volume/h, and adenosine penetrates to the effluent; With the flow velocity eluting adenosine of organic solvent-water mixed flow with 0.5～3 bed volume/h, eluent merges behind thin-layer chromatographic analysis, again through concentrate, after the crystallization the product adenosine, resin column can reuse after organic solvent-water flushing regeneration respectively.
[summary of the invention]
The objective of the invention is to overcome the deficiencies in the prior art, the flocculation extracting method of effective ingredient in a kind of artificial culture Cordyceps militaris (L.) Link. waste liquid is provided.
The objective of the invention is to be achieved through the following technical solutions:
(1) flocculating agent is dissolved in the water, the flocculating agent mass fraction is 0.5～5%, can adopt the pH value of acetic acid or sodium hydrate regulator solution according to the difference of flocculating agent, is 3～9;
Described flocculating agent is selected from acrylamide series flocculating agent, microbial flocculant, organic many living polymers flocculating agent, aluminium porcelain enamelling flocculating agent, chitosan flocculant, a kind of in iron preparation flocculating agent or the natural organic high-molecular flocculant;
Described flocculating agent is preferably chitosan and iron preparation flocculating agent;
(2) be under 20～30 ℃ in temperature, the Cordyceps waste liquid is placed container, add deployed flocculant solution, the mass fraction that flocculating agent accounts for solution is 1: 100～1: 1000, further stir, mixing speed is 40～80r/min, and mixing time is 10～60 minutes, make flocculating agent fully contact, reach better flocculating effect with macromole in the waste liquid;
(3) stop to stir, static 2～4 hours, make flocculation sediment complete; Supernatant is removed, and flco is by centrifugalize, and the moisture less precipitation that obtains is removed, and does further processing;
(4) precipitation that obtains of step (3) is handled, obtained polyose, described processing method is a spray drying, oven dry, extraction, a kind of in the adsorption method;
For the situation that adopts chitosan and iron preparation flocculating agent, the precipitation that obtains of step (3) is directly carried out spray drying or oven dry, obtain polyose.
Compared with prior art, good effect of the present invention is:
(1) treatment step simple and fast of the present invention reclaims rich choice of products, and is various;
(2) the flocculating agent flocculation ability of the present invention's employing is strong, and flco separates easily, and this has very strong realistic meaning to handling a large amount of Cordyceps waste liquids;
(3) chitosan flocculant of the present invention's employing has multiple functions such as the immunity of raising, activating cell, prophylaxis of cancer, blood fat reducing, blood sugar regulation, adjusting body environment; This can increase beneficiating ingredient in the Cordyceps waste liquid precipitum, and the value that improves precipitum is had positive effect.
[description of drawings]
Fig. 1 process chart of the present invention;
The former waste liquid chromatogram of Fig. 2;
Fig. 3 supernatant chromatogram.
[specific embodiment]
The specific embodiment of the flocculation extracting method that the present invention manually cultivates effective ingredient in the Cordyceps militaris (L.) Link. waste liquid below is provided.
Embodiment 1
Use the method that chitosan flocculant extracts effective ingredient in the Cordyceps waste liquid
The chitosan molecule formula is (C
6H
11NO
4)
n, structural formula is:
(1) 1 gram chitosan is dissolved in the 100ml1% acetic acid solution, the pH value of regulator solution is 5～6;
(2) be under 25 ℃ in temperature, the Cordyceps waste liquid is placed container, add deployed flocculant solution, the mass fraction that adds is 500: 1, further stir, mixing speed is 60r/min, and mixing time is 30 minutes, make flocculating agent fully contact, reach better flocculating effect with macromole in the waste liquid;
(3) stop to stir, static 3 hours, make flocculation sediment complete; Supernatant is removed, and flco is by centrifugalize, and the moisture less precipitation that obtains is removed, and does further processing;
(4) for the situation that adopts chitosan and iron preparation flocculating agent, the precipitation that obtains of step (3) is directly carried out spray drying or oven dry, obtain polyose;
The result:
Get supernatant 100ml dry 1.0～1.5 the gram light brown product; 1000ml Cordyceps waste liquid gained precipitum is dried under 90～95 degrees centigrade condition, get 3.0～3.5 gram dark brown products.
High performance liquid chromatogram detects the contained effective ingredient of Cordyceps waste liquid:
Condition: wavelength is 214nm; Mobile phase A is a ultra-pure water; Mobile phase B is 10% isopropyl alcohol～acetonitrile solution;
Gradient condition: 0～5min:100%A; 5～35min:0～85%B; 35～45:85%～85%B; 45～55:100%A;
High performance liquid chromatogram detects contained effective ingredient in the supernatant:
Condition: wavelength is 214nm; Mobile phase A is a ultra-pure water; Mobile phase B is 10% isopropyl alcohol～acetonitrile solution;
Gradient condition: 0～5min:100%A; 5～35min:0～85%B; 35～45:85%～85%B; 45～55:100%A;
Comparative drawings figs 1 and accompanying drawing 2,60%～70% saccharide and protein are settled down in the Cordyceps waste liquid as can be known;
The result
Cordyceps polysaccharide and protein equal size are 90～98% in the oven dry product, have very high value; The Cordyceps waste liquid COD value drops to about 2000 by 25000, reduces treatment cost of waste liquor greatly.Therefore, use flocculating agent especially chitosan flocculant extract that effective ingredient is the very wide method of a kind of prospect in the Cordyceps waste liquid.
The above only is a preferred implementation of the present invention; should be pointed out that for those skilled in the art, without departing from the inventive concept of the premise; can also make some improvements and modifications, these improvements and modifications also should be considered within the scope of protection of the present invention.
Claims (3)
1. the flocculation extracting method of effective ingredient in the artificial culture Cordyceps militaris (L.) Link. waste liquid is characterized in that concrete steps are:
(1) flocculating agent is dissolved in the water, the flocculating agent mass fraction is 0.5%～5%, adopts the pH value of acetic acid or sodium hydrate regulator solution, is 3～9;
Described flocculating agent is selected from acrylamide series flocculating agent, microbial flocculant, organic many living polymers flocculating agent, aluminium porcelain enamelling flocculating agent, chitosan flocculant, a kind of in iron preparation flocculating agent or the natural organic high-molecular flocculant;
(2) be under 20～30 ℃ in temperature, the Cordyceps waste liquid is placed container, add deployed flocculant solution, the mass fraction that flocculating agent accounts for solution is 1: 100～1: 1000, further stir, mixing speed is 40～80r/min, and mixing time is 10～60 minutes;
(3) stop to stir, static 2～4 hours, make flocculation sediment complete; Supernatant is removed, and flco is by centrifugalize, and the moisture less precipitation that obtains is removed, and does further processing;
(4) precipitation that step (3) is obtained is handled, and obtains polyose, and described processing method is a spray drying, oven dry, extraction, a kind of in the adsorption method.
2. the flocculation extracting method of effective ingredient is characterized in that in the artificial culture Cordyceps militaris (L.) Link. waste liquid as claimed in claim 1, and in described step (1), described flocculating agent is chitosan or iron preparation flocculating agent.
3. the flocculation extracting method of effective ingredient is characterized in that in the artificial culture Cordyceps militaris (L.) Link. waste liquid as claimed in claim 1, when flocculating agent is chitosan or iron preparation flocculating agent, described precipitation treatment method be spray drying or the oven dry in a kind of.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 200910045487 CN101780118B (en) | 2009-01-19 | 2009-01-19 | Method for extracting active ingredients of artificially cultured cordceps militaris waste liquor by flocculation |
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| CN 200910045487 CN101780118B (en) | 2009-01-19 | 2009-01-19 | Method for extracting active ingredients of artificially cultured cordceps militaris waste liquor by flocculation |
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| CN101780118A true CN101780118A (en) | 2010-07-21 |
| CN101780118B CN101780118B (en) | 2013-04-24 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103445229A (en) * | 2013-09-09 | 2013-12-18 | 南京农业大学 | Method for simultaneously and effectively removing laver protein and laver polysaccharide from laver extracting solution |
| CN107011451A (en) * | 2016-04-25 | 2017-08-04 | 上海辉文生物技术股份有限公司 | White fungus different poly- polysaccharide and its extract, preparation method and application |
| CN117801965A (en) * | 2024-02-29 | 2024-04-02 | 南京师范大学 | Method for preparing biological sponge for adsorbing sewage by using cordyceps militaris and application of biological sponge |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1177925C (en) * | 2001-08-13 | 2004-12-01 | 沈阳联美植物细胞工程有限公司 | Fermenting culture process of produicng Cordyceps extract |
| CN100469785C (en) * | 2007-02-12 | 2009-03-18 | 浙江大学 | Method of reclaiming adenosine from low concentration Chinese caterpillar fungus fermentation waste water by large aperture adsorption resin |
-
2009
- 2009-01-19 CN CN 200910045487 patent/CN101780118B/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103445229A (en) * | 2013-09-09 | 2013-12-18 | 南京农业大学 | Method for simultaneously and effectively removing laver protein and laver polysaccharide from laver extracting solution |
| CN107011451A (en) * | 2016-04-25 | 2017-08-04 | 上海辉文生物技术股份有限公司 | White fungus different poly- polysaccharide and its extract, preparation method and application |
| CN107011451B (en) * | 2016-04-25 | 2019-11-08 | 上海辉文生物技术股份有限公司 | The different poly- polysaccharide of tremella and its extract, preparation method and application |
| CN117801965A (en) * | 2024-02-29 | 2024-04-02 | 南京师范大学 | Method for preparing biological sponge for adsorbing sewage by using cordyceps militaris and application of biological sponge |
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| CN101780118B (en) | 2013-04-24 |
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