CN108299570A - A kind of preparation method of polysaccharides - Google Patents
A kind of preparation method of polysaccharides Download PDFInfo
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- CN108299570A CN108299570A CN201810409400.6A CN201810409400A CN108299570A CN 108299570 A CN108299570 A CN 108299570A CN 201810409400 A CN201810409400 A CN 201810409400A CN 108299570 A CN108299570 A CN 108299570A
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- 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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Abstract
The present invention relates to a kind of preparation methods of polysaccharides, specific steps include that matrimony vine is cleaned, soaks, being crushed, purified water extraction is added, removing matrimony vine pulp through beater removal matrimony vine seed, centrifuge, by filtrate respectively by ceramic membrane, organic membrane system, the concentrated freeze-drying of extracting solution is obtained into product polysaccharides.Present invention determine that extraction stage most effective purified water water temperature and ratio, ensure that being fully dissolved out for polysaccharides, greatly improve the recovery rate of polysaccharides；The bioactivity for utmostly maintaining polysaccharides avoids the problem of polysaccharide caused by heating up using alcohol deposition method, protein inactivation and flocculation cause loss of effective components.
Description
Technical field
The invention belongs to technical field of polysaccharide extraction, and in particular to a kind of polysaccharides and preparation method thereof.
Background technology
People show that polysaccharides is most important active constituent, matrimony vine in matrimony vine to the result of study of matrimony vine in recent years
Polysaccharide is a kind of water-soluble polysaccharide, it, which has, promotes immune, anti-aging, antitumor, removing free radical, antifatigue, reducing blood lipid, drop
Blood glucose adjusts the effects that immune, radioresistance, liver protection, reproductive function protection and improvement.As people are to the weight of matrimony vine medicine price cheating value
Diopter increases, and the extracting method of polysaccharides and application become research hotspot.The extraction process of existing polysaccharides is mostly tradition
Hot water extraction or organic solvent (ether, ethyl alcohol, petroleum ether etc.) degreasing after Hot water extraction, it is molten in these conventional methods
Agent dosage is big, time-consuming and recovery rate is low, to improve the economic benefit of the fruit of Chinese wolfberry, improves in the fruit of Chinese wolfberry effectively at the extraction of hair
Rate finds the important subject that rapidly and effectively polysaccharides extracting method is wolfberry industryization development.Such as China
The patent of invention of entitled " a kind of extracting method of polysaccharides " of Department of Intellectual Property's Granted publication on the 31st of August in 2016, patent
Number it is：201410628540 .4, this publication disclose a kind of extracting method of polysaccharides, this method includes wolfberry fruit powder
Preparation, impregnate in water, activated carbon decolorizing be added, cellulase degradation is added, adds alkali protease and ficin
Enzyme, under microwave condition digest, digest after concentrate and decolourize, centrifuge, take supernatant concentration alcohol precipitation, be freeze-dried, matrimony vine it is more
Sugar.Method using the present invention extracts polysaccharide from matrimony vine, using enzyme effect mild condition, using a variety of different enzymes by matrimony vine
In fat, cellulase hydrolysis, Polyose extraction therein is come out, the utilization rate of matrimony vine, method using the present invention are improved
Obtaining polysaccharide, not only yield is high, but also purity is also high.
In above-mentioned polysaccharides extracting method, have the following problems：1, enzymolysis and microwave under microwave condition is used to carry
It takes, the activity of polysaccharides is likely to decrease according to the intervention of current research microwave equipment.2, it can be improved using enzymatic isolation method more
The yield of sugar, but due to needing to carry out high temperature enzyme deactivation to the material after enzymolysis, to eliminate the activity of enzyme, the temperature of enzyme deactivation generally exists
100 DEG C or so, during enzyme deactivation, it can also substantially reduce the activity of polysaccharides.
Polysaccharides activity and yield and the higher polysaccharides production technology of purity can effectively be kept by how providing one kind,
As the direction of people's research.
Invention content
In view of the above-mentioned deficiencies in the prior art, it is an object of the present invention to provide a kind of bioactivity, effectively of utmostly keeping
The high polysaccharides and preparation method thereof of component content.
The present invention to achieve the above object the technical solution adopted is that：A kind of preparation method of polysaccharides prepares work
Skill is as follows：
1）Dry wolfberry or fresh fructus lycii are selected, after cleaning, the water that 0-4 times of matrimony vine weight is added impregnates 0-1 hour；
2）By after above-mentioned immersion matrimony vine and soak squeeze into disintegrating apparatus and matrimony vine crushed；
3）The water stirring extraction of 0.5-4 times of matrimony vine weight 1-4 hours is added in above-mentioned crushing liquid；
4）Said extracted liquid is filtered, it is spare to collect filtrate；For the matrimony vine seed filtered out for extracting Chinese wolfberry fruit oil, fructus lycii is meat
In preparing Chinese wolfberry fruit drink；
5）By above-mentioned filtrate by ceramic membrane, organic membrane filter after, concentrated, be freeze-dried to obtain product polysaccharides.
The water that above-mentioned technical process uses is pure water, and temperature is maintained at 18-35 DEG C.
The aperture of above-mentioned ceramic membrane is 50nm.
Above-mentioned organic film is by organic film that molecular weight is 200-6000 dalton.
It is 200-2000 dalton NF membranes that above-mentioned NF membrane, which is by molecular weight,；Ultrafiltration membrane is to be by molecular weight
The ultrafiltration membrane of 1000-6000 dalton.
Above-mentioned ceramic membrane, organic membrane filter mistake film temperature be less than 35 DEG C, cross film pressure 0.2Mpa.
Above-mentioned concentration technology is concentrated using low-temperature negative-pressure, and thickening temperature is not higher than 35 DEG C, concentrates pressure 0.8Mpa, concentration
To 0.2-0.25 times of original volume.
Water used is pure water when above-mentioned cleaning, immersion and stirring extraction, and water temperature is at 30-35 DEG C.
In conclusion by adopting the above-described technical solution, the beneficial effects of the invention are as follows：
（1）Present invention determine that extraction stage most effective purified water water temperature and ratio, ensure that being fully dissolved out for polysaccharides,
Greatly improve the recovery rate of polysaccharides；
（2）All processes of the present invention are carried out at 35 DEG C or less, utmostly maintain the bioactivity of polysaccharides, greatly
The quality for improving polysaccharides is avoided using the heating needed for alcohol deposition method except during alcohol, caused by polysaccharide, protein lose
The problem of living or flocculation causes loss of effective components；
（3）Present invention uses two pass mashing and two-stage centrifugal systems, eliminate matrimony vine seed and Chinese holly in extracting solution to the greatest extent
Fructus lycii meat；
（4）Using ceramic membrane purpose be by Physical entrapment by the way of remove minute impurities in extracting solution, as matrimony vine is extracted
The other impurity of molecular level, pectin in liquid can make juice from Chinese wolfberry that transparence be presented, while can filter the bacterium in fructus lycii extracted solution
It removes, realizes that extracting solution is sterilized online；
The purpose of organic film is to remove monosaccharide, oligosaccharides, salt ion etc. in fructus lycii extracted solution, to reach retention polysaccharides
Purpose
（5）Present invention uses NF membrane and/or the organic membrane system of ultrafiltration membrane, it is more to can remove monosaccharide, small molecule in extracting solution
Sugar, inorganic ion, oligosaccharides and pigment etc. ensure that the purity and bioactivity of polysaccharides.
Specific implementation mode
Below in conjunction with the embodiment of the present invention, technical scheme in the embodiment of the invention is clearly and completely described.
Based on the embodiments of the present invention, obtained by those of ordinary skill in the art without making creative efforts all
Other embodiment shall fall within the protection scope of the present invention.
Embodiment 1
A kind of preparation method of polysaccharides, is as follows：
1）500 grams of dried fruit of lycium barbarum is weighed, after purified water vibrations cleaning showers 15 minutes, 2 kilograms 35 DEG C or so pure is added
Change water to impregnate 1 hour；
2）By after above-mentioned immersion matrimony vine and soak be crushed, broken material is ground by colloid mill again, is reached
Dispersion, crushing, emulsification, homogeneous, mixing purpose
3）In the material that above-mentioned steps are ground, 2 kilograms of 35 DEG C of purified waters, stirring extraction 2 hours or so is added；
4）Said extracted liquid is filtered, it is spare to collect filtered fluid；The obtained matrimony vine seed of filtering, the thick pulp of matrimony vine, can use
In extraction Boxthorn Seed Oil and make Chinese wolfberry fruit drink.
Double-channel beater removal matrimony vine seed can be used in filtering, then removes the thick pulp of matrimony vine, centrifugal rotational speed through decanter centrifuge
3700r/min, then remove matrimony vine pulp, centrifugal rotational speed 7800r/min through butterfly centrifugal machine；
5）By above-mentioned filtered fluid by the ceramic membrane equipment that membrane aperture is 50nm, 35 DEG C, pressure 0.2Mpa of film temperature is crossed, is collected
Filtrate；
Since the diameter of microorganism is in 200nm or so, so microorganism can not be by ceramic membrane, which just can reach degerming work
With；
6）By above-mentioned filtrate by the nanofiltration membrane system of 400 dalton of molecular weight, 30 DEG C of film temperature is crossed, crosses film pressure 0.2Mpa,
NF membrane trapped fluid is collected, then by the ultrafiltration membrane that molecular weight is 5000 dalton, crosses 30 DEG C of film temperature, crosses film pressure
0.2MPa collects ultrafiltration membrane trapped fluid；
7）Above-mentioned ultrafiltration membrane trapped fluid is concentrated to after 0.25 times or so of ultrafiltration membrane trapped fluid volume, it is freeze-dried to obtain
Polysaccharides.
Product polysaccharides 6.38g is obtained, the part that molecular weight 1000-10000Da is measured through HPLC accounts for 95%, and kelvin is fixed
Nitrogen method measures protein content 12%, and anthrone-sulphuric acid method neutral polysaccharide content 45%, carbazole method measures glucuronic acid content 5%.
Embodiment 2
In the above-described embodiments, matrimony vine uses fresh fructus lycii, is as follows：
1）2500 grams of dried fruit of lycium barbarum is weighed, shakes cleaning showers 8 minutes or so using purified water；
2）Fresh fructus lycii after above-mentioned cleaning is crushed, broken material is ground by colloid mill again；
3）In the material that above-mentioned steps are ground, 2 kilograms of 35 DEG C of purified waters, stirring extraction 1 hour or so is added；
4）Said extracted liquid is filtered, it is spare to collect filtered fluid；The obtained matrimony vine seed of filtering, the thick pulp of matrimony vine, can use
In extraction Boxthorn Seed Oil and Chinese wolfberry fruit drink.
Double-channel beater removal matrimony vine seed can be used in filtering, then removes the thick pulp of matrimony vine, centrifugal rotational speed through decanter centrifuge
3700r/min, then remove matrimony vine pulp, centrifugal rotational speed 7800r/min through butterfly centrifugal machine；
5）By above-mentioned filtered fluid by the ceramic membrane equipment that membrane aperture is 50nm, 35 DEG C, pressure 0.2Mpa of film temperature is crossed, is collected
Filtrate；
6）By above-mentioned filtrate by the nanofiltration membrane system of 400 dalton of molecular weight, 30 DEG C of film temperature is crossed, crosses film pressure 0.2Mpa,
NF membrane trapped fluid is collected, then by the ultrafiltration membrane that molecular weight is 5000 dalton, crosses 30 DEG C of film temperature, crosses film pressure
0.2MPa collects ultrafiltration membrane trapped fluid；
7）Above-mentioned ultrafiltration membrane trapped fluid is concentrated to after 0.25 times or so of ultrafiltration membrane trapped fluid volume, it is freeze-dried to obtain
Polysaccharides.
Product polysaccharides 6.52g is obtained, the part that molecular weight 1000-10000Da is measured through HPLC accounts for 95%, and kelvin is fixed
Nitrogen method measures protein content 12%, and anthrone-sulphuric acid method neutral polysaccharide content 45%, carbazole method measures glucuronic acid content 5%.
Embodiment 3：
1）Gold is visited（Ø0.5mm）Organic dried fruit of lycium barbarum 500g afterwards shakes cleaning showers 15min, by defending using purified water
Raw grade screw pump is sent in sanitation-grade steeping tank；
2) 35 DEG C of purified waters of 4 times of dried fruit of lycium barbarum quality are added, impregnate 1h；
3）Using crusher in crushing, then by sanitation-grade colloid mill, obtain matrimony vine soak, rotating speed 3000r/min；
4）By above-mentioned soak, 4 times of 35 DEG C of purified waters are added, stirring extraction 2h, rotating speed 100r/min obtain extracting solution；
5）Extracting solution is removed into matrimony vine seed, rotating speed 1440r/min through double-channel beater；Again the thick fruit of matrimony vine is removed through decanter centrifuge
Meat, centrifugal rotational speed 3700r/min, then matrimony vine pulp is removed through butterfly centrifugal machine, centrifugal rotational speed 7800r/min obtains extracting solution
Ⅰ；
6）Extracting solution I collects ceramic membrane separation filtrate, obtains extracting solution II, mistake by the ceramic membrane equipment that membrane aperture is 50nm
35 DEG C of film temperature, pressure 0.2MPa；
7）Extracting solution II crosses 30 DEG C of film temperature by the nanofiltration membrane system of 400 dalton of molecular weight, crosses film pressure 0.2Mpa, receives
It collects membrane retention liquid and obtains extracting solution III；
8）Extracting solution III is fruit of Chinese wolfberry raw material when being concentrated into volume through single-action concentrator, 35 DEG C, pressure 0.8MPa of thickening temperature
0.25 times of quality, obtains extracting solution IV；
9）Extracting solution IV is freeze-dried 30h, and chilled, primary drying, parsing-desiccation obtain polysaccharides；It is freeze-dried temperature-
40 DEG C~30 DEG C, -40 DEG C of cryogenic temperature, 30 DEG C, pressure 0.35MPa of primary drying temperature, 30 DEG C of parsing-desiccation temperature, pressure
0.2Mpa。
Product polysaccharides 6.42g is obtained, the part that molecular weight 1000-10000Da is measured through HPLC accounts for 90%, and kelvin is fixed
Nitrogen method measures protein content 11%, and anthrone-sulphuric acid method neutral polysaccharide content 40%, carbazole method measures glucuronic acid content 7%.
Embodiment 3
A kind of preparation method of polysaccharides, is as follows：
1）Gold is visited（Ø0.5mm）Organic dried fruit of lycium barbarum 500g afterwards shakes cleaning showers 15min, by defending using purified water
Raw grade screw pump is sent in sanitation-grade steeping tank；
2) 35 DEG C of purified waters of 4 times of dried fruit of lycium barbarum quality are added, impregnate 1h；
3）Using crusher in crushing, then by sanitation-grade colloid mill, obtain matrimony vine soak, rotating speed 3000r/min；
4）By above-mentioned soak, 4 times of 35 DEG C of purified waters are added, stirring extraction 2h, rotating speed 100r/min obtain extracting solution；
5）Extracting solution is removed into matrimony vine seed, rotating speed 1440r/min through double-channel beater；Again the thick fruit of matrimony vine is removed through decanter centrifuge
Meat, centrifugal rotational speed 3700r/min, then matrimony vine pulp is removed through butterfly centrifugal machine, centrifugal rotational speed 7800r/min obtains extracting solution
Ⅰ；
6）Extracting solution I collects ceramic membrane separation filtrate, obtains extracting solution II, mistake by the ceramic membrane equipment that membrane aperture is 50nm
35 DEG C of film temperature, pressure 0.2MPa；
7）Extracting solution II crosses 30 DEG C of film temperature by the ultrafiltration membrane that molecular weight is 5000 dalton, crosses film pressure 0.2MPa, collects
Ultrafiltration membrane trapped fluid obtains extracting solution III；
8）Extracting solution III is fruit of Chinese wolfberry raw material when being concentrated into volume through single-action concentrator, 35 DEG C, pressure 0.8MPa of thickening temperature
0.25 times of quality, obtains extracting solution IV；
9）Extracting solution IV is freeze-dried 30h, and chilled, primary drying, parsing-desiccation obtain polysaccharides；It is freeze-dried temperature-
40 DEG C~30 DEG C, -40 DEG C of cryogenic temperature, 30 DEG C, pressure 0.35MPa of primary drying temperature, 30 DEG C of parsing-desiccation temperature, pressure
0.2Mpa。
Product polysaccharides 6.40g is obtained, the part that molecular weight 1000-10000Da is measured through HPLC accounts for 91%, and kelvin is fixed
Nitrogen method measures protein content 13%, and anthrone-sulphuric acid method neutral polysaccharide content 48%, carbazole method measures glucuronic acid content 13%.
Above-described embodiment simply to illustrate that the present invention technical concepts and features, it is in the art the purpose is to be to allow
Those of ordinary skill cans understand the content of the present invention and implement it accordingly, and it is not intended to limit the scope of the present invention.It is all
It is the equivalent changes or modifications made by the essence according to the content of present invention, should all covers within the scope of the present invention..
Claims (8)
1. a kind of preparation method of polysaccharides, preparation process are as follows：
1）Dry wolfberry or fresh fructus lycii are selected, after cleaning, the water that 0-4 times of matrimony vine weight is added impregnates 0-1 hour；
2）By after above-mentioned immersion matrimony vine and soak squeeze into disintegrating apparatus and matrimony vine crushed；
3）The water stirring extraction of 0.5-4 times of matrimony vine weight 1-4 hours is added in above-mentioned crushing liquid；
4）Said extracted liquid is filtered, it is spare to collect filtrate；For the matrimony vine seed filtered out for extracting Chinese wolfberry fruit oil, fructus lycii is meat
In preparing Chinese wolfberry fruit drink；
5）By above-mentioned filtrate by ceramic membrane, organic membrane filter after, concentrated, be freeze-dried to obtain product polysaccharides.
2. according to a kind of preparation method of polysaccharides as described in claim 1, it is characterised in that above-mentioned technical process uses
Water be pure water, temperature is maintained at 18-35 DEG C.
3. a kind of preparation method of polysaccharides according to claim 1 or 2, it is characterised in that the aperture of above-mentioned ceramic membrane
For 50nm.
4. a kind of preparation method of polysaccharides according to claim 3, it is characterised in that above-mentioned organic film is by dividing
Son amount is the organic film of 200-6000 dalton.
5. a kind of preparation method of polysaccharides according to claim 4, it is characterised in that above-mentioned NF membrane is by dividing
Son amount is 200-2000 dalton NF membranes；Ultrafiltration membrane is by ultrafiltration membrane that molecular weight is 1000-6000 dalton.
6. a kind of preparation method of polysaccharides according to claim 5, it is characterised in that above-mentioned ceramic membrane, organic film mistake
The mistake film temperature of filter is less than 35 DEG C, crosses film pressure 0.2Mpa.
7. a kind of preparation method of polysaccharides according to claim 6, it is characterised in that above-mentioned concentration technology is to use
Low-temperature negative-pressure concentrates, and thickening temperature is not higher than 35 DEG C, concentrates pressure 0.8Mpa, is concentrated into 0.2-0.25 times of original volume.
8. a kind of preparation method of polysaccharides according to claim 7, it is characterised in that above-mentioned cleaning, immersion and stirring
Water used is pure water when extraction, and water temperature is at 30-35 DEG C.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109315668A (en) * | 2018-11-20 | 2019-02-12 | 中国科学院兰州化学物理研究所 | A kind of fructus lycii Radix Glycyrrhizae solid beverage and preparation method thereof |
| CN110801019A (en) * | 2019-12-02 | 2020-02-18 | 宁夏天仁枸杞生物科技股份有限公司 | Preparation method of lycium barbarum glycopeptide granules |
| CN110840964A (en) * | 2019-12-02 | 2020-02-28 | 宁夏天仁枸杞生物科技股份有限公司 | Preparation method of lycium barbarum glycopeptide |
| CN111419868A (en) * | 2019-01-09 | 2020-07-17 | 宁夏天仁枸杞生物科技股份有限公司 | Application of lycium barbarum polysaccharide in preparation of medicine or health-care product for repairing damaged nerves |
| CN111419869A (en) * | 2019-01-09 | 2020-07-17 | 宁夏天仁枸杞生物科技股份有限公司 | Application of lycium barbarum polysaccharide in preparation of medicine for preventing and treating eye diseases |
| CN111944072A (en) * | 2020-08-20 | 2020-11-17 | 宋现伟 | Wolfberry polysaccharide extraction method, wolfberry polysaccharide tablet and preparation method thereof |
| CN112006281A (en) * | 2020-08-23 | 2020-12-01 | 赣州禾绿康健生物技术有限公司 | Preparation device and process of micromolecular ginseng syrup |
| CN112521524A (en) * | 2020-12-24 | 2021-03-19 | 中国科学院兰州化学物理研究所 | Composition for synergistically reducing blood sugar by using lycium barbarum polysaccharide and acaudina molpadioides functional peptide |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109315668A (en) * | 2018-11-20 | 2019-02-12 | 中国科学院兰州化学物理研究所 | A kind of fructus lycii Radix Glycyrrhizae solid beverage and preparation method thereof |
| CN111419868A (en) * | 2019-01-09 | 2020-07-17 | 宁夏天仁枸杞生物科技股份有限公司 | Application of lycium barbarum polysaccharide in preparation of medicine or health-care product for repairing damaged nerves |
| CN111419869A (en) * | 2019-01-09 | 2020-07-17 | 宁夏天仁枸杞生物科技股份有限公司 | Application of lycium barbarum polysaccharide in preparation of medicine for preventing and treating eye diseases |
| CN110801019A (en) * | 2019-12-02 | 2020-02-18 | 宁夏天仁枸杞生物科技股份有限公司 | Preparation method of lycium barbarum glycopeptide granules |
| CN110840964A (en) * | 2019-12-02 | 2020-02-28 | 宁夏天仁枸杞生物科技股份有限公司 | Preparation method of lycium barbarum glycopeptide |
| CN111944072A (en) * | 2020-08-20 | 2020-11-17 | 宋现伟 | Wolfberry polysaccharide extraction method, wolfberry polysaccharide tablet and preparation method thereof |
| CN112006281A (en) * | 2020-08-23 | 2020-12-01 | 赣州禾绿康健生物技术有限公司 | Preparation device and process of micromolecular ginseng syrup |
| CN112521524A (en) * | 2020-12-24 | 2021-03-19 | 中国科学院兰州化学物理研究所 | Composition for synergistically reducing blood sugar by using lycium barbarum polysaccharide and acaudina molpadioides functional peptide |
| CN112521524B (en) * | 2020-12-24 | 2022-05-24 | 中国科学院兰州化学物理研究所 | Composition for synergistically reducing blood sugar by using lycium barbarum polysaccharide and acaudina molpadioides functional peptide |
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Application publication date: 20180720 |