CN115109169A - Preparation process of aminoglucomannan - Google Patents
Preparation process of aminoglucomannan Download PDFInfo
- Publication number
- CN115109169A CN115109169A CN202210898193.1A CN202210898193A CN115109169A CN 115109169 A CN115109169 A CN 115109169A CN 202210898193 A CN202210898193 A CN 202210898193A CN 115109169 A CN115109169 A CN 115109169A
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- China
- Prior art keywords
- glucomannan
- ammonia
- water
- aminoglucomannan
- tank body
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- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- LUEWUZLMQUOBSB-FSKGGBMCSA-N (2s,3s,4s,5s,6r)-2-[(2r,3s,4r,5r,6s)-6-[(2r,3s,4r,5s,6s)-4,5-dihydroxy-2-(hydroxymethyl)-6-[(2r,4r,5s,6r)-4,5,6-trihydroxy-2-(hydroxymethyl)oxan-3-yl]oxyoxan-3-yl]oxy-4,5-dihydroxy-2-(hydroxymethyl)oxan-3-yl]oxy-6-(hydroxymethyl)oxane-3,4,5-triol Chemical compound O[C@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1O[C@@H]1[C@@H](CO)O[C@@H](O[C@@H]2[C@H](O[C@@H](OC3[C@H](O[C@@H](O)[C@@H](O)[C@H]3O)CO)[C@@H](O)[C@H]2O)CO)[C@H](O)[C@H]1O LUEWUZLMQUOBSB-FSKGGBMCSA-N 0.000 claims abstract description 25
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 24
- 229920002581 Glucomannan Polymers 0.000 claims abstract description 24
- 229940046240 glucomannan Drugs 0.000 claims abstract description 24
- 239000000463 material Substances 0.000 claims abstract description 23
- 238000003756 stirring Methods 0.000 claims abstract description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000001035 drying Methods 0.000 claims abstract description 19
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 16
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 16
- 238000010521 absorption reaction Methods 0.000 claims abstract description 14
- 238000005086 pumping Methods 0.000 claims abstract description 12
- 239000008213 purified water Substances 0.000 claims abstract description 12
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000005119 centrifugation Methods 0.000 claims abstract description 8
- 238000004519 manufacturing process Methods 0.000 claims abstract description 8
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 4
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 4
- 238000004806 packaging method and process Methods 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 9
- 230000008569 process Effects 0.000 claims description 9
- 230000002829 reductive effect Effects 0.000 claims description 7
- 239000000126 substance Substances 0.000 claims description 4
- 239000012153 distilled water Substances 0.000 claims description 2
- 238000009776 industrial production Methods 0.000 abstract description 5
- 238000000746 purification Methods 0.000 abstract description 2
- 241000700605 Viruses Species 0.000 description 9
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 5
- 230000002401 inhibitory effect Effects 0.000 description 5
- 239000007788 liquid Substances 0.000 description 5
- 229920001282 polysaccharide Polymers 0.000 description 5
- 239000005017 polysaccharide Substances 0.000 description 5
- 238000005576 amination reaction Methods 0.000 description 4
- 230000000840 anti-viral effect Effects 0.000 description 4
- 210000004027 cell Anatomy 0.000 description 4
- 150000004676 glycans Chemical class 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000003814 drug Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000009471 action Effects 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 238000005915 ammonolysis reaction Methods 0.000 description 2
- 230000036039 immunity Effects 0.000 description 2
- 231100000053 low toxicity Toxicity 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000007935 neutral effect Effects 0.000 description 2
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 2
- 238000013518 transcription Methods 0.000 description 2
- 230000035897 transcription Effects 0.000 description 2
- 230000003612 virological effect Effects 0.000 description 2
- 108091032955 Bacterial small RNA Proteins 0.000 description 1
- 206010028980 Neoplasm Diseases 0.000 description 1
- 108010059722 Viral Fusion Proteins Proteins 0.000 description 1
- 108010067390 Viral Proteins Proteins 0.000 description 1
- 102000018265 Virus Receptors Human genes 0.000 description 1
- 108010066342 Virus Receptors Proteins 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000002155 anti-virotic effect Effects 0.000 description 1
- 230000006907 apoptotic process Effects 0.000 description 1
- 230000004071 biological effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 230000023555 blood coagulation Effects 0.000 description 1
- -1 cationic polysaccharide Chemical class 0.000 description 1
- 210000000170 cell membrane Anatomy 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 230000002147 killing effect Effects 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 108020004707 nucleic acids Proteins 0.000 description 1
- 102000039446 nucleic acids Human genes 0.000 description 1
- 150000007523 nucleic acids Chemical class 0.000 description 1
- 239000013612 plasmid Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000010076 replication Effects 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 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
- C08B37/006—Heteroglycans, i.e. polysaccharides having more than one sugar residue in the main chain in either alternating or less regular sequence; Gellans; Succinoglycans; Arabinogalactans; Tragacanth or gum tragacanth or traganth from Astragalus; Gum Karaya from Sterculia urens; Gum Ghatti from Anogeissus latifolia; Derivatives thereof
- C08B37/0087—Glucomannans or galactomannans; Tara or tara gum, i.e. D-mannose and D-galactose units, e.g. from Cesalpinia spinosa; Tamarind gum, i.e. D-galactose, D-glucose and D-xylose units, e.g. from Tamarindus indica; Gum Arabic, i.e. L-arabinose, L-rhamnose, D-galactose and D-glucuronic acid units, e.g. from Acacia Senegal or Acacia Seyal; Derivatives thereof
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Molecular Biology (AREA)
- General Health & Medical Sciences (AREA)
- Emergency Medicine (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 preparation process of aminoglucomannan, belonging to the field of preparation processes, comprising the following steps: preparing a stirring tank body, pumping purified water according to the production capacity in advance, slowly pouring glucomannan into the purified water, and stirring to completely dissolve the glucomannan in the purified water; pumping the gelatinized glucomannan solution into ammonia water or liquid ammonia, starting a stirring device after pumping to completely mix the ammonia water or liquid ammonia with the glucomannan gel, wherein the ammonia gas, water vapor and carbon dioxide flow with heat can be generated and absorbed by an absorption device; starting an ultrasonic device, and carrying out ultrasonic cavitation treatment on the materials in the stirring tank body; after the ultrasonic cavitation is finished, the materials are pumped into a vacuum centrifuge for centrifugal drying in a grading way; and (5) after the material centrifugation is finished, drying the material in a dryer, and then packaging the finished product. The invention can realize the industrial production of the aminoglucomannan and can ensure the production and purification purity of the aminoglucomannan.
Description
Technical Field
The invention relates to the field of preparation processes, and in particular relates to a preparation process of aminoglucomannan.
Background
Polysaccharides have a variety of biological activities: regulating immunity, resisting virus, resisting tumor, resisting radiation, reducing blood sugar, delaying aging, resisting blood coagulation, inducing apoptosis, etc. Polysaccharide antiviral can be achieved by inhibiting transcription and modification of transcription of viral genome, inhibiting replication of viral genome nucleic acid, and inhibiting synthesis and transport of viral protein. The carried negative charge directly acts with the surface of the virus, thereby inhibiting the infectivity of the virus or directly killing the virus to make the virus lose the infectivity. The polysaccharide as an antiviral medicament has good activity, can improve the immunity of organisms, has the characteristics of low toxicity and low medicament resistance, has wide medicinal prospect and has attracted high attention of the medical field.
Aminoglucomannan (AGM) is a cationic polysaccharide formed by amination of glucomannan. AGM can bind to negatively charged DNA molecules, bringing plasmid DNA and small RNAs into the cell across the cell membrane. The research proves that AGM can have a certain inhibiting effect on viruses such as HBV, RSV and the like, the action mechanism of AGM is mainly to inhibit the viruses by preventing virus adsorption, taking virus fusion protein as a target spot to be combined with a virus receptor, exerting the electrostatic action to inhibit the virus encapsidation and other ways, and AGM has no obvious toxic effect on cells when reaching the maximum concentration of 2.5um, so that the AGM is a safe, low-toxicity and high-efficiency antiviral medicament.
Currently, the industrial production of the aminoglucomannan is still in the blank field in China, and a formed industrial production process and a flow are not available, so that the aminoglucomannan is used as a polysaccharide substance with a great medical application prospect, can be industrially produced, is applied to the field of medical treatment and health, gives full play to the performance of the antiviral field, and makes an important contribution to the anti-virus process at home and abroad.
Disclosure of Invention
For the problems in the prior art, the preparation process of the aminoglucomannan provided by the invention can realize the industrial production of the aminoglucomannan and can ensure the production and purification purity of the aminoglucomannan.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows: a preparation process of aminoglucomannan comprises the following steps:
(1) preparing a stirring tank body, wherein the stirring tank body is provided with an absorption device and an ultrasonic device, pumping purified water according to the production quantity in advance, slowly pouring glucomannan into the purified water, and stirring for 15 minutes to ensure that the glucomannan is completely dissolved when meeting the purified water;
(2) pumping the gelled glucomannan solution into ammonia water or liquid ammonia, wherein the proportion of the pumped ammonia water or liquid ammonia is 8-10% of the weight of the total substances in the tank body, starting a stirring device to stir for 5-15 minutes after pumping, so that the ammonia water or liquid ammonia is completely mixed with the glucomannan gel, ammonia gas, water vapor and carbon dioxide flow with heat can be generated, and the air flow is absorbed by an absorption device;
(3) starting an ultrasonic device, and carrying out ultrasonic cavitation treatment on the materials in the stirring tank body;
(4) after the ultrasonic cavitation is finished, the materials are pumped into a vacuum centrifuge for centrifugal drying in batches;
(5) and (5) after the material centrifugation is finished, drying the material in a dryer, and then packaging the finished product.
Preferably, the glucomannan obtained in step (1) has a purity of 96% or more.
Preferably, the ultrasonic device in the step (3) requires power not lower than 20MHz, and ultrasonic cavitation is carried out for 60-120 min.
Preferably, the temperature of the vacuum centrifuge in the step (4) is 30 +/-2 ℃, the rotating speed is 1400rpm, and the centrifugal drying time is more than or equal to 120 min.
Preferably, the indication of the end of centrifugation in step (4) is that the pumping of 2/3 remains.
Preferably, the pH of the material is measured after the centrifugation in step (4).
Preferably, distilled water is appropriately added to the centrifuge of step (4) if the water content is reduced.
Preferably, the dryer is a crawler-type tunnel dryer.
Preferably, the drying temperature of the dryer is set to be 100-120 ℃, and the index of the end of the drying time is that the moisture content of the material is less than or equal to 10%.
Preferably, the absorption apparatus is an absorption tower.
The invention has the advantages that:
1. the invention realizes industrial production by amination of glucomannan by ammonia water or liquid ammonia, the cavitation effect of ultrasonic waves in liquid can generate instantaneous temperature of 5000 ℃, so that energy required by the reaction process is provided, the energy provided by ultrasonic cavitation can enable hydroxyl of glucomannan to carry out ammonolysis reaction in the ammonia water or the liquid ammonia, but the integral structure of sugar chains is not changed, only the exchange of the amino and the hydroxyl is carried out, the sugar chains are not broken, and the length is not changed.
2. According to the invention, free ammonia in the solution is reduced by the vacuum centrifuge, so that the pH value of the glucomannan after amination is reduced to about 7 from 9.0-11.0, and the nearly neutral AGM solution can be suitable for cells.
Detailed Description
The present invention is further described below to facilitate understanding by those skilled in the art.
A preparation process of aminoglucomannan comprises the following steps:
(1) preparing a stirring tank body, wherein the stirring tank body is provided with an absorption device and an ultrasonic device, the absorption device preferably adopts an absorption tower, purified water is pumped into the absorption tower in advance according to the production quantity, glucomannan with the purity of more than or equal to 96 percent is slowly poured into the purified water, the adding proportion is 0.18 to 0.22 percent, and the stirring is carried out for 15 minutes to ensure that the glucomannan is completely dissolved in the purified water;
(2) pumping the gelled glucomannan solution into ammonia water or liquid ammonia, wherein the proportion of the pumped ammonia water or liquid ammonia is 8-10 percent of the weight of the total substances in the tank body, starting a stirring device to stir for 5-15 minutes after the ammonia water or liquid ammonia is pumped into the tank body, so that the ammonia water or liquid ammonia is completely mixed with the glucomannan gel, ammonia gas, water vapor and carbon dioxide flow with heat can be generated, and the airflow is absorbed by an absorption device;
(3) starting an ultrasonic device, carrying out ultrasonic cavitation treatment on the materials in the stirring tank body, wherein the ultrasonic device requires power not lower than 20MHZ, and carrying out ultrasonic cavitation for 60-120min, the cavitation effect of ultrasonic waves in liquid can generate instantaneous temperature of 5000 ℃, so that energy required by the reaction process is provided, and the energy provided by the ultrasonic cavitation can enable hydroxyl of glucomannan to carry out ammonolysis reaction in ammonia water or liquid ammonia, but the integral structure of a sugar chain is not changed, only the exchange of amino and hydroxyl is carried out, the sugar chain is not broken, and the length is not changed;
(4) after the ultrasonic cavitation is finished, the material is pumped into a vacuum centrifuge for centrifugal drying in several times, the temperature of the vacuum centrifuge is 30 +/-2 ℃, the rotating speed is 1400rpm, the centrifugal drying time is more than or equal to 120min, distillation can be properly supplemented if the water content is reduced in the centrifugal process, the index of the centrifugal end is that the pumping of the material is stopped when the residual 2/3 is left, and the pH value of the material is required to be measured after the centrifugal end is finished, the free ammonia in the solution is reduced by the vacuum centrifuge, so that the pH value of the aminated glucomannan is reduced to about 7 from 9.0-11.0, and the nearly neutral AGM solution can be suitable for cells;
and (3) after the material centrifugation is finished, drying the material in a dryer, preferably a crawler-type tunnel dryer, setting the drying temperature of the dryer to be 100-120 ℃, and packaging the finished product after the drying time is finished, wherein the moisture content of the material is less than or equal to 10%.
The invention utilizes ammonia water or liquid ammonia which is an amination agent with the widest application to be mixed with glucomannan containing a large number of hydroxyl groups, ultrasonic waves are transmitted in a medium in the form of longitudinal waves, when ultrasonic waves with huge energy pass through liquid, extremely violent density change of the liquid is caused, a dense area is pressed, a sparse area is pulled, the capacity of the liquid for bearing pulling force is poorer, the sparse area can not bear the pulling force and is torn, a micro gap similar to vacuum is generated, a cavity is compressed and suddenly closed after a very short time, local high temperature, high pressure and discharge phenomena are generated, further, the instantaneous temperature of 5 kilo DEG C can be generated, and the energy required by the reaction process can be provided.
It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should also be understood that various alterations, modifications and/or variations can be made to the present invention by those skilled in the art after reading the technical content of the present invention, and all such equivalents fall within the protective scope defined by the claims of the present application.
Claims (10)
1. The preparation process of the aminoglucomannan is characterized by comprising the following steps:
(1) preparing a stirring tank body, wherein the stirring tank body is provided with an absorption device and an ultrasonic device, pumping purified water according to the production quantity in advance, slowly pouring glucomannan into the purified water, and stirring for 15 minutes to ensure that the glucomannan is completely dissolved when meeting the purified water;
(2) pumping the gelled glucomannan solution into ammonia water or liquid ammonia, wherein the proportion of the pumped ammonia water or liquid ammonia is 8-10% of the weight of the total substances in the tank body, starting a stirring device to stir for 5-15 minutes after pumping, so that the ammonia water or liquid ammonia is completely mixed with the glucomannan gel, ammonia gas, water vapor and carbon dioxide flow with heat can be generated, and the air flow is absorbed by an absorption device;
(3) starting an ultrasonic device, and carrying out ultrasonic cavitation treatment on the materials in the stirring tank body;
(4) after the ultrasonic cavitation is finished, the materials are pumped into a vacuum centrifuge for centrifugal drying in a grading way;
(5) and (5) after the material centrifugation is finished, drying the material in a dryer, and then packaging the finished product.
2. The process for preparing aminoglucomannan according to claim 1, wherein the purity of glucomannan in step (1) is not less than 96%.
3. The process of claim 1, wherein the ultrasonic cavitation is carried out for 60-120min at the power required by the ultrasonic device in step (3) not lower than 20 MHz.
4. The process for preparing aminoglucomannan according to claim 1, wherein the temperature of the vacuum centrifuge in step (4) is 30 ± 2 ℃, the rotation speed is 1400rpm, and the centrifugal drying time is not less than 120 min.
5. The process according to claim 1, wherein the end of centrifugation in step (4) is indicated by the time 2/3 is left.
6. The process according to claim 1, wherein the pH of the material is measured after the centrifugation step (4).
7. The process according to claim 1, wherein distilled water is added to the centrifuge of step (4) if the water content is reduced.
8. The process of claim 1, wherein the drying machine is a tracked tunnel drying machine.
9. The process of claim 1, wherein the drying temperature of the dryer is set at 100-120 ℃, and the end of the drying time is the moisture content of the material is less than or equal to 10%.
10. The process according to claim 1, wherein the absorption apparatus is an absorption tower.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210898193.1A CN115109169A (en) | 2022-07-28 | 2022-07-28 | Preparation process of aminoglucomannan |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210898193.1A CN115109169A (en) | 2022-07-28 | 2022-07-28 | Preparation process of aminoglucomannan |
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| Publication Number | Publication Date |
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| CN115109169A true CN115109169A (en) | 2022-09-27 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN202210898193.1A Pending CN115109169A (en) | 2022-07-28 | 2022-07-28 | Preparation process of aminoglucomannan |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN120209174A (en) * | 2025-05-30 | 2025-06-27 | 山东汇润膳食堂股份有限公司 | A method for preparing high-purity glucomannan |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101316865A (en) * | 2004-12-03 | 2008-12-03 | 科学与工业研究委员会 | Method for preparing biodegradable film from semi-refined kappa carrageenan |
| CN105669877A (en) * | 2016-01-29 | 2016-06-15 | 苏州求是本草健康科技有限公司 | Method for preparing high-purity glucomannan |
| CN112370419A (en) * | 2020-10-16 | 2021-02-19 | 江苏大学 | Preparation method of Pickering emulsion gel with alcohol-soluble protein, amino acid or/and polysaccharide synergistically stabilized |
| CN114380927A (en) * | 2022-02-28 | 2022-04-22 | 西南大学 | A kind of modified glucomannan and preparation method thereof |
-
2022
- 2022-07-28 CN CN202210898193.1A patent/CN115109169A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101316865A (en) * | 2004-12-03 | 2008-12-03 | 科学与工业研究委员会 | Method for preparing biodegradable film from semi-refined kappa carrageenan |
| CN105669877A (en) * | 2016-01-29 | 2016-06-15 | 苏州求是本草健康科技有限公司 | Method for preparing high-purity glucomannan |
| CN112370419A (en) * | 2020-10-16 | 2021-02-19 | 江苏大学 | Preparation method of Pickering emulsion gel with alcohol-soluble protein, amino acid or/and polysaccharide synergistically stabilized |
| CN114380927A (en) * | 2022-02-28 | 2022-04-22 | 西南大学 | A kind of modified glucomannan and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 刘永康: "氨基葡甘露聚糖跨细胞膜转运的研究", 《中国优秀博硕士学位论文全文数据库（硕士） 基础科学辑》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN120209174A (en) * | 2025-05-30 | 2025-06-27 | 山东汇润膳食堂股份有限公司 | A method for preparing high-purity glucomannan |
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Application publication date: 20220927 |