CN110467684A - A kind of method of cation macroreticular resin purification Blackfungus polyhexose - Google Patents
A kind of method of cation macroreticular resin purification Blackfungus polyhexose Download PDFInfo
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- 239000011347 resin Substances 0.000 title claims abstract description 53
- 229920005989 resin Polymers 0.000 title claims abstract description 53
- 238000000034 method Methods 0.000 title claims abstract description 28
- 150000001768 cations Chemical class 0.000 title claims abstract description 23
- 238000000746 purification Methods 0.000 title abstract description 7
- 241000233866 Fungi Species 0.000 claims abstract description 46
- 235000009508 confectionery Nutrition 0.000 claims abstract description 45
- 238000000502 dialysis Methods 0.000 claims abstract description 23
- 239000002994 raw material Substances 0.000 claims abstract description 21
- 150000003384 small molecules Chemical class 0.000 claims abstract description 11
- 238000009777 vacuum freeze-drying Methods 0.000 claims abstract description 11
- 238000003809 water extraction Methods 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 42
- 150000004676 glycans Chemical class 0.000 claims description 25
- 229920001282 polysaccharide Polymers 0.000 claims description 25
- 239000005017 polysaccharide Substances 0.000 claims description 25
- 239000012153 distilled water Substances 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 10
- 238000000605 extraction Methods 0.000 claims description 8
- 238000004587 chromatography analysis Methods 0.000 claims description 6
- 239000000706 filtrate Substances 0.000 claims description 6
- 235000011389 fruit/vegetable juice Nutrition 0.000 claims description 6
- 239000008399 tap water Substances 0.000 claims description 6
- 235000020679 tap water Nutrition 0.000 claims description 6
- 238000002360 preparation method Methods 0.000 claims description 5
- 238000007670 refining Methods 0.000 claims description 4
- 241000487918 Acacia argyrodendron Species 0.000 claims description 3
- 235000011222 chang cao shi Nutrition 0.000 claims description 3
- 238000012545 processing Methods 0.000 claims description 3
- 125000002091 cationic group Chemical group 0.000 abstract description 2
- 239000012535 impurity Substances 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 102000004169 proteins and genes Human genes 0.000 description 12
- 108090000623 proteins and genes Proteins 0.000 description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 5
- 238000009835 boiling Methods 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 4
- 230000014759 maintenance of location Effects 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 241000221377 Auricularia Species 0.000 description 3
- 230000002378 acidificating effect Effects 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000003463 adsorbent Substances 0.000 description 2
- 230000001093 anti-cancer Effects 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 238000005342 ion exchange Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000049 pigment Substances 0.000 description 2
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 1
- QCVGEOXPDFCNHA-UHFFFAOYSA-N 5,5-dimethyl-2,4-dioxo-1,3-oxazolidine-3-carboxamide Chemical compound CC1(C)OC(=O)N(C(N)=O)C1=O QCVGEOXPDFCNHA-UHFFFAOYSA-N 0.000 description 1
- 241000221198 Basidiomycota Species 0.000 description 1
- 102000002322 Egg Proteins Human genes 0.000 description 1
- 108010000912 Egg Proteins Proteins 0.000 description 1
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- 241000287828 Gallus gallus Species 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000003712 anti-aging effect Effects 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- 230000008827 biological function Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005341 cation exchange Methods 0.000 description 1
- 239000003729 cation exchange resin Substances 0.000 description 1
- 229940023913 cation exchange resins Drugs 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- NKLPQNGYXWVELD-UHFFFAOYSA-M coomassie brilliant blue Chemical compound [Na+].C1=CC(OCC)=CC=C1NC1=CC=C(C(=C2C=CC(C=C2)=[N+](CC)CC=2C=C(C=CC=2)S([O-])(=O)=O)C=2C=CC(=CC=2)N(CC)CC=2C=C(C=CC=2)S([O-])(=O)=O)C=C1 NKLPQNGYXWVELD-UHFFFAOYSA-M 0.000 description 1
- 239000000287 crude extract Substances 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 235000014103 egg white Nutrition 0.000 description 1
- 210000000969 egg white Anatomy 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000007667 floating Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000000055 hyoplipidemic effect Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000003456 ion exchange resin Substances 0.000 description 1
- 229920003303 ion-exchange polymer Polymers 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229930014626 natural product Natural products 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000001117 sulphuric acid Substances 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
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
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- Molecular Biology (AREA)
- General Health & Medical Sciences (AREA)
- Sustainable Development (AREA)
- Biochemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The invention discloses a kind of methods of cationic macroreticular resin purification black fungus Thick many candies, belong to field of biotechnology.This method includes the following steps: the pretreatment of A. raw material；B. hot water extraction prepares Thick many candies；C. 732 resin cation of macroreticular resin is handled；D. dialysis removes small molecule；E. vacuum freeze drying；It is prepared into the black fungus Thick many candies of purification.This method can remove most of albumen and small molecular weight impurity, be suitble to industrialized production Blackfungus polyhexose.
Description
Technical field
The invention belongs to field of biotechnology, are specifically related to a kind of slightly more using 732 resin cations purification black fungus
The method of sugar.
Background technique
Black fungus [Auricularia auricular (L.ex Hook) Underw] also known as wood fungus, tree chicken, black dish, are us
The medicinal and edible fungus of state's preciousness, belongs to agaric system Mycophyta Basidiomycetes.Main product is lucky in Heilongjiang Province's Xing'anling mountains
The ground such as woods Changbai Mountain.Studies have shown that Blackfungus polyhexose is one of most effective active constituent in black fungus, there is enhancing body to exempt from
The biological functions such as epidemic disease power, anti-oxidant, anti-aging, anti-cancer, anticancer, it has also become one of hot fields studied both at home and abroad.But mesh
The preceding research isolated and purified to Blackfungus polyhexose is incomplete.
Due to the complicated composition of polysaccharide, the molecular size of polysaccharide crude extract is not exactly the same, and the black wood after extraction
Contain a certain amount of albumen, pigment and small-molecule substance in ear Thick many candies, influences the further research of the chemical structure of polysaccharide, because
This is it is necessary to further isolate and purify Thick many candies, but the conventional method for removing the protein in Thick many candies is with Sevage method
Main, the organic solvent that this method uses is toxic, may will affect the bioactivity of polysaccharide, being also not suitable for will be pure by this method
The Thick many candies changed are used to prepare food or drug.
Macroreticular resin has macropore stereoscopic three-dimensional reticular structure and a biggish specific surface area, internal hole it is not only more but also
Greatly, activated centre is more, and ion diffusion velocity is very fast, and ion-exchange speed is also fast, therefore has good exchange adsorption activity.Closely
It is widely used in the purification of the active constituent of natural products over year, certain macroreticular resins have been used up the research of the deproteinized in polysaccharide
In, achieve good effect.732 cationic macroreticular resin, has skeleton identical with macroporous adsorbent used by this law
Structure, after macroporous adsorbent synthesis, obtained strong acidic ion resin after being re-introduced into chemical functional group can be with hydrogen
The various cations that ion exchange is encountered, therefore can better adsorbed proteins and polysaccharide.But under different conditions, egg
White matter is different with the adsorption effect of polysaccharide, can utilize this property, separating polyose and protein.
The easy to operate of isolating protein is gone using ion-exchange-resin process, required equipment is simple, and it is at low cost, shorten production week
Phase, treating capacity is big, and does not have the problem of organic reagent remains, is suitable for large-scale industrial production.And it can not only be removed
Protein also has certain effect for decoloration.
The patent of related Blackfungus polyhexose preparation aspect has, patent 1: the extracting method (application publication number of Auricularia polysaccharide
It CN106589156A is exactly) using Sevage method deproteinized；A kind of patent 2: preparation method (application publication number of Auricularia polysaccharide
CN107177007A it is) being used cooperatively using a variety of enzymes, the hypolipidemic activity of polysaccharide is improved, for whether removing protein not
It refers to.
Summary of the invention
The object of the present invention is to provide a kind of techniques for refining black fungus Thick many candies, and core of the invention technology is: application
Cation exch ange adsorption resin replaces traditional Sevage method, and scale industrialization is suitble to prepare black fungus Thick many candies.
The technical solution adopted by the invention is as follows:
Black fungus Thick many candies are refined using 732 resin cations, include the following steps: the pretreatment of A. raw material；B. hot water extraction
Prepare Thick many candies；C. 732 resin cation of macroreticular resin is handled；D. dialysis removes small molecule；E. vacuum freeze drying；It is prepared into
The black fungus Thick many candies of purification.
Mentioned-above method, Preferable scheme is that, the pretreatment of step A. raw material refers to, takes dry black fungus heat
Bubble sends out 2-4h, takes the black fungus after being soaked to be placed in juice extractor, the water that 1:1.5-3 is added smashes raw material.
Mentioned-above method, Preferable scheme is that, step B. hot water extraction prepares Thick many candies and refers to, by the original after smashing
Water is added by solid-to-liquid ratio 1:80-100 in material, and the pH of water is 8-10, and 4h, 4 layers of filtered through gauze, by filter residue are extracted in 90 DEG C of water-baths
Extraction 2 times is repeated, merges each filtrate, is centrifuged 20min under the conditions of 4000rpm/min, obtain the extraction of black fungus Thick many candies
Liquid.
Mentioned-above method, Preferable scheme is that, the processing of 732 resin cation of step C. macroreticular resin refers to, black wood
The extracting solution of ear Thick many candies is added in the resin chromatography column of pretreated 732 resin cation, high according to the diameter of amount of resin
Than for 1:15-25, flow control is 5-7 in 1-2.5mL/min, extracting solution pH, extracting solution solubility is 0.2-0.5mg/mL, is extracted
Liquid dosage is the condition of 20mL, collects efflux.The pretreatment of resin is referred to, 732 cation exchange resins use first
Distilled water is swollen, and is taken its amount to be approximately equal to twice of resin volume processed, resin is placed in distilled water after stirring evenly and is carried out
Natural subsidence, inclines the floating material in supernatant after a period of time, then adds the water mixing of certain volume, is repeated several times
.It goes after water plus 4h is impregnated in 4 times of amount 1mol/L hydrochloric acid stirrings, after draining acid solution, distilled water is washed till weakly acidic pH repeatedly.Again plus 4
4h is impregnated in the 1mol/L sodium hydroxide stirring of amount again, after draining lye, after distilled water is washed till weakly acidic pH repeatedly, and measured with 4 times
4h is impregnated in the stirring of 1mol/L hydrochloric acid.Finally neutrality is washed to distillation.
Mentioned-above method, Preferable scheme is that, step D. dialysis removes small molecule and refers to, by bag filter in boiling water
10min is boiled, is packed into polysaccharide solution, and by both sides rope tying, first with tap water dialysis 48h, is then dialysed with distilled water
24h。
Mentioned-above method, Preferable scheme is that, step E. vacuum freeze drying refers to, the solution after dialysis is poured into
Surface plate, pre-freeze for 24 hours, is then placed in vacuum freeze-drying machine and is freeze-dried in refrigerator, and the black fungus refined is thick
Polysaccharide.
The invention discloses a kind of preparation process for refining black fungus Thick many candies, preparation process is as follows: 1, the pre- place of raw material
Reason；2, hot water extraction prepares Thick many candies；3,732 resin cation of macroreticular resin is handled；4, dialysis removes small molecule；5, vacuum is cold
It is lyophilized dry.The most of protein of removing is finally obtained using the technique and pigment, the black fungus Thick many candies of small molecular weight impurity obtain
Higher polysaccharide retention rate, albumen removal efficiency.
Specific embodiment
Technical solution of the present invention is described in detail below with reference to embodiment, but the scope of protection is not limited by this.
Embodiment 1 refines black fungus Thick many candies using 732 resin cations, includes the following steps:
A. it the pretreatment of raw material: takes dry black fungus to be soaked 2h with hot water, takes the black fungus after being soaked to be placed in juice extractor, add
The water for entering 1:1.5 smashes raw material.
B. hot water extraction prepares Thick many candies: water is added by solid-to-liquid ratio 1:80 in the raw material after smashing, the pH of water is 8,90
4h is extracted in DEG C water-bath, filter residue is repeated extraction 2 times, merges each filtrate, in 4000rpm/min item by 4 layers of filtered through gauze
It is centrifuged 20min under part, obtains the extracting solution of black fungus Thick many candies.
C. 732 resin cation of macroreticular resin is handled: the extracting solutions of black fungus Thick many candies be added pretreated 732 sun from
In the resin chromatography column of subtree rouge, compare according to the diameter height of amount of resin for 1:15, flow control is in 1mL/min, extracting solution pH
5, extracting solution solubility is 0.2mg/mL, and extracting solution dosage is the condition of 20mL, collects efflux.
D. dialysis removes small molecule: bag filter being boiled 10min in boiling water, is packed into polysaccharide solution, and both sides are restricted
Then sub- tying is dialysed for 24 hours first with tap water dialysis 48h with distilled water.
E. vacuum freeze drying: the solution after dialysis is poured into surface plate, pre-freeze for 24 hours, is then placed in vacuum in refrigerator
The black fungus Thick many candies for being freeze-dried, and being refined in freeze dryer.
Embodiment 2 refines black fungus Thick many candies using 732 resin cations, includes the following steps:
A. it the pretreatment of raw material: takes dry black fungus to be soaked 4h with hot water, takes the black fungus after being soaked to be placed in juice extractor, add
The water for entering 1:3 smashes raw material.
B. hot water extraction prepares Thick many candies: water is added by solid-to-liquid ratio 1:100 in the raw material after smashing, the pH of water is 10, In
4h is extracted in 90 DEG C of water-baths, filter residue is repeated extraction 2 times, merges each filtrate, in 4000rpm/min by 4 layers of filtered through gauze
Under the conditions of be centrifuged 20min, obtain the extracting solution of black fungus Thick many candies.
C. 732 resin cation of macroreticular resin is handled: the extracting solutions of black fungus Thick many candies be added pretreated 732 sun from
In the resin chromatography column of subtree rouge, compare according to the diameter height of amount of resin for 1:25, flow control is in 2.5mL/min, extracting solution pH
It is 7, extracting solution solubility is 0.5mg/mL, and extracting solution dosage is the condition of 20mL, collects efflux.
D. dialysis removes small molecule: bag filter being boiled 10min in boiling water, is packed into polysaccharide solution, and both sides are restricted
Then sub- tying is dialysed for 24 hours first with tap water dialysis 48h with distilled water.
E. vacuum freeze drying: the solution after dialysis is poured into surface plate, pre-freeze for 24 hours, is then placed in vacuum in refrigerator
The black fungus Thick many candies for being freeze-dried, and being refined in freeze dryer.
Embodiment 3 refines black fungus Thick many candies using 732 resin cations, includes the following steps:
A. it the pretreatment of raw material: takes dry black fungus to be soaked 4h with hot water, takes the black fungus after being soaked to be placed in juice extractor, add
The water for entering 1:1.5 smashes raw material.
B. hot water extraction prepares Thick many candies: water is added by solid-to-liquid ratio 1:90 in the raw material after smashing, the pH of water is 10,90
4h is extracted in DEG C water-bath, filter residue is repeated extraction 2 times, merges each filtrate, in 4000rpm/min item by 4 layers of filtered through gauze
It is centrifuged 20min under part, obtains the extracting solution of black fungus Thick many candies.
C. 732 resin cation of macroreticular resin is handled: the extracting solutions of black fungus Thick many candies be added pretreated 732 sun from
In the resin chromatography column of subtree rouge, compare according to the diameter height of amount of resin for 1:20, flow control is in 1mL/min, extracting solution pH
6, extracting solution solubility is 0.4mg/mL, and extracting solution dosage is the condition of 20mL, collects efflux.
D. dialysis removes small molecule: bag filter being boiled 10min in boiling water, is packed into polysaccharide solution, and both sides are restricted
Then sub- tying is dialysed for 24 hours first with tap water dialysis 48h with distilled water.
E. vacuum freeze drying: the solution after dialysis is poured into surface plate, pre-freeze for 24 hours, is then placed in vacuum in refrigerator
The black fungus Thick many candies for being freeze-dried, and being refined in freeze dryer.
Embodiment 4 refines black fungus Thick many candies using 732 resin cations, includes the following steps:
A. it the pretreatment of raw material: takes dry black fungus to be soaked 2h with hot water, takes the black fungus after being soaked to be placed in juice extractor, add
The water for entering 1:3 smashes raw material.
B. hot water extraction prepares Thick many candies: water is added by solid-to-liquid ratio 1:80 in the raw material after smashing, the pH of water is 10,90
4h is extracted in DEG C water-bath, filter residue is repeated extraction 2 times, merges each filtrate, in 4000rpm/min item by 4 layers of filtered through gauze
It is centrifuged 20min under part, obtains the extracting solution of black fungus Thick many candies.
C. 732 resin cation of macroreticular resin is handled: the extracting solutions of black fungus Thick many candies be added pretreated 732 sun from
In the resin chromatography column of subtree rouge, compare according to the diameter height of amount of resin for 1:20, flow control is in 2.5mL/min, extracting solution pH
It is 6, extracting solution solubility is 0.4mg/mL, and extracting solution dosage is the condition of 20mL, collects efflux.
D. dialysis removes small molecule: bag filter being boiled 10min in boiling water, is packed into polysaccharide solution, and both sides are restricted
Then sub- tying is dialysed for 24 hours first with tap water dialysis 48h with distilled water.
E. vacuum freeze drying: the solution after dialysis is poured into surface plate, pre-freeze for 24 hours, is then placed in vacuum in refrigerator
The black fungus Thick many candies for being freeze-dried, and being refined in freeze dryer.
The measurement of 3 gained Blackfungus polyhexose content of test example experimental example and protein content and removal of protein rate and
The calculating of polysaccharide retention rate.
Determination of polysaccharide uses phend-sulphuric acid, and protein content determination uses dying method with coomassie brilliant blue.
Removal of protein rate %=(C0-C)/C0× 100%, C0 is the original concentration of protein in extracting solution in formula, and C is
Cross the concentration of protein in efflux after column.
Polysaccharide retention rate %=C/C0× 100%, C0 is the original concentration of polysaccharide in extracting solution in formula, and C was to flow after column
Out in liquid polysaccharide concentration.
The method that the present invention refines Blackfungus polyhexose using 732 resin cations, compared with the polysaccharide solution before processing
Compared with removal of protein rate is 90%, and polysaccharide retention rate is 69%.
Claims (6)
1. refining black fungus Thick many candies using 732 resin cations, include the following steps: the pretreatment of A. raw material；B. hot water soaks
Obtain through refining standby Thick many candies；C. 732 resin cation of macroreticular resin is handled；D. dialysis removes small molecule；E. vacuum freeze drying；Preparation
The black fungus Thick many candies that must be refined.
2. according to the method described in claim 1, it is characterized in that, the pretreatment of step A. raw material refers to, takes dry black fungus
It is soaked 2-4h with hot water, takes the black fungus after being soaked to be placed in juice extractor, the water that 1:1.5-3 is added smashes raw material.
3. according to the method described in claim 1, it is characterized in that, step B. hot water extraction prepares Thick many candies and refers to, after smashing
Raw material water is added by solid-to-liquid ratio 1:80-100, the pH of water is 8-10,4h is extracted in 90 DEG C of water-baths, 4 layers of filtered through gauze will
Filter residue repeats extraction 2 times, merges each filtrate, is centrifuged 20min under the conditions of 4000rpm/min, obtains black fungus Thick many candies
Extracting solution.
4. according to the method described in claim 1, it is characterized in that, 732 resin cation of step C. macroreticular resin processing refers to, it is black
The extracting solution of agaric Thick many candies is added in the resin chromatography column of pretreated 732 resin cation, according to the diameter of amount of resin
Height is than being 1:15-25, and flow control is 5-7 in 1-2.5mL/min, extracting solution pH, and extracting solution solubility is 0.2-0.5mg/mL, mentions
Taking liquid dosage is the condition of 20mL, collects efflux.
5. according to the method described in claim 1, it is characterized in that, step D. dialysis remove small molecule refer to, bag filter is being boiled
10min is boiled in water, is packed into polysaccharide solution, and by both sides rope tying, first with tap water dialysis 48h, then uses distilled water
Dialysis is for 24 hours.
6. according to the method described in claim 1, it is characterized in that, step E. vacuum freeze drying refers to, by the solution after dialysis
Pour into surface plate, in refrigerator pre-freeze for 24 hours, the black wood for being then placed in vacuum freeze-drying machine and being freeze-dried, and refined
Ear Thick many candies.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63226293A (en) * | 1987-03-17 | 1988-09-20 | Takasago Corp | Production of polysaccharide of auricularia auricula |
| US20030225001A1 (en) * | 2002-06-04 | 2003-12-04 | Chan Sun Sun | Preparation of an auricularia auricula polysaccharide and its use in mammals |
| CN101514234A (en) * | 2009-03-09 | 2009-08-26 | 王振宇 | Blackfungus polyhexose extraction method |
| CN101812137A (en) * | 2009-12-28 | 2010-08-25 | 大兴安岭科丽尔生物工程有限责任公司 | Method for enriching agaric polysaccharide in purified black agaric by using macroporous absorption resin |
| CN102585032A (en) * | 2012-03-09 | 2012-07-18 | 武汉大学 | Water-soluble polysaccharide extracted from black fungus and preparation method thereof |
| CN104031159A (en) * | 2014-06-25 | 2014-09-10 | 陈文灵 | Method for refining inonotus obliquus crude polysaccharide by use of 732 cationic resin |
-
2018
- 2018-05-11 CN CN201810445945.2A patent/CN110467684A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63226293A (en) * | 1987-03-17 | 1988-09-20 | Takasago Corp | Production of polysaccharide of auricularia auricula |
| US20030225001A1 (en) * | 2002-06-04 | 2003-12-04 | Chan Sun Sun | Preparation of an auricularia auricula polysaccharide and its use in mammals |
| CN101514234A (en) * | 2009-03-09 | 2009-08-26 | 王振宇 | Blackfungus polyhexose extraction method |
| CN101812137A (en) * | 2009-12-28 | 2010-08-25 | 大兴安岭科丽尔生物工程有限责任公司 | Method for enriching agaric polysaccharide in purified black agaric by using macroporous absorption resin |
| CN102585032A (en) * | 2012-03-09 | 2012-07-18 | 武汉大学 | Water-soluble polysaccharide extracted from black fungus and preparation method thereof |
| CN104031159A (en) * | 2014-06-25 | 2014-09-10 | 陈文灵 | Method for refining inonotus obliquus crude polysaccharide by use of 732 cationic resin |
Non-Patent Citations (3)
| Title |
|---|
| XIN ZHAO等: ""Optimization of ultrasonic wave extraction technology of Polysaeeharides from aurieularia aurieula by response surface methodology and molecular weight distributions"", 《ADVANCED MATERIALS RESEARCH》 * |
| 朱磊: ""黑木耳多糖分离纯化、理化性质及抗疲劳功能的研究"", 《万方数据知识服务平台》 * |
| 赵鑫: ""黑木耳分级多糖抗氧化活性及其相关生理功能研究"", 《万方数据知识服务平台》 * |
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