CN107652373B - A kind of preparation method of low-molecular weight chitoglycan - Google Patents
A kind of preparation method of low-molecular weight chitoglycan Download PDFInfo
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- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0006—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
- C08B37/0024—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid beta-D-Glucans; (beta-1,3)-D-Glucans, e.g. paramylon, coriolan, sclerotan, pachyman, callose, scleroglucan, schizophyllan, laminaran, lentinan or curdlan; (beta-1,6)-D-Glucans, e.g. pustulan; (beta-1,4)-D-Glucans; (beta-1,3)(beta-1,4)-D-Glucans, e.g. lichenan; Derivatives thereof
- C08B37/0027—2-Acetamido-2-deoxy-beta-glucans; Derivatives thereof
- C08B37/003—Chitin, i.e. 2-acetamido-2-deoxy-(beta-1,4)-D-glucan or N-acetyl-beta-1,4-D-glucosamine; Chitosan, i.e. deacetylated product of chitin or (beta-1,4)-D-glucosamine; Derivatives thereof
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Abstract
The invention belongs to Degradation technologies of chitosan fields, and in particular to a kind of preparation method of low-molecular weight chitoglycan.The preparation method of low-molecular weight chitoglycan provided by the invention, including by chitosan be immersed in containing hydrogen peroxide, water-soluble humic acid solution in, after being soaked for a period of time, filtering, obtains filter residue, and gained filter residue is carried out freezing processing three times, it thaws, chitosan after defrosting is dried in the shade, fine powder is ground into, gained fine powder is carried out to radiation treatment at normal temperatures and pressures.Irradiation dose not only can be effectively reduced in the preparation method of low-molecular weight chitoglycan provided by the invention, but also products obtained therefrom narrow molecular weight distribution, molecular weight are low.
Description
Technical field
The invention belongs to Degradation technologies of chitosan fields, and in particular to a kind of preparation method of low-molecular weight chitoglycan.
Background technique
Chitosan is a kind of natural polymers, belongs to glycosaminoglycan, and scientific name is [(Isosorbide-5-Nitrae) -2- acetylaminohydroxyphenylarsonic acid 2-
Deoxidation-β-D-Glucose], it is the unique alkaline polysaccharide with cationic charge found up to now.Chitosan is in nature
It is widely present in unicellular lower eukaryote mushroom, the cell of algae, in the shell of section branch animal shrimp, crab, insect etc., the biofacies of chitosan
Capacitive is good, toxicity is low, biodegradable, is widely used in the fields such as food, medicine, health care, bioengineering.Chitosan is to a variety of
The growth of bacterium is inhibited, shows the feature of similar antibiotic.Chitosan can promote skin histology to heal and repair
It is multiple.Chitosan has anastalsis, and chitosan itself has anastalsis.Meanwhile chitosan passes through it between erythrocyte membrane
Interaction, hemostasis mainly is realized to the agglutination of red blood cell.Chitosan has film forming, and chitosan is with its hydrogen bond
It is cross-linked with each other and reticulates structure, be a kind of ideal film forming matter.The hemostasis of chitosan, antibacterial, antibiotic property, biocompatibility, rush
Its superperformance for being used as hemostatic material is assigned into wound healing and the property for being easily formed gel.Chitosan is widely present in
In the shrimp shell of nature, crab shell and fungi, although there is special bioactivity, since its molecular weight is big, poorly water-soluble, in people
It is not easy to be absorbed and be restricted its application in vivo.
Through obtained low-molecular weight chitoglycan of degrading, especially relative molecular mass is 1 × 104Oligopolymerization chitosan below
Sugar is not only soluble in water, also has unique physiological activity and physico-chemical property, thus application range is widened significantly.Such as oligopolymerization chitosan
Sugar, which has, promotes spleen antibody tormation, inhibits the physiological function of tumour growth；It can effectively reduce the cholesterol in liver and serum；
Liver function can be strengthened, prevent gout and gastric ulcer.In addition, it can also be used in food additives, immobilized enzyme, protein are mentioned
It is pure, paper industry and water treatment industry etc..Low-molecular weight chitoglycan preparation method has acid-hydrolysis method, oxidation degradation method, enzyme
Solution and irradiation method etc..Enzyme edman degradation Edman is to carry out biodegradable method to chitosan with specificity or non-specific enzyme, is used
This method can obtain the lower oligosaccharide of average relative molecular mass and monosaccharide.Add in entire degradation process without other reaction reagents
Enter, no other side reactions occur, and degradation condition is mild, and degradation process and molecular weight of product distribution are relatively easy to control.The disadvantage is that being made
Enzyme is more special, and the vigor of enzyme is limited, while at high cost, and the production cycle is long, is difficult to industrialized production.Mechanical degradation
Method is mainly using physics modes such as microwave, ultrasonic wave and gamma-rays come chitosan of degrading, and the most commonly used is sonications.It is super
Sonication is easy to operate, but 95% ultrasonic energy is used for system heat effect rather than product degradation effect, therefore degrades
Efficiency is lower, while having that molecular weight of product is distributed more widely, the higher problem of molecular weight.
Chinese patent application CN1563106A discloses the side that a kind of radiation method prepares small-molecular-weight or water soluble chitosan
Method, the solid or solution of the high molecular weight chitosan by purification are used60Co- gamma-rays carries out irradiation-induced degradation, and catabolite is through molten
The post-processing steps such as solution, decoloration obtain small-molecular-weight or water soluble chitosan.
Chinese patent application CN101481427A discloses a kind of shell of catalyzing oxidizing degrading chitosan preparation low molecular weight
(viscosity average molecular weigh is 1 × 10 to glycan4-7×103) method, the invention use with viscosity average molecular weigh be 1.4 × 106Chitosan is
Raw material, using the metal phthalocyanine of hydrophobic ionic liquid dissolution as catalyst, molecular oxygen is as oxidant, and reaction is made in a kettle
Standby its viscosity average molecular weigh of low-molecular weight chitoglycan is 1 × 104-7×103。
That currently, existing irradiation method prepares low-molecular weight chitoglycan, there are irradiation doses is big, product molecular weight distribution is wide etc.
Disadvantage.
Summary of the invention
In view of the deficiencies of the prior art, the purpose of the present invention is to provide a kind of preparation methods of low-molecular weight chitoglycan.
Irradiation dose, but also products obtained therefrom molecule not only can be effectively reduced in the preparation method of low-molecular weight chitoglycan provided by the invention
Narrowly distributing is measured, molecular weight is low.
The technical scheme is that：
A kind of preparation method of low-molecular weight chitoglycan, includes the following steps：
It is the hydrogenperoxide steam generator of 5-12% that S1, which takes mass concentration, and water-soluble humic acid, the matter of water-soluble humic acid is added
Amount is the 0.2-0.6% of above-mentioned hydrogenperoxide steam generator, stirs evenly, obtains mixed liquor；
Chitosan is immersed in mixed liquor obtained by step S1 by S2, and the mass concentration of chitosan is 25-35%, impregnates 30-
50min, filtering, obtains filter residue；
Filter residue obtained by step S2 is carried out freezing processing three times by S3, and first time cryogenic temperature is -4 DEG C, when freezing for the first time
Between be 2-4h, second cryogenic temperature is -10 DEG C, and second of cooling time is 1-3h, and third time cryogenic temperature is -19 DEG C, the
Cooling time is 40-60min three times, thaws, the filter residue after defrosting is dried in the shade, and is ground into fine powder, crosses 40-60 mesh, obtains fine powder；
Fine powder obtained by step S3 is carried out radiation treatment by S4 at normal temperatures and pressures, and irradiation dose 20-30kGy is dry, i.e.,
?.
Further, it is 10% hydrogenperoxide steam generator that the step S1, which takes mass concentration,.
Further, the quality of the step S1 water solubility humic acid is the 0.4% of above-mentioned hydrogenperoxide steam generator.
Further, the mass concentration of the step S2 chitosan is 30%.
Further, the step S2 impregnates 40min.
Further, the step S3 first time cooling time is 3h, and second of cooling time is 2h, when third time freezes
Between be 50min.
Further, the step S3 crosses 50 meshes.
Further, radiation source used is when the step S4 carries out radiation treatment60Co- gamma-rays, irradiation dose are
25kGy。
In the present invention, hydrogen peroxide can glycosidic bond in oxidation scission chitosan molecule chain, promote the drop of chitosan
Solution changes chitosan macromolecular depositing in system in addition, the addition of water-soluble humic acid can act synergistically with hydrogen peroxide
In state, and then the glycosidic bond in chitosan molecule chain is made to be detached from shielding, enhances free radical to a certain extent to attack site
The purpose of attack.In addition, will treated chitosan after freezing processing three times, the part of chitosan can not only be destroyed
Intermolecular hydrogen bonding changes the arrangement between chitosan molecule, reduces the binding force in chitosan molecule structure between molecule, will
The strand of chitosan is opened, its molecular structure is unfolded, and further promotes the degradation of chitosan, and pass through at freezing three times
After reason, the free volume being capable of increasing in chitosan is swollen amorphous area and crystalline region, makes amorphous area and crystalline region degradation journey
Degree synchronizes, so that the narrow molecular weight distribution of chitosan after processing, homogeneity is good.Finally, in the synergistic effect of high-energy ray
Under, by controlling radiation source, irradiation dose, to reach synergistic, guarantee that the degradation of chitosan effectively smoothly carries out, and
It realizes the molecular weight of catabolite and its control of distribution, obtains narrow molecular weight distribution, the low product of molecular weight.
Inventor has found through numerous studies, chitosan is passed through in the solution containing hydrogen peroxide, water-soluble humic acid impregnate,
Freezing and etc. processing after, the strand of chitosan can be opened, unfold its molecular structure, promote the degradation of chitosan,
So that irradiation dose is small, irradiation time is short, and product molecular weight distribution is narrow.In addition, carrying out spoke with chitosan fine powder after processing
According to processing, chitosan is solid state at this time, will not destroy the amino in chitosan molecule chain, be conducive to low-molecular weight chitoglycan
The holding of physiological activity, and molecular weight is easy to control.
Molecular weight determination shows the preparation method using low-molecular weight chitoglycan provided by the invention, preparation it is low
Molecular weight≤1985 of molecular weight chitosan, this explanation, the preparation method of the low-molecular weight chitoglycan provided through the invention obtain
The molecular weight of the low-molecular weight chitoglycan arrived is lower.
Dispersivity test the result shows that, using the preparation method of low-molecular weight chitoglycan provided by the invention, preparation it is low
Dispersion degree≤1.08 of molecular weight chitosan, dispersion degree are small.This explanation, the system of the low-molecular weight chitoglycan provided through the invention
The narrow molecular weight distribution for the low-molecular weight chitoglycan that Preparation Method obtains.
It is found through antibacterial tests, with the preparation method of low-molecular weight chitoglycan provided by the invention, the low molecular weight of preparation
Chitosan is to bacteriostasis rate >=96.8% of Escherichia coli, to bacteriostasis rate >=95.7% of bacillus subtilis, to golden yellow grape
Bacteriostasis rate >=96.6% of coccus.This explanation, the preparation method of the low-molecular weight chitoglycan provided through the invention obtain low
Molecular weight chitosan has stronger bacteriostatic activity.
Anti-fatigue test discovery, when the swimming of the mouse of the embodiment group of stomach-filling low-molecular weight chitoglycan prepared by the present invention
Between >=1.28min.It can be seen that the low molecular weight shell that the preparation method of the low-molecular weight chitoglycan provided through the invention obtains
Glycan has significant antifatigue effect.
Compared with prior art, the preparation method of low-molecular weight chitoglycan provided by the invention has the advantage that：
(1) narrow molecular weight distribution of the preparation method products obtained therefrom of the low-molecular weight chitoglycan provided through the invention, point
Son amount is low.
(2) preparation method of low-molecular weight chitoglycan provided by the invention can be effectively reduced irradiation dose, and can contract
The short irradiation time.
(3) preparation method of low-molecular weight chitoglycan provided by the invention is convenient, safety, economical, practical.
(4) preparation method of low-molecular weight chitoglycan provided by the invention will not destroy the amino in chitosan molecule chain,
Be conducive to the holding of low-molecular weight chitoglycan physiological activity.
Specific embodiment
The following describes the present invention further through the description of specific embodiments, but it is to limit of the invention that this, which is not,
System, those skilled in the art's basic thought according to the present invention can make various modifications or improvements, but without departing from this
The basic thought of invention, is all within the scope of the present invention.
Chitosan of the present invention is purchased from Zhejiang Yuhuan Marine Bio Co., Ltd., molecular weight 580,000, deacetylation 90%；Water
Dissolubility humic acid is purchased from Lingshou County Yu Feng mineral products processing factory, model C H6-5.
Embodiment 1, a kind of preparation method of low-molecular weight chitoglycan
The preparation method of the low-molecular weight chitoglycan, includes the following steps：
It is 5% hydrogenperoxide steam generator that S1, which takes mass concentration, and water-soluble humic acid is added, and the quality of water-soluble humic acid is
The 0.2% of above-mentioned hydrogenperoxide steam generator, stirs evenly, and obtains mixed liquor；
Chitosan is immersed in mixed liquor obtained by step S1 by S2, and the mass concentration of chitosan is 25%, impregnates 30min,
Filtering, obtains filter residue；
Filter residue obtained by step S2 is carried out freezing processing three times by S3, and first time cryogenic temperature is -4 DEG C, when freezing for the first time
Between be 2h, second cryogenic temperature is -10 DEG C, and second of cooling time is 1h, and third time cryogenic temperature is -19 DEG C, third time
Cooling time is 40min, thaws, the filter residue after defrosting is dried in the shade, and is ground into fine powder, crosses 40 meshes, obtains fine powder；
Fine powder obtained by step S3 is carried out radiation treatment by S4 at normal temperatures and pressures, irradiation dose 20kGy, it is dry to get.
The step S4 when carrying out radiation treatment radiation source used be60Co- gamma-rays.
Embodiment 2, a kind of preparation method of low-molecular weight chitoglycan
The preparation method of the low-molecular weight chitoglycan, includes the following steps：
It is 12% hydrogenperoxide steam generator that S1, which takes mass concentration, and water-soluble humic acid, the quality of water-soluble humic acid is added
It is the 0.6% of above-mentioned hydrogenperoxide steam generator, stirs evenly, obtain mixed liquor；
Chitosan is immersed in mixed liquor obtained by step S1 by S2, and the mass concentration of chitosan is 35%, impregnates 50min,
Filtering, obtains filter residue；
Filter residue obtained by step S2 is carried out freezing processing three times by S3, and first time cryogenic temperature is -4 DEG C, when freezing for the first time
Between be 4h, second cryogenic temperature is -10 DEG C, and second of cooling time is 3h, and third time cryogenic temperature is -19 DEG C, third time
Cooling time is 60min, thaws, the filter residue after defrosting is dried in the shade, and is ground into fine powder, crosses 60 meshes, obtains fine powder；
Fine powder obtained by step S3 is carried out radiation treatment by S4 at normal temperatures and pressures, irradiation dose 30kGy, it is dry to get.
The step S4 when carrying out radiation treatment radiation source used be60Co- gamma-rays.
Embodiment 3, a kind of preparation method of low-molecular weight chitoglycan
The preparation method of the low-molecular weight chitoglycan, includes the following steps：
It is 10% hydrogenperoxide steam generator that S1, which takes mass concentration, and water-soluble humic acid, the quality of water-soluble humic acid is added
It is the 0.4% of above-mentioned hydrogenperoxide steam generator, stirs evenly, obtain mixed liquor；
Chitosan is immersed in mixed liquor obtained by step S1 by S2, and the mass concentration of chitosan is 30%, impregnates 40min,
Filtering, obtains filter residue；
Filter residue obtained by step S2 is carried out freezing processing three times by S3, and first time cryogenic temperature is -4 DEG C, when freezing for the first time
Between be 3h, second cryogenic temperature is -10 DEG C, and second of cooling time is 2h, and third time cryogenic temperature is -19 DEG C, third time
Cooling time is 50min, thaws, the filter residue after defrosting is dried in the shade, and is ground into fine powder, crosses 50 meshes, obtains fine powder；
Fine powder obtained by step S3 is carried out radiation treatment by S4 at normal temperatures and pressures, irradiation dose 25kGy, it is dry to get.
The step S4 when carrying out radiation treatment radiation source used be60Co- gamma-rays.
Comparative example 1, a kind of preparation method of low-molecular weight chitoglycan
The preparation method of the low-molecular weight chitoglycan, includes the following steps：
It is 10% hydrogenperoxide steam generator that S1, which takes mass concentration, and water-soluble humic acid, the quality of water-soluble humic acid is added
It is the 0.4% of above-mentioned hydrogenperoxide steam generator, stirs evenly, obtain mixed liquor；
Chitosan is immersed in mixed liquor obtained by step S1 by S2, and the mass concentration of chitosan is 30%, impregnates 40min,
Filtering, obtains filter residue, gained filter residue is dried in the shade, and is ground into fine powder, crosses 50 meshes, obtains fine powder；
Fine powder obtained by step S2 is carried out radiation treatment by S3 at normal temperatures and pressures, irradiation dose 25kGy, it is dry to get.
The step S4 when carrying out radiation treatment radiation source used be60Co- gamma-rays.
The preparation method of the low-molecular weight chitoglycan is similar to Example 3.
As different from Example 3, freezing processing is not carried out to filter residue obtained by step S2.
Comparative example 2, a kind of preparation method of low-molecular weight chitoglycan
The preparation method of the low-molecular weight chitoglycan, includes the following steps：
Chitosan is dissolved in the acetic acid solution that pH value is 5.0 by S1, and the mass concentration for controlling chitosan is 22%, and stirring is equal
It is even, obtain chitosan solution；
Chitosan solution obtained by step S1 is placed in ultrasonic response kettle by S2, and ultrasonic response kettle is passed through circulating condensing
Water, control water temperature be no more than 50 DEG C, ultrasonic 0.5h, supersonic frequency 30kHz, obtain it is ultrasonic after solution；
Hydrogen peroxide is added into solution after ultrasound obtained by step S2 by S3, and the quality of hydrogen peroxide is chitosan mass
18%, ultrasound 1.2h, supersonic frequency 28kHz, then adds 50% hydrogen peroxide of chitosan mass again, stirs after mixing evenly
Ultrasound 1.5h after mixing uniformly, then acquired solution is filtered, filtrate pass through spray drying to get.
Comparative example 2 is to simulate existing preferred technique to carry out low-molecular weight chitoglycan preparation.
Comparative example 3, a kind of preparation method of low-molecular weight chitoglycan
The preparation method of the low-molecular weight chitoglycan is similar to Example 3.
As different from Example 3, water-soluble humic acid is not added by the step S2.
The measurement of test example one, molecular weight, dispersion degree
1, test material：Embodiment 1, embodiment 2, embodiment 3, comparative example 1, comparative example 2, comparative example 3 prepare low point
Son amount chitosan.
2, test method：
It is made with high performance liquid chromatograph measurement embodiment 1, embodiment 2, embodiment 3, comparative example 1, comparative example 2, comparative example 3
The molecular weight of standby low-molecular weight chitoglycan.
Determination condition is：Molecular weight, mobile phase 0.2MHAC+0.1MNaCl are surveyed with high performance liquid chromatography, flow velocity is
0.5mL/min, column temperature are 30 DEG C, 20 μ L of sample introduction, and chromatographic column is TSKG3000PW gel chromatographic columns.
3, test result：
Test result is as shown in Table 1 and Table 2.
Table 1：Molecular weight determination
| Group | Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative example 1 | Comparative example 2 | Comparative example 3 |
| Molecular weight | 1985 | 1942 | 1868 | 5632 | 3815 | 4525 |
As can be seen from Table 1, the molecule for the low-molecular weight chitoglycan that prepared by the embodiment of the present invention 1, embodiment 2, embodiment 3
Amount, hence it is evident that lower than the molecular weight of low-molecular weight chitoglycan prepared by comparative example 1, comparative example 2, comparative example 3.It can be seen that passing through
The molecular weight for the low-molecular weight chitoglycan that the preparation method of low-molecular weight chitoglycan provided by the invention obtains is lower.
Table 2：Dispersivity test result
| Group | Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative example 1 | Comparative example 2 | Comparative example 3 |
| Dispersion degree | 1.08 | 1.05 | 1.02 | 1.52 | 1.65 | 1.43 |
As can be seen from Table 2, the dispersion for the low-molecular weight chitoglycan that prepared by the embodiment of the present invention 1, embodiment 2, embodiment 3
Degree, hence it is evident that lower than the dispersion degree of low-molecular weight chitoglycan prepared by comparative example 1, comparative example 2, comparative example 3.This explanation, passes through this
The narrow molecular weight distribution for the low-molecular weight chitoglycan that the preparation method for the low-molecular weight chitoglycan that invention provides obtains.
Test example two, antibacterial tests
1, test material：Embodiment 1, embodiment 2, embodiment 3, comparative example 1, comparative example 2, comparative example 3 prepare low point
Son amount chitosan.
2, subjects：Escherichia coli, bacillus subtilis, staphylococcus aureus.
3, test method：
Test material is made into the low-molecular weight chitoglycan solution that mass fraction is 0.5% with distilled water, it is spare after sterilizing.
0.1mL bacterium solution and 0.1mL low-molecular weight chitoglycan solution is added in each antimicrobial flat-plate, be in blank plate with
The sterile water of 0.1mL replaces, and coating is uniform.It places and cultivates 18h in 37 DEG C of constant incubators, take out thin on each plate of identification
The growing state of bacterium.
The calculation formula of bacteriostasis rate is：η %=(N1—N2)/N1
Wherein：N1For the clump count of the bacterium on blank plate；
N2For the clump count for being coated with bacterium on the plate of low-molecular weight chitoglycan.
4, test result：
Test result is as shown in table 3.
Table 3：Bacteriostasis rate measurement result
As can be seen from Table 3, low-molecular weight chitoglycan made from the embodiment of the present invention 1, embodiment 2 and embodiment 3 is to big
Enterobacteria, bacillus subtilis, staphylococcus aureus all have significant inhibitory effect, and fungistatic effect is substantially better than comparative example
1, low-molecular weight chitoglycan made from comparative example 2 and comparative example 3.This explanation, the low-molecular weight chitoglycan provided through the invention
The obtained low-molecular weight chitoglycan of preparation method there is stronger bacteriostatic activity.
Test example three, anti-fatigue test
1, test material：Embodiment 1, embodiment 2, embodiment 3, comparative example 1, comparative example 2, comparative example 3 prepare low point
Son amount chitosan.
2, subjects：Healthy male kunming mouse 70,2 monthly ages, weight 20g.
3, test method：
70 mouse are randomly divided into seven groups, every group 10, respectively blank control group, example 1 group, 2 groups of embodiment,
3 groups of embodiment, 1 group of comparative example, 2 groups of comparative example, 3 groups of comparative example.
Example 1 group, 2 groups of embodiment, 3 groups of embodiment, 1 group of comparative example, 2 groups of comparative example, 3 groups of comparative example daily stomach-fillings are raw
Manage salt water 0.4mL, and respectively stomach-filling embodiment 1, embodiment 2, embodiment 3, comparative example 1, comparative example 2, comparative example 3 prepare it is low
Molecular weight chitosan 3g/kg, the physiological saline of the daily stomach-filling equivalent of blank control group, continuously feeds 15d.
It after last stomach-filling 1h, weighs respectively to each group mouse, then the weight bearing of every tail portion system weight 3%, is put into the depth of water
Carry out swimming test in 27 DEG C of 20cm, water temperature ponds, time that record mouse is persistently swum in water (it avales to mouse nostril,
Until inability floats).
4, test result is as shown in table 4.
Table 4：Anti-fatigue test result
As can be seen from Table 4, compared with 1 group of comparative example, 2 groups of comparative example, 3 groups of comparative example, 2 groups of example 1 group, embodiment
It is significantly higher with the swimming time of 3 groups of mouse of embodiment.It can be seen that the low-molecular weight chitoglycan provided through the invention
The low-molecular weight chitoglycan that preparation method obtains has significant antifatigue effect.
Claims (8)
1. a kind of preparation method of low-molecular weight chitoglycan, which is characterized in that include the following steps：
It is the hydrogenperoxide steam generator of 5-12% that S1, which takes mass concentration, and water-soluble humic acid is added, and the quality of water-soluble humic acid is
The 0.2-0.6% of above-mentioned hydrogenperoxide steam generator, stirs evenly, and obtains mixed liquor；
Chitosan is immersed in mixed liquor obtained by step S1 by S2, and the mass concentration of chitosan is 25-35%, impregnates 30-
50min, filtering, obtains filter residue；
Filter residue obtained by step S2 is carried out freezing processing three times by S3, and first time cryogenic temperature is -4 DEG C, and first time cooling time is
2-4h, second of cryogenic temperature are -10 DEG C, and second of cooling time is 1-3h, and third time cryogenic temperature is -19 DEG C, third time
Cooling time is 40-60min, thaws, the filter residue after defrosting is dried in the shade, and is ground into fine powder, crosses 40-60 mesh, obtains fine powder；
Fine powder obtained by step S3 is carried out radiation treatment by S4 at normal temperatures and pressures, irradiation dose 20-30kGy, it is dry to get.
2. the preparation method of low-molecular weight chitoglycan as described in claim 1, which is characterized in that the step S1 takes quality dense
The hydrogenperoxide steam generator that degree is 10%.
3. the preparation method of low-molecular weight chitoglycan as described in claim 1, which is characterized in that the step S1 is water-soluble rotten
The quality for growing acid is the 0.4% of above-mentioned hydrogenperoxide steam generator.
4. the preparation method of low-molecular weight chitoglycan as described in claim 1, which is characterized in that the step S2 chitosan
Mass concentration is 30%.
5. the preparation method of low-molecular weight chitoglycan as described in claim 1, which is characterized in that the step S2 impregnates
40min。
6. the preparation method of low-molecular weight chitoglycan as described in claim 1, which is characterized in that the step S3 is cold for the first time
The jelly time is 3h, and second of cooling time is 2h, and third time cooling time is 50min.
7. the preparation method of low-molecular weight chitoglycan as described in claim 1, which is characterized in that the step S3 crosses 50 mesh
Sieve.
8. the preparation method of low-molecular weight chitoglycan as described in claim 1, which is characterized in that the step S4 is irradiated
Radiation source used is when processing60Co- gamma-rays, irradiation dose 25kGy.
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| CN108586635A (en) * | 2018-05-10 | 2018-09-28 | 扬州日兴生物科技股份有限公司 | A method of preparing chitosan oligosaccharide |
| CN108675365A (en) * | 2018-05-30 | 2018-10-19 | 佛山市航祥千安科技有限公司 | A kind of preparation method of water purification agent |
| CN110128566B (en) * | 2019-04-30 | 2021-09-07 | 盐城工学院 | Near-infrared fluorescent polymer probe for identifying formaldehyde and preparation method and application thereof |
| CN110407955B (en) * | 2019-08-12 | 2021-09-14 | 浙江海洋大学 | Preparation method of water-soluble marine oligosaccharide |
| CN111670995B (en) * | 2020-06-08 | 2021-05-18 | 颜如玉医药科技有限公司 | Preparation method of wheat protein peptide |
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| CN1401652A (en) * | 2001-08-14 | 2003-03-12 | 华东理工大学 | Process for industrial production of oligochitose and chitooligose |
| CN1563106A (en) * | 2004-03-29 | 2005-01-12 | 中国科学院长春应用化学研究所 | Preparing water soluble chitosan or in small molecular weight through radiation method |
| CN102477106A (en) * | 2010-11-22 | 2012-05-30 | 大连创达技术交易市场有限公司 | Method for preparing water-soluble chitosan through radiation process |
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