CN105348404A - Method for extracting flammulina velutipes polysaccharide from flammulina velutipes - Google Patents
Method for extracting flammulina velutipes polysaccharide from flammulina velutipes Download PDFInfo
- Publication number
- CN105348404A CN105348404A CN201510735327.8A CN201510735327A CN105348404A CN 105348404 A CN105348404 A CN 105348404A CN 201510735327 A CN201510735327 A CN 201510735327A CN 105348404 A CN105348404 A CN 105348404A
- Authority
- CN
- China
- Prior art keywords
- washing
- needle mushroom
- flammulina velutipes
- adsorbent resin
- macroporous adsorbent
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0003—General processes for their isolation or fractionation, e.g. purification or extraction from biomass
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
Abstract
The invention discloses a method for extracting flammulina velutipes polysaccharide from flammulina velutipes. The method comprises 1, carrying out extraction on flammulina velutipes by a hydrochloric acid solution with a mass fraction of 0.25-0.35% at a temperature of 30-40 DEG C for 1-3h to obtain extract, 2, adding base into the extract to adjust pH to 7.5-8.0, and carrying out solid-liquid separation to remove insoluble substances and to obtain a clear aqueous solution A, 3, adding an acid into the aqueous solution A to adjust pH to 4.0-4.5 and carrying out solid-liquid separation to remove insoluble substances and to obtain a clear aqueous solution B, 4, adding the aqueous solution B into a macroporous adsorption resin column, washing the macroporous adsorption resin column by water to remove un-adsorbed impurities, washing the macroporous adsorption resin column by an ethanol solution with a volume fraction of 15-20% to remove high-polarity impurities, washing the macroporous adsorption resin column by an ethanol solution with a volume fraction of 65-70% as a desorption solution, collecting the desorption solutions obtained by washing, carrying out vacuum concentration and carrying out drying to obtain flammulina velutipes extract. The method has reasonable processes, high extraction efficiency and simple processes and is suitable for industrial production.
Description
Technical field
The present invention relates to a kind of method extracting flammulina velutipes from needle mushroom, the present invention relates to biomedicine field.
Background technology
Needle mushroom formal name used at school hair handle money bacterium (Flammulinavelutipes), also known as the little fiery mushroom of hair handle, structure bacterium, plain mushroom, dried mushroom, plain wild rice, freezes bacterium, golden mushroom, intelligence mushroom etc.
The amino acid whose content of needle mushroom is very abundant, and higher than general mushroom class, especially the content of Methionin is high especially, and Methionin has the function promoting children ' s intelligence development.Containing protein 8.87% in needle mushroom dry product, carbohydrate 60.2%, robust fibre reaches 7.4%, often eats and can prevent and treat Peptic Ulcers.
Also containing a kind of polysaccharide material being Flammulin in needle mushroom, have enhancing body to the resist ability of cancer cells, research finds, the Flammulin contained in needle mushroom, has obvious restraining effect to small white mouse sarcoma S-180, ehrlich's ascite cell etc.
At present, mainly concentrate protein-based both at home and abroad to the report of needle mushroom, the extraction research carried out flammulina velutipes in needle mushroom is also less.
Summary of the invention
The technical problem that the present invention solves is, conveniently, from needle mushroom, extracts flammulina velutipes economically, improves the content of flammulina velutipes in gold needle mushroom extract.
Technical scheme of the present invention is, provides a kind of method extracting flammulina velutipes from needle mushroom, comprises the following steps:
(1) be that the hydrochloric acid soln of 0.25-0.35% extracts needle mushroom 1-3h at 30-40 DEG C with massfraction, the mass ratio of hydrochloric acid soln and needle mushroom is 3-5:1, obtains extracting solution;
(2) described extracting solution is added alkali adjust ph to 7.5-8.0, then solid-liquid separation removing insolubles, obtain the water-soluble of clarification
Liquid A;
(3) in described water solution A, acid for adjusting pH value is added to 4.0-4.5, then solid-liquid separation removing insolubles, obtain clarification
Aqueous solution B;
(4) described aqueous solution B is joined in 100L macroporous adsorptive resins with the flow velocity of 50-100L/h, first remove not by the impurity adsorbed with the flow velocity of 100-200L/h washing macroporous adsorbent resin with water; By volume fraction be again the ethanolic soln of 15-20% with the flow velocity of 30-50L/h washing macroporous adsorbent resin except the higher impurity of depolarization; By volume fraction be again the ethanolic soln of 65-70% as stripping liquid with the flow velocity of 40-60L/h washing macroporous adsorbent resin, collect the stripping liquid after washing, through concentrating under reduced pressure, dry gold needle mushroom extract.
Further, in step (1), the massfraction of described hydrochloric acid soln is 0.3%.
Further, described solid-liquid separation is filtration or centrifugal.
Further, described macroporous adsorbent resin is intermediate-polarity macroporous adsorption resin.
Further, described macroporous adsorbent resin is AB-8 macroporous adsorbent resin.
Further, described acid is acetic acid.
Further, described alkali is calcium hydroxide.
Further, in described step (4), the temperature of concentrating under reduced pressure is 60-65 DEG C.
Further, described drying is vacuum-drying or spraying dry, and the moisture being dried to gold needle mushroom extract is no more than 5%.
Further, before described step (1), needle mushroom is crushed to below 0.5cm.
The usual employing of current similar substance be alcohol extracting, cost is high, removing impurity is precipitated for a long time with low temperature after concentrated, major defect is temperature requirement high (about 4 DEG C), time length (leaving standstill 12-48 hour), Impurity removal are incomplete, thus cause that the production cycle produces, cost is high, and active constituent content low, be difficult to industrialization.The advantage that the present invention gives prominence to is, employing aqueous hydrochloric acid extracts, cost is low, and do not need to concentrate, technique is simply coherent, alkali adjust ph is directly added to 7.5-8.0 after extracting solution solid-liquid separation, can precipitate rapidly under weakly alkaline at the impurity that acidic conditions is solvable in solution, add acetic acid adjust ph to 4.0-4.5, can precipitate rapidly under slightly acidic at the impurity that weak basic condition is solvable in solution, do not need low temperature to leave standstill for a long time, then can dilute, be separated immediately by normal temperature, greatly shorten the production cycle.Re-use and obtain macroporous adsorptive resins separation on acidic aqueous solution, the impurity of strong polarity cannot adsorb on resin, then adopts the washing with alcohol of 15-20% to remove the impurity of middle polarity, and Impurity removal is complete, and product effective constituent is high.Extracting method conventional at present, in extract, the content of target product is generally 5%, and uses method of the present invention, and in extract, the content of flammulina velutipes can reach 40-60%.The product that the present invention prepares is mainly used in dietary supplements, dietary supplements.
Advantage of the present invention is:
1, in present method, the extraction continuity of flammulina velutipes is good, and technique is simple, is applicable to commercial introduction.
2, present method rational technology, active constituent content is high, extraction efficiency is high, simple to operate, be applicable to suitability for industrialized production.
3, the extract purity prepared by the present invention is stablized, and flammulina velutipes content is between 40-60%.
4, preparation method's yield of the present invention is high; Solvent can recycling.
Embodiment
embodiment 1
Take dry needle mushroom 100kg and be crushed to below 0.5cm, drop in extractor, and add 0.3% hydrochloric acid soln 500L, open stirring; Open jacket steam when being heated to 40 DEG C, start timing, extract 3h, feed liquid crosses 400 order filter bags; After refluxing extraction, feed liquid crosses 400 order filter bags, filtrate adding calcium hydroxide adjust ph to 7.5, centrifugation; Centrifugal clear liquid adds acetic acid adjust ph to 5.0, centrifugation; The centrifugal stillness of night joins in 100L macroporous adsorptive resins with the flow velocity of 80L/h, first removes not by the impurity adsorbed with the flow velocity of 120L/h washing macroporous adsorbent resin with water; By volume fraction be again 15% ethanolic soln with the flow velocity of 45L/h washing macroporous adsorbent resin except the higher impurity of depolarization; By volume fraction be again 65% ethanolic soln as stripping liquid with the flow velocity of 50L/h washing macroporous adsorbent resin, collect the stripping liquid after washing, through concentrating under reduced pressure, dry gold needle mushroom extract, flammulina velutipes content is 59.7%.
embodiment 2
Take dry needle mushroom 100kg and be crushed to below 0.5cm, drop in extractor, and add 0.25% hydrochloric acid soln 300L, open stirring; Open jacket steam when being heated to 30 DEG C, start timing, extract 2h, feed liquid crosses 400 order filter bags; After refluxing extraction, feed liquid crosses 400 order filter bags, filtrate adding calcium hydroxide adjust ph to 8.0, centrifugation; Centrifugal clear liquid adds acetic acid adjust ph to 4.5, centrifugation; The centrifugal stillness of night joins in 100L macroporous adsorptive resins with the flow velocity of 50L/h, first removes not by the impurity adsorbed with the flow velocity of 100L/h washing macroporous adsorbent resin with water; By volume fraction be again 15% ethanolic soln with the flow velocity of 30L/h washing macroporous adsorbent resin except the higher impurity of depolarization; By volume fraction be again 70% ethanolic soln as stripping liquid with the flow velocity of 40L/h washing macroporous adsorbent resin, collect the stripping liquid after washing, through concentrating under reduced pressure, dry gold needle mushroom extract, flammulina velutipes content is 42.8%.
embodiment 3
Take dry needle mushroom 100kg and be crushed to below 0.5cm, drop in extractor, and add 0.35% hydrochloric acid soln 400L, open stirring; Open jacket steam when being heated to 35 DEG C, start timing, extract 1h, feed liquid crosses 400 order filter bags; After refluxing extraction, feed liquid crosses 400 order filter bags, filtrate adding calcium hydroxide adjust ph to 7.8, centrifugation; Centrifugal clear liquid adds acetic acid adjust ph to 4.8, centrifugation; The centrifugal stillness of night joins in 100L macroporous adsorptive resins with the flow velocity of 100L/h, first removes not by the impurity adsorbed with the flow velocity of 200L/h washing macroporous adsorbent resin with water; By volume fraction be again 20% ethanolic soln with the flow velocity of 50L/h washing macroporous adsorbent resin except the higher impurity of depolarization; By volume fraction be again 65% ethanolic soln as stripping liquid with the flow velocity of 60L/h washing macroporous adsorbent resin, collect the stripping liquid after washing, through concentrating under reduced pressure, dry gold needle mushroom extract 312g, flammulina velutipes content is 54.5%.
Claims (10)
1. from needle mushroom, extract a method for flammulina velutipes, it is characterized in that, comprise the following steps:
(1) be that the hydrochloric acid soln of 0.25-0.35% extracts needle mushroom 1-3h at 30-40 DEG C with massfraction, the mass ratio of hydrochloric acid soln and needle mushroom is 3-5:1, obtains extracting solution;
(2) described extracting solution is added alkali adjust ph to 7.5-8.0, then solid-liquid separation removing insolubles, obtain the water-soluble of clarification
Liquid A;
(3) in described water solution A, acid for adjusting pH value is added to 4.0-4.5, then solid-liquid separation removing insolubles, obtain clarification
Aqueous solution B;
(4) described aqueous solution B is joined in 100L macroporous adsorptive resins with the flow velocity of 50-100L/h, first remove not by the impurity adsorbed with the flow velocity of 100-200L/h washing macroporous adsorbent resin with water; By volume fraction be again the ethanolic soln of 15-20% with the flow velocity of 30-50L/h washing macroporous adsorbent resin except the higher impurity of depolarization; By volume fraction be again the ethanolic soln of 65-70% as stripping liquid with the flow velocity of 40-60L/h washing macroporous adsorbent resin, collect the stripping liquid after washing, through concentrating under reduced pressure, dry gold needle mushroom extract.
2. the method for claim 1, is characterized in that, in step (1), the massfraction of described hydrochloric acid soln is 0.3%.
3. the method for claim 1, is characterized in that, described solid-liquid separation is filtration or centrifugal.
4. the method for claim 1, is characterized in that, described macroporous adsorbent resin is intermediate-polarity macroporous adsorption resin.
5. the method for claim 1, is characterized in that, described macroporous adsorbent resin is AB-8 macroporous adsorbent resin.
6. the method for claim 1, is characterized in that, described acid is acetic acid.
7. the method for claim 1, is characterized in that, described alkali is calcium hydroxide.
8. the method for claim 1, is characterized in that, in described step (4), the temperature of concentrating under reduced pressure is 60-65 DEG C.
9. the method for claim 1, is characterized in that, described drying is vacuum-drying or spraying dry, is dried to
The moisture of gold needle mushroom extract is no more than 5%.
10. the method for claim 1, is characterized in that, before described step (1), is crushed to by needle mushroom
Below 5cm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510735327.8A CN105348404A (en) | 2015-11-03 | 2015-11-03 | Method for extracting flammulina velutipes polysaccharide from flammulina velutipes |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510735327.8A CN105348404A (en) | 2015-11-03 | 2015-11-03 | Method for extracting flammulina velutipes polysaccharide from flammulina velutipes |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105348404A true CN105348404A (en) | 2016-02-24 |
Family
ID=55324482
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510735327.8A Pending CN105348404A (en) | 2015-11-03 | 2015-11-03 | Method for extracting flammulina velutipes polysaccharide from flammulina velutipes |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105348404A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110563856A (en) * | 2019-10-29 | 2019-12-13 | 沈阳翔源科技有限公司 | extraction method of flammulina velutipes polysaccharide |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104940246A (en) * | 2015-07-17 | 2015-09-30 | 湖南杰萃生物技术有限公司 | Method for extracting coprinus comatus extractive from coprinus comatus |
-
2015
- 2015-11-03 CN CN201510735327.8A patent/CN105348404A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104940246A (en) * | 2015-07-17 | 2015-09-30 | 湖南杰萃生物技术有限公司 | Method for extracting coprinus comatus extractive from coprinus comatus |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110563856A (en) * | 2019-10-29 | 2019-12-13 | 沈阳翔源科技有限公司 | extraction method of flammulina velutipes polysaccharide |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104940246B (en) | A method of extracting coprinus comatus element from coprinus comatus | |
| CN102702163B (en) | Method for preparing high-purity monomer epigallocatechin gallate from processed leftovers of tea leaves | |
| CN103289430A (en) | Method for extracting and purifying anthocyanins from blueberry pomaces | |
| CN102011337B (en) | Preparation method of modified bentonite particle retention aid for papermaking | |
| CN101525306A (en) | Method for extracting and separating natural taurine from octopus leftovers | |
| CN103980121B (en) | Method for producing chlorogenic acids from fresh eucommia leaves | |
| CN104326912B (en) | A kind of separation method of tobacco leaf effective constituent | |
| CN102993154A (en) | Method for extracting purple sweet potato anthocyanin | |
| CN103509028B (en) | The preparation method of a kind of chlorophyll cupric acid and copper sodium | |
| CN104448020A (en) | Method for extracting and purifying lentinan | |
| CN104418743B (en) | A kind of method of slightly getting refining chlorogenic acid thing from Japanese Honeysuckle | |
| CN102675910B (en) | Preparation method of high-color-value beet root red color | |
| CN102060856B (en) | Method for extracting tabersonine from voacanga seeds | |
| CN102249961A (en) | Method for extracting alliin from garlic | |
| CN102633764A (en) | Production process for preparing anthocyanin and pectin by black soya bean hull | |
| CN105267254A (en) | Method of extracting Collybia albuminosa polysaccharide from Collybia albuminosa | |
| CN105348404A (en) | Method for extracting flammulina velutipes polysaccharide from flammulina velutipes | |
| CN104119229A (en) | Technology for producing pure chlorogenic acid | |
| CN104926719A (en) | Method for extracting gynesine from fructus cannabis | |
| CN105273099A (en) | Method for extracting straw mushroom polysaccharide from straw mushrooms | |
| CN104945450A (en) | Method for extracting stibene glucoside from vines of multiflower knotweeds | |
| CN103289969A (en) | Method for extracting superoxide dismutase from plant stem leaves | |
| CN103058882B (en) | Method for separating natural theanine | |
| CN105273102A (en) | Method for extracting auricularia auricula polysaccharide from auricularia auricula | |
| CN113164428A (en) | Preparation method of red perilla leaf extract |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20160224 |