CN105906738B - The method of separating polyose is extracted in a kind of cockscomb - Google Patents
The method of separating polyose is extracted in a kind of cockscomb Download PDFInfo
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- CN105906738B CN105906738B CN201610486671.2A CN201610486671A CN105906738B CN 105906738 B CN105906738 B CN 105906738B CN 201610486671 A CN201610486671 A CN 201610486671A CN 105906738 B CN105906738 B CN 105906738B
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- 241000561734 Celosia cristata Species 0.000 title claims abstract description 29
- 210000001520 comb Anatomy 0.000 title claims abstract description 29
- 238000000034 method Methods 0.000 title claims abstract description 25
- 150000004676 glycans Chemical class 0.000 claims abstract description 28
- 229920001282 polysaccharide Polymers 0.000 claims abstract description 27
- 239000005017 polysaccharide Substances 0.000 claims abstract description 27
- 238000003756 stirring Methods 0.000 claims abstract description 22
- 102000002322 Egg Proteins Human genes 0.000 claims abstract description 19
- 108010000912 Egg Proteins Proteins 0.000 claims abstract description 19
- 238000001914 filtration Methods 0.000 claims abstract description 19
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 17
- 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 claims abstract description 16
- 235000014103 egg white Nutrition 0.000 claims abstract description 16
- 210000000969 egg white Anatomy 0.000 claims abstract description 16
- 239000002244 precipitate Substances 0.000 claims abstract description 15
- 235000009508 confectionery Nutrition 0.000 claims abstract description 14
- 239000003463 adsorbent Substances 0.000 claims abstract description 7
- 238000013019 agitation Methods 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 6
- 239000006228 supernatant Substances 0.000 claims abstract description 4
- 239000002994 raw material Substances 0.000 claims abstract description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 8
- 229910052799 carbon Inorganic materials 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims 1
- 239000002904 solvent Substances 0.000 abstract description 5
- 238000002360 preparation method Methods 0.000 abstract description 4
- 238000013459 approach Methods 0.000 abstract description 2
- 238000003912 environmental pollution Methods 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 238000000746 purification Methods 0.000 abstract description 2
- 238000000926 separation method Methods 0.000 abstract description 2
- 241000196324 Embryophyta Species 0.000 description 12
- 235000019441 ethanol Nutrition 0.000 description 6
- 239000000203 mixture Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 210000003278 egg shell Anatomy 0.000 description 3
- 235000013601 eggs Nutrition 0.000 description 3
- OQUKIQWCVTZJAF-UHFFFAOYSA-N phenol;sulfuric acid Chemical compound OS(O)(=O)=O.OC1=CC=CC=C1 OQUKIQWCVTZJAF-UHFFFAOYSA-N 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 238000010792 warming Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
- 229920002472 Starch Polymers 0.000 description 2
- 239000008280 blood Substances 0.000 description 2
- 210000004369 blood Anatomy 0.000 description 2
- 239000001913 cellulose Substances 0.000 description 2
- 229920002678 cellulose Polymers 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 229920001277 pectin Polymers 0.000 description 2
- 239000001814 pectin Substances 0.000 description 2
- 235000010987 pectin Nutrition 0.000 description 2
- 102000004169 proteins and genes Human genes 0.000 description 2
- 108090000623 proteins and genes Proteins 0.000 description 2
- 238000004062 sedimentation Methods 0.000 description 2
- 239000008107 starch Substances 0.000 description 2
- 235000019698 starch Nutrition 0.000 description 2
- 241000287828 Gallus gallus Species 0.000 description 1
- 241000219315 Spinacia Species 0.000 description 1
- 235000009337 Spinacia oleracea Nutrition 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 230000001142 anti-diarrhea Effects 0.000 description 1
- 230000003471 anti-radiation Effects 0.000 description 1
- 230000000259 anti-tumor effect Effects 0.000 description 1
- 230000002155 anti-virotic effect Effects 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000000872 buffer Substances 0.000 description 1
- 235000010980 cellulose Nutrition 0.000 description 1
- 238000005352 clarification Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000004440 column chromatography Methods 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000012869 ethanol precipitation Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 231100001261 hazardous Toxicity 0.000 description 1
- 230000023597 hemostasis Effects 0.000 description 1
- 230000002218 hypoglycaemic effect Effects 0.000 description 1
- 230000002519 immonomodulatory effect Effects 0.000 description 1
- 230000001900 immune effect Effects 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 238000013332 literature search Methods 0.000 description 1
- 210000004185 liver Anatomy 0.000 description 1
- 235000012054 meals Nutrition 0.000 description 1
- 230000005906 menstruation Effects 0.000 description 1
- 230000004060 metabolic process Effects 0.000 description 1
- 235000015097 nutrients Nutrition 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000004224 protection Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 235000013619 trace mineral Nutrition 0.000 description 1
- 239000011573 trace mineral Substances 0.000 description 1
- 235000013311 vegetables Nutrition 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
Landscapes
- 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 present invention relates to separation of polysaccharides technical field of purification, a kind of method that separating polyose is extracted in cockscomb is particularly disclosed.The method that separating polyose is extracted in the cockscomb, using cockscomb as raw material, it is characterized in that: it smashs to pieces, squeezes after cockscomb is cleaned, filtering obtains polysaccharide solution；Into polysaccharide solution, egg white is added in stirring, is filtered after standing, and supernatant is Thick many candies solution；Thick many candies solution is heated, adsorbent is added to decolourize, is filtered；Solution is concentrated after filtering, agitation and dropping ethanol solution, until there is white precipitate, stops stirring, filters after standing, precipitate polysaccharide obtained by drying.Preparation process of the present invention is simple, easy to operate, and equipment investment is few, and solvent consumption is few, and non-environmental-pollution, production cost is low, and the content of yield and functional component is high, to develop the medical value of cockscomb, realizing that the industrialization of cockscomb polysaccharide provides a kind of new approaches.
Description
(1) technical field
The present invention relates to separation of polysaccharides technical field of purification, in particular to the side of separating polyose is extracted in a kind of cockscomb
Method.
(2) background technique
It is more than 10 glycan that plant polyose, also known as plant polysaccharide, which are the degree of polymerization that plant metabolism generates, generally
It is present in natural plant body, including starch, fiber, polysaccharide, pectin etc..Due to from a wealth of sources, the difference of plant polyose
The molecule of the plant polyose of kind is constituted and molecular weight is different.Some plant polyoses early have become such as starch, cellulose, pectin
For the important component in people's daily life.
Plant polyose research now is of increasing concern, and international scientific circle even proposes that 21 century is the century of polysaccharide；Section
It learns experimental study to show, many plant polyoses have bioactivity, have including immunological regulation, antitumor, hypoglycemic, drop blood
The health-care effects such as rouge, anti-radiation, anti-bacteria and anti-virus, protection liver.So plant polyose is widely used medical field, meal already
It drinks in the popular lifes fields such as boundary.
Cockscomb originates in India, belongs to amaranthaceous plant, alias chicken hair worn in a bun or coil flower, tropical spinach.Cockscomb scape, Ye Kezuo vegetables,
Flower, which dries in the shade, can make food.Cockscomb medical value is higher, civil for treating the diseases such as hemostasis, antidiarrheal, menstruation regulating blood nourishing.
It is reported that rich in nutrients such as good protein, cellulose and various trace elements in the flower and seed of cockscomb
Matter, and can be used for food, polysaccharide component especially therein even more has preferable immunoloregulation function, thus shows
Good development and application values.But purifying by literature search, is extracted to plant polyose, the method containing polysaccharide of acquisition is adopted
With high-temp extracting, sevag method takes off albumen, resin column chromatography enriching and purifying to realize, these extracting methods often have solvent use
The disadvantages of larger, extraction time is longer, working efficiency is lower is measured, is especially needed in preparation process to extracting solution, extract liquor or is washed
De- liquid carries out multiple lane Soviet Union, since heating concentration alleviation is more, be easy to cause effective component destruction or is lost, gained is caused to extract
The recovery rate of object and the rate of transform of effective component be not high, and to use the hazardous solvents such as high boiling n-butanol, causes to environment
Pollution.In addition, traditional ethanol precipitation be easy to cause the sedimentation of the impurity such as protein, so that the purity of polysaccharide is not high.
(3) summary of the invention
That in order to compensate for the shortcomings of the prior art, the present invention provides a kind of preparation processes is simple, solvent consumption is few, without environment
The method of separating polyose is extracted in the cockscomb of pollution.
The present invention is achieved through the following technical solutions:
A kind of method that separating polyose is extracted in cockscomb includes the following steps: using cockscomb as raw material
(1) it smashs to pieces, squeezes after cleaning cockscomb, filtering obtains polysaccharide solution；
(2) into polysaccharide solution, egg white is added in stirring, until egg white concentration is 65-80mg/L, is stood 12-18h, is filtered, on
Clear liquid is Thick many candies solution；
(3) heating Thick many candies solution adds adsorbent to decolourize to 50-60 DEG C, after stir process 30-60min, filtering；
(4) solution after filtering is concentrated into the 1/5 of original volume, agitation and dropping ethanol solution stops until there is white precipitate
Stirring, stands 12-15h, and filtering precipitates polysaccharide obtained by drying.
More excellent technical solution of the invention are as follows:
In step (2), egg white is added in polysaccharide solution, is stood after stirring 30min；Use the property of egg white ampholytes
Matter assembles charged particle, and adsorbs other suspended matters and form larger aggregation to sink together, to reach clarification effect
Fruit, simple process and pollution-free.
In step (3), adsorbent is the mixture of diatomite and active carbon, and the mass ratio of diatomite and active carbon is 1-
2:1；The mass ratio of adsorbent and Thick many candies solution is 0.5-1:100-150；The suction mixed using diatomite and active carbon
Attached dose, not only good decolorizing effect, also substantially increases the rate of filtration of liquid.
In step (4), the mass concentration of the ethanol solution is 95%；Using the mode that ethyl alcohol is slowly added dropwise, the polysaccharide is set to be in
Powdered precipitation reduces the sedimentation of other impurities.
Preparation process of the present invention is simple, easy to operate, and equipment investment is few, and solvent consumption is few, non-environmental-pollution, production cost
Low, the content of yield and functional component is high, to develop the medical value of cockscomb, realizing that the industrialization of cockscomb polysaccharide provides
A kind of new approaches.
(4) specific embodiment
Embodiment 1: the method for separating polyose in cockscomb
(1) it pre-processes: taking fresh cockscomb 1.0Kg, cleaned, smashed to pieces with clear water, squeeze, filtering obtains polysaccharide solution
245g；
(2) egg white is handled: taking the solution in step (1), under agitation, Fresh Egg eggshell takes an aperture, slowly
Egg white is added, until the final concentration of 65mg/L of egg white, stirs 30min, stands 12h；Filtering, supernatant is Thick many candies 215g；
(3) decolourize: Thick many candies solution obtained by step (2) is warming up to 50 DEG C, and diatomite and Mixture of Activated Carbon is added
1.3g, the two ratio are 1:1, handle 30min under stirring condition, filter；
(4) it precipitates: step (3) acquired solution being taken to be concentrated into the 1/5 of original volume, under stirring condition, 95% second is slowly added dropwise
Alcohol stops stirring until there is white precipitate, stands 12h, and filtering precipitates polysaccharide powder 89.1g obtained by drying.Using phenol-
Sulfuric acid process is measured resulting polyoses content, polyoses content 81.2g, purity 91.1%.
Embodiment 2: the method for separating polyose in cockscomb
(1) it pre-processes: taking fresh cockscomb 1.1Kg, cleaned, smashed to pieces with clear water, squeeze, filtering obtains polysaccharide solution
258g；
(2) egg white is handled: taking the solution in step (1), under agitation, Fresh Egg eggshell takes an aperture, slowly
Egg white is added, until the final concentration of 75mg/L of egg white, stirs 30min, stands 14h；Filtering, upper Thick many candies solution 238g；
(3) decolourize: Thick many candies solution obtained by step (2) is warming up to 55 DEG C, and diatomite and Mixture of Activated Carbon is added
1.5g, the two ratio are 3:2, handle 40min under stirring condition, filter；
(4) it precipitates: step (3) acquired solution being taken to be concentrated into the 1/5 of original volume, under stirring condition, 95% second is slowly added dropwise
Alcohol stops stirring until there is white precipitate, stands 13h, and filtering precipitates polysaccharide powder 94.0g obtained by drying.Using phenol-
Sulfuric acid process is measured resulting polyoses content, polyoses content 85.1g, purity 90.5%.
Embodiment 3: the method for separating polyose in cockscomb
(1) it pre-processes: taking fresh cockscomb 1.5Kg, cleaned, smashed to pieces with clear water, squeeze, filtering obtains polysaccharide solution
261g；
(2) egg white is handled: taking the solution in step (1), under agitation, Fresh Egg eggshell takes an aperture, slowly
Egg white is added, until the final concentration of 80mg/L of egg white, stirs 30min, stands 15h；Filtering, supernatant is Thick many candies 240g；
(3) decolourize: Thick many candies solution obtained by step (2) is warming up to 60 DEG C, and diatomite and Mixture of Activated Carbon is added
1.5g, the two ratio are 2:1, handle 60min under stirring condition, filter；
(4) it precipitates: step (3) acquired solution being taken to be concentrated into the 1/5 of original volume, under stirring condition, 95% second is slowly added dropwise
Alcohol stops stirring until there is white precipitate, stands 15h, and filtering precipitates polysaccharide powder 96.8g obtained by drying.Using phenol-
Sulfuric acid process is measured resulting polyoses content, polyoses content 86.5g, purity 89.3%.
The specific embodiments of the present invention do not constitute a limitation of the present invention, all using similar structure of the invention and change
Change, is within the scope of the invention.
Claims (2)
1. a kind of method that separating polyose is extracted in cockscomb, using cockscomb as raw material, it is characterized in that, include the following steps: (1)
It smashs to pieces, squeezes after cockscomb is cleaned, filtering obtains polysaccharide solution；(2) into polysaccharide solution, egg white is added in stirring, until egg white
Concentration is 65-80mg/L, stands 12-18h after stirring 30min, is filtered, and supernatant is Thick many candies solution；(3) heating Thick many candies are molten
Liquid adds adsorbent to decolourize to 50-60 DEG C, after stir process 30-60min, filtering；Adsorbent is the mixing of diatomite and active carbon
Object, and the mass ratio of diatomite and active carbon is 1-2:1；The mass ratio of adsorbent and Thick many candies solution is 0.5-1:100-150；
(4) solution after filtering is concentrated into the 1/5 of original volume, agitation and dropping ethanol solution stops stirring until there is white precipitate, quiet
12-15h is set, filters, precipitates polysaccharide obtained by drying.
2. extracting the method for separating polyose in cockscomb according to claim 1, it is characterised in that: described in step (4)
The mass concentration of ethanol solution is 95%.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| KR102349970B1 (en) * | 2020-03-05 | 2022-01-12 | 김희태 | Polysaccharide from Celosia cristata flower extract, method of extracting the same and immunostimulating composition comprising the same |
| CN113999324B (en) * | 2021-11-11 | 2022-09-09 | 北京亚东生物制药(安国)有限公司 | Method for deproteinizing hericium erinaceus liquid |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1392160A (en) * | 2001-06-15 | 2003-01-22 | 中国科学院化工冶金研究所 | Flocculating extraction process of seawweed polysaccharide |
| CN101139402A (en) * | 2007-10-18 | 2008-03-12 | 西北大学 | Method for extracting polysaccharide from jujube |
| CN101942035A (en) * | 2010-09-07 | 2011-01-12 | 天津强微特生物科技有限公司 | Method for extracting and refining rhizobia exocellular polysaccharide |
| CN102993321A (en) * | 2012-09-27 | 2013-03-27 | 河南牧翔动物药业有限公司 | Preparation method of astragalus polysaccharide |
| CN103130905A (en) * | 2013-01-09 | 2013-06-05 | 华东理工大学 | Herbage plant polysaccharide purification method by utilization of microwave-assisted extraction and integration flocculation technology |
-
2016
- 2016-06-29 CN CN201610486671.2A patent/CN105906738B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1392160A (en) * | 2001-06-15 | 2003-01-22 | 中国科学院化工冶金研究所 | Flocculating extraction process of seawweed polysaccharide |
| CN101139402A (en) * | 2007-10-18 | 2008-03-12 | 西北大学 | Method for extracting polysaccharide from jujube |
| CN101942035A (en) * | 2010-09-07 | 2011-01-12 | 天津强微特生物科技有限公司 | Method for extracting and refining rhizobia exocellular polysaccharide |
| CN102993321A (en) * | 2012-09-27 | 2013-03-27 | 河南牧翔动物药业有限公司 | Preparation method of astragalus polysaccharide |
| CN103130905A (en) * | 2013-01-09 | 2013-06-05 | 华东理工大学 | Herbage plant polysaccharide purification method by utilization of microwave-assisted extraction and integration flocculation technology |
Non-Patent Citations (2)
| Title |
|---|
| Purification, characterization and immunomodulatory activity of a polysaccharide from Celosia cristata;Zhenliang Sun et al.;《Carbohydrate Polymers》;20150708;第337-344页 |
| 鸡冠花的营养成分分析;翁德宝，等;《营养学报》;19950331;第17卷(第1期);第59-62页 |
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Application publication date: 20160831 Assignee: Zibo High tech Zone Xingrui Qingke Environmental Technology Research Institute Assignor: SCIENGREEN (SHANDONG) ENVIRONMENT TECHNOLOGY CO.,LTD. Contract record no.: X2023980047555 Denomination of invention: A method for extracting and isolating polysaccharides from cockscomb flowers Granted publication date: 20190322 License type: Common License Record date: 20231204 |