CN115645603A - Medical antibacterial hydrogel and preparation method thereof - Google Patents
Medical antibacterial hydrogel and preparation method thereof Download PDFInfo
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- CN115645603A CN115645603A CN202211375006.8A CN202211375006A CN115645603A CN 115645603 A CN115645603 A CN 115645603A CN 202211375006 A CN202211375006 A CN 202211375006A CN 115645603 A CN115645603 A CN 115645603A
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- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 48
- 239000000017 hydrogel Substances 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- PTHCMJGKKRQCBF-UHFFFAOYSA-N Cellulose, microcrystalline Chemical class OC1C(O)C(OC)OC(CO)C1OC1C(O)C(O)C(OC)C(CO)O1 PTHCMJGKKRQCBF-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000003242 anti bacterial agent Substances 0.000 claims abstract description 24
- 239000007863 gel particle Substances 0.000 claims abstract description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000001866 hydroxypropyl methyl cellulose Substances 0.000 claims abstract description 23
- 235000010979 hydroxypropyl methyl cellulose Nutrition 0.000 claims abstract description 23
- 229920003088 hydroxypropyl methyl cellulose Polymers 0.000 claims abstract description 23
- UFVKGYZPFZQRLF-UHFFFAOYSA-N hydroxypropyl methyl cellulose Chemical compound OC1C(O)C(OC)OC(CO)C1OC1C(O)C(O)C(OC2C(C(O)C(OC3C(C(O)C(O)C(CO)O3)O)C(CO)O2)O)C(CO)O1 UFVKGYZPFZQRLF-UHFFFAOYSA-N 0.000 claims abstract description 23
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims abstract description 21
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 21
- 239000011734 sodium Substances 0.000 claims abstract description 21
- 229920001661 Chitosan Polymers 0.000 claims abstract description 12
- MQWFLKHKWJMCEN-UHFFFAOYSA-N n'-[3-[dimethoxy(methyl)silyl]propyl]ethane-1,2-diamine Chemical compound CO[Si](C)(OC)CCCNCCN MQWFLKHKWJMCEN-UHFFFAOYSA-N 0.000 claims abstract description 12
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 claims abstract description 11
- 125000002057 carboxymethyl group Chemical group [H]OC(=O)C([H])([H])[*] 0.000 claims abstract description 11
- 239000000499 gel Substances 0.000 claims description 89
- 239000000243 solution Substances 0.000 claims description 70
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 63
- 239000011159 matrix material Substances 0.000 claims description 32
- 239000011259 mixed solution Substances 0.000 claims description 31
- 238000003756 stirring Methods 0.000 claims description 23
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 15
- 238000002156 mixing Methods 0.000 claims description 13
- 238000006243 chemical reaction Methods 0.000 claims description 11
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 10
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 10
- 238000004108 freeze drying Methods 0.000 claims description 10
- 239000008055 phosphate buffer solution Substances 0.000 claims description 10
- 239000000843 powder Substances 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 8
- 230000003647 oxidation Effects 0.000 claims description 7
- 238000007254 oxidation reaction Methods 0.000 claims description 7
- 238000010025 steaming Methods 0.000 claims description 7
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims description 6
- 239000000661 sodium alginate Substances 0.000 claims description 6
- 235000010413 sodium alginate Nutrition 0.000 claims description 6
- 229940005550 sodium alginate Drugs 0.000 claims description 6
- 238000005520 cutting process Methods 0.000 claims description 5
- 238000004821 distillation Methods 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- 238000004080 punching Methods 0.000 claims description 5
- 238000005096 rolling process Methods 0.000 claims description 5
- 238000002791 soaking Methods 0.000 claims description 5
- 238000004321 preservation Methods 0.000 claims description 3
- 238000007865 diluting Methods 0.000 claims description 2
- 230000005855 radiation Effects 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 239000012295 chemical reaction liquid Substances 0.000 claims 1
- 230000001590 oxidative effect Effects 0.000 abstract description 7
- 239000002994 raw material Substances 0.000 abstract description 7
- 125000004029 hydroxymethyl group Chemical group [H]OC([H])([H])* 0.000 abstract description 6
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 abstract description 6
- 125000003172 aldehyde group Chemical group 0.000 abstract description 5
- 238000006460 hydrolysis reaction Methods 0.000 abstract description 3
- 229920002678 cellulose Polymers 0.000 abstract description 2
- 239000001913 cellulose Substances 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract description 2
- 230000001276 controlling effect Effects 0.000 description 18
- 238000012360 testing method Methods 0.000 description 18
- 208000027418 Wounds and injury Diseases 0.000 description 12
- 206010052428 Wound Diseases 0.000 description 9
- 238000000034 method Methods 0.000 description 9
- 229920000247 superabsorbent polymer Polymers 0.000 description 8
- 238000005303 weighing Methods 0.000 description 8
- 238000005273 aeration Methods 0.000 description 6
- 230000008569 process Effects 0.000 description 6
- 230000003385 bacteriostatic effect Effects 0.000 description 5
- 230000006378 damage Effects 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 238000004140 cleaning Methods 0.000 description 4
- 238000002390 rotary evaporation Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 241000191967 Staphylococcus aureus Species 0.000 description 3
- 230000009471 action Effects 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 239000012213 gelatinous substance Substances 0.000 description 3
- 208000014674 injury Diseases 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 230000001105 regulatory effect Effects 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- 229920001817 Agar Polymers 0.000 description 2
- 241000588724 Escherichia coli Species 0.000 description 2
- 239000008272 agar Substances 0.000 description 2
- 239000007853 buffer solution Substances 0.000 description 2
- 238000012258 culturing Methods 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
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- 239000000203 mixture Substances 0.000 description 2
- 206010061218 Inflammation Diseases 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- -1 amino cellulose gel Chemical compound 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 229940124350 antibacterial drug Drugs 0.000 description 1
- 230000001580 bacterial effect Effects 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 238000001804 debridement Methods 0.000 description 1
- 230000003467 diminishing effect Effects 0.000 description 1
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 230000002439 hemostatic effect Effects 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 230000004054 inflammatory process Effects 0.000 description 1
- 230000009545 invasion Effects 0.000 description 1
- 238000000968 medical method and process Methods 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 239000004005 microsphere Substances 0.000 description 1
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- 238000011056 performance test Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- SCPYDCQAZCOKTP-UHFFFAOYSA-N silanol Chemical compound [SiH3]O SCPYDCQAZCOKTP-UHFFFAOYSA-N 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
Landscapes
- Materials For Medical Uses (AREA)
Abstract
The invention relates to medical antibacterial hydrogel and a preparation method thereof, and belongs to the technical field of negative pressure drainage dressings. The antibacterial hydrogel comprises the following components in parts by weight: 40-55 parts of aminated cellulose gel particles, 1-5 parts of carboxymethyl chitosan, 3-6 parts of antibacterial agent and 1-8 parts of SAP micropowder, wherein the aminated cellulose gel particles are prepared by taking hydroxypropyl methyl cellulose as a raw material, grafting 3- (2-aminoethylamino) propyl methyl dimethoxy silane onto molecules of hydroxypropyl methyl cellulose through hydrolysis reaction in an alkaline alcohol-water environment, introducing amino with higher activity onto the molecules of the hydroxypropyl methyl cellulose, and using sodium aescinate as the raw material of the antibacterial agent, oxidizing hydroxymethyl on the sodium aescinate into aldehyde groups by using ozone matched with ultraviolet irradiation to react with the amino on the aminated cellulose gel molecules, fixing the sodium aescinate on the molecules of the aminated cellulose, thus the long-acting antibacterial effect can be achieved, and the antibacterial agent can be applied to negative pressure drainage dressings.
Description
Technical Field
The invention belongs to the technical field of negative pressure drainage dressings, and particularly relates to medical antibacterial hydrogel and a preparation method thereof.
Background
The skin is the largest organ of the human body and is a natural barrier for maintaining the stability of the environment in the body and preventing the invasion of microorganisms; however, the large area of the skin is exposed to the outside, so that the skin is easily damaged by external injuries such as burns and mechanical injuries. The traditional medical method is to use materials such as gauze, hemostatic cloth and the like to wrap the wound, and because the materials have poor protective performance and are easy to adhere to the wound, and patients feel pain during dressing change, gel dressing is developed, and a small amount of antibacterial drugs are added into the gel to achieve the antibacterial effect, for example, chinese patent CN111494702B discloses an antibacterial hydrogel and a preparation method and application thereof, and sodium alginate microspheres loaded with nano silver are added into methacrylated chitosan hydrogel to achieve the slow-release antibacterial effect.
In order to facilitate the cleaning of wounds, dressings capable of conducting negative pressure drainage are developed in the prior art, a negative pressure source is arranged on the surface of a gel matrix, medicines and cleaning liquid are introduced into the gel dressings through a catheter, the wounds are treated, but the strength of the existing gel dressings after being soaked is not high, the existing gel dressings are easy to deform during negative pressure cleaning, the degree of fit between the dressings and the wounds is influenced, the existing dressing antibacterial materials are easily separated from the gel matrix, the antibacterial effect is reduced after the dressing is washed, the gel dressings need to be replaced after general debridement and administration, secondary injury is easily caused to the wounds, and the working strength of medical workers is increased.
Disclosure of Invention
In order to solve the technical problems mentioned in the background art, the invention aims to provide a medical antibacterial hydrogel and a preparation method thereof.
The purpose of the invention can be realized by the following technical scheme:
a medical antibacterial hydrogel comprises 40-55 parts of aminated cellulose gel particles, 1-5 parts of carboxymethyl chitosan, 3-6 parts of antibacterial agent and 1-8 parts of SAP micro powder;
the aminated cellulose gel particles are prepared by the following steps:
step A1: taking hydroxypropyl methylcellulose and an ethanol solution, stirring until the hydroxypropyl methylcellulose and the ethanol solution are completely dissolved, and then dropwise adding ammonia water to adjust the pH value of the dissolved solution to 8.2-8.7 to prepare a mixed solution a;
step A2: taking 3- (2-aminoethylamino) propyl-methyldimethoxysilane, and stirring and diluting the 3- (2-aminoethylamino) propyl-methyldimethoxysilane with an ethanol solution to prepare a mixed solution b;
step A3: heating the mixed solution a to 38-45 ℃ in a stirring water bath, keeping stirring, slowly adding the mixed solution b dropwise, hydrolyzing 3- (2-aminoethylamino) propyl methyldimethoxysilane into silanol under an alkaline environment, then reacting with hydroxyl on hydroxypropyl methyl cellulose molecules, grafting the 3- (2-aminoethylamino) propyl methyldimethoxysilane onto the molecules of the hydroxypropyl methyl cellulose, introducing amino on the hydroxypropyl methyl cellulose, controlling the reaction time to be 20-40min, generating a gelatinous substance, centrifuging the reaction solution, taking down the gel layer, and obtaining the prefabricated gel;
step A4: and (3) putting the preformed gel into a freeze dryer for freeze drying for 24 hours, taking out the preformed gel and putting the preformed gel into a grinder for grinding to prepare the aminated cellulose gel particles.
Furthermore, the mass ratio of the hydroxypropyl methylcellulose to the 3- (2-aminoethylamino) propyl-methyldimethoxysilane is 1.
Further, the particle size of the aminated cellulose gel particles is 0.2-1mm.
The antibacterial agent is prepared by the following steps:
step B1: dissolving sodium aescinate and an ethanol solution by stirring, dropwise adding acetic acid to adjust the pH value of the solution to 5, adding sodium alginate to adjust the viscosity of the solution to 500-800cP at room temperature, slowly introducing ozone into the mixed solution under ultraviolet irradiation, and oxidizing hydroxymethyl on the sodium aescinate into aldehyde groups under the oxidation action of the ozone to prepare an oxidizing solution;
and step B2: adjusting pH of the oxidation solution to 7 with ammonia water, removing part of solvent by rotary evaporation under reduced pressure, and freeze drying to obtain the antibacterial agent.
Furthermore, the ultraviolet wavelength of the ultraviolet radiation is 100-300nm, the ozone introducing speed is 0.18-0.25vvm, and the introducing time is 60-80min.
A preparation method of medical antibacterial hydrogel comprises the following steps:
step S1: putting the aminated cellulose gel particles, carboxymethyl chitosan, an antibacterial agent and SAP micro powder into a mixing machine, uniformly mixing, adding an ethanol solution, uniformly stirring, then carrying out water bath heat preservation at the temperature of 58-65 ℃ for 20-30min, softening the aminated cellulose gel particles into gel when meeting water, reacting amino and carboxymethyl chitosan on the surface with aldehyde groups on the antibacterial agent, combining the aminated cellulose gel, carboxymethyl chitosan and the antibacterial agent together, and filtering to obtain a gel matrix;
step S2: placing the gel matrix into a mold, flatly paving, transferring the mold and the gel matrix into a reduced pressure distillation kettle, removing part of water and ethanol, removing bubbles from the gel matrix, rolling out for forming, and punching to obtain a gel sheet;
and step S3: and cutting the gel sheet, and then putting the gel sheet into PBS buffer solution for soaking and softening to obtain the medical antibacterial hydrogel.
The invention has the beneficial effects that:
1. according to the aminated cellulose gel particles, hydroxypropyl methyl cellulose is used as a raw material, 3- (2-aminoethylamino) propyl methyldimethoxysilane is grafted to molecules of hydroxypropyl methyl cellulose through a hydrolysis reaction in an alkaline alcohol-water environment, amino with high activity is introduced to the molecules of the hydroxypropyl methyl cellulose, and simultaneously introduced siloxane is hydrolyzed, so that the crosslinking degree of gel is improved, the matrix strength of the gel is improved, the capacity of the gel for resisting external force damage and the capacity of the gel for resisting deformation under the action of external force are improved, and the gel is suitable for external drainage dressings.
2. According to the antibacterial agent, sodium aescinate is used as a raw material, ozone is used for being matched with ultraviolet irradiation, hydroxymethyl on the sodium aescinate is oxidized into aldehyde groups, the aldehyde groups react with amino groups introduced on amino cellulose gel molecules in the process of preparing gel, the sodium aescinate is fixed on the amino cellulose molecules, the sodium aescinate is prevented from entering wounds along with drainage fluid and is pasted on the surfaces of the wounds, the wounds can be subjected to inflammation diminishing, the sodium aescinate is combined with the gel in a grafting mode and is not easy to lose, a long-acting antibacterial effect can be achieved, the sodium aescinate is applied to negative pressure drainage dressings, cleaning liquid is introduced through negative pressure, and the long-term use can be achieved.
3. The invention adopts the mixing of the tiny aminated cellulose gel particles, the antibacterial agent and the carboxymethyl chitosan, the continuous hydrolysis is carried out through the water bath heat preservation to prepare the gel matrix, the gel matrix is decompressed, steamed in a rotary manner and rolled to form the gel sheet, the density of the gel is improved, the gel can be used after being cut and soaked according to the use environment of the gel, and the operation of changing the medicine is simpler.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The embodiment of preparing the medical antibacterial hydrogel comprises the following specific implementation processes:
the first step is to prepare aminated cellulose gel particles:
A1. heating 3L of 30 mass percent ethanol solution in a stirrer to 40 ℃, weighing 200g of hydroxypropyl methyl cellulose, slowly adding the hydroxypropyl methyl cellulose into the ethanol solution under the stirring state, stirring until the hydroxypropyl methyl cellulose is completely dissolved, then adding ammonia water into the stirrer to adjust the pH value of the dissolved solution to be 8.2, and marking as a mixed solution a;
A2. weighing 12g of 3- (2-aminoethylamino) propyl-methyldimethoxysilane and 150g of ethanol solution with the mass fraction of 60 percent, adding the mixture into a stirrer, and mixing for 10min to obtain mixed solution b;
A3. adding the mixed solution a into a water bath reactor, regulating and controlling the temperature of the mixed solution a to be 38 ℃, controlling the rotating speed to be 300rpm after the temperature is constant, slowly dropwise adding the mixed solution b into the mixed solution a, controlling the dropwise adding time to be 40min, generating a gel substance in the reactor, transferring the reaction solution into a centrifugal machine, centrifuging for 10min, leading out the solution on the upper layer, and taking out the gel on the lower layer to obtain a prefabricated gel;
A4. placing the preformed gel in a freeze dryer, setting the temperature of a cold trap at-20 ℃, freeze-drying for 24h, taking out the freeze-dried hard gel, placing the freeze-dried hard gel in a high-speed blade type crusher, and crushing until the particle size is about 1mm to obtain the aminated cellulose gel particles.
Step two, preparing an antibacterial agent:
B1. taking 15g of sodium aescinate and 120g of ethanol solution with the mass fraction of 80% and stirring until the sodium aescinate and the ethanol solution are completely dissolved, dropwise adding acetic acid solution to adjust the pH value of the solution to 5, then slowly adding sodium alginate and stirring until the viscosity of the solution is 500cP, increasing the viscosity to facilitate full aeration reaction, installing an aeration pipe in the solution, placing the solution in ultraviolet irradiation equipment, introducing ozone into the mixed solution at the medium ultraviolet ray wavelength of 200-300nm at the ozone introduction rate of 0.25vvm for 60min, and oxidizing hydroxymethyl on sodium aescinate molecules to prepare an oxidized solution;
B2. adjusting pH of the oxidation solution to about 7 with ammonia water, vacuumizing to-0.1 MPa at 80 deg.C, rotary steaming under reduced pressure for 30min, taking out rotary steaming product, placing into a freeze drier, setting cold trap temperature to-20 deg.C, and freeze drying for 24 hr to obtain the antibacterial agent.
Step three, preparing medical antibacterial hydrogel:
s1, weighing 200g of aminated cellulose gel particles, 25g of commercially available carboxymethyl chitosan, 15g of antibacterial agent and 5g of commercially available SAP (super absorbent polymer) micro powder (with the calibration fineness of 100 meshes), adding the raw materials into a powder mixer, mixing for 10min, transferring into a water bath reaction kettle, adding 6L of ethanol solution with the mass fraction of 30%, stirring and mixing uniformly, heating the water bath to 58 ℃, keeping the temperature of the water bath for 30min, generating gel substances again, and filtering out gel to obtain a gel matrix;
s2, placing the gel matrix into a mold, flatly paving, controlling the thickness to be about 5mm, then transferring the mold and the gel matrix into a reduced pressure distillation kettle, vacuumizing to-0.1 MPa, controlling the temperature to be 80 ℃, carrying out reduced pressure rotary evaporation for 50min, removing partial water and ethanol to enable the gel matrix to be in a solidified state, then taking out and placing the gel matrix into a roller mill, controlling the roller temperature to be 60 ℃ and the roller interval to be 2mm, rolling the gel matrix in the solidified state into a sheet shape, and then punching to obtain a gel sheet;
and S3, cutting the gel sheet into a designed size, and then soaking in a PBS (phosphate buffer solution) for 10min to obtain the medical antibacterial hydrogel.
Example 2
The embodiment of the preparation of the medical antibacterial hydrogel comprises the following specific implementation processes:
the first step is to prepare aminated cellulose gel particles:
A1. heating 3.3L of 30 mass percent ethanol solution in a stirrer to 40 ℃, weighing 230g of hydroxypropyl methyl cellulose, slowly adding the hydroxypropyl methyl cellulose into the ethanol solution under the stirring state, stirring until the hydroxypropyl methyl cellulose is completely dissolved, then adding ammonia water into the stirrer to adjust the pH value of the dissolved solution to be 8.5, and marking as a mixed solution a;
A2. weighing 18.4g of 3- (2-aminoethylamino) propyl methyldimethoxysilane and 200g of 60% ethanol solution, adding into a stirrer, and mixing for 12min, and marking as mixed solution b;
A3. adding the mixed solution a into a water bath reactor, regulating the temperature of the mixed solution a to be 42 ℃, controlling the rotating speed to be 300rpm after the temperature is constant, slowly dropwise adding the mixed solution b into the mixed solution a, controlling the dropwise adding time to be 30min, generating a gel substance in the reactor, transferring the reaction solution into a centrifuge, centrifuging for 10min, leading out the solution on the upper layer, and taking out the gel on the lower layer to obtain a prefabricated gel;
A4. and (3) placing the prefabricated gel in a freeze dryer, setting the temperature of a cold trap at-20 ℃, freeze-drying for 24 hours, taking out the freeze-dried hard gel, and putting the gel into a high-speed blade type crusher for crushing until the particle size is about 0.5mm, thus obtaining the aminated cellulose gel particles.
Step two, preparing an antibacterial agent:
B1. taking 22g of sodium aescinate and 200g of an ethanol solution with the mass fraction of 80%, stirring until the sodium aescinate and the ethanol solution are completely dissolved, dropwise adding an acetic acid solution to adjust the pH value of the solution to 5, then slowly adding sodium alginate, stirring until the viscosity of the solution is 700cP, increasing the viscosity to facilitate full aeration reaction, installing an aeration pipe in the solution, placing the solution in an ultraviolet irradiation device, introducing ozone into the mixed solution at the wavelength of 100-200nm at the ultraviolet ray vacuum ultraviolet ray speed of 0.2vvm for 70min, and oxidizing hydroxymethyl on sodium aescinate molecules to obtain an oxidized solution;
B2. adjusting pH of the oxidation solution to about 7 with ammonia water, vacuumizing to-0.1 MPa at 80 deg.C, rotary steaming under reduced pressure for 35min, taking out rotary steaming product, placing into a freeze drier, setting cold trap temperature to-20 deg.C, and freeze drying for 24 hr to obtain the antibacterial agent.
Step three, preparing medical antibacterial hydrogel:
s1, weighing 240g of aminated cellulose gel particles, 18g of commercially available carboxymethyl chitosan, 24g of antibacterial agent and 18g of commercially available SAP (super absorbent polymer) micro powder (with the calibration fineness of 100 meshes), adding the raw materials into a powder mixer, mixing for 10min, transferring into a water bath reaction kettle, adding 7L of ethanol solution with the mass fraction of 30%, stirring and mixing uniformly, heating the water bath to 62 ℃, keeping the temperature of the water bath for 25min, generating a gelatinous substance again, and filtering out gel to obtain a gel matrix;
s2, placing the gel matrix into a mold, flatly paving, controlling the thickness to be about 5mm, then transferring the mold and the gel matrix into a reduced pressure distillation kettle, vacuumizing to-0.1 MPa, controlling the temperature to be 80 ℃, carrying out reduced pressure rotary evaporation for 50min, removing partial water and ethanol to enable the gel matrix to be in a solidified state, then taking out and placing the gel matrix into a roller mill, controlling the roller temperature to be 60 ℃ and the roller interval to be 2mm, rolling the gel matrix in the solidified state into a sheet shape, and then punching to obtain a gel sheet;
and S3, cutting the gel sheet into a designed size, and then soaking in a PBS (phosphate buffer solution) for 10min to obtain the medical antibacterial hydrogel.
Example 3
The embodiment of preparing the medical antibacterial hydrogel comprises the following specific implementation processes:
the first step is to prepare aminated cellulose gel particles:
A1. heating 3.8L of 30 mass percent ethanol solution in a stirrer to 40 ℃, weighing 260g of hydroxypropyl methylcellulose, slowly adding the hydroxypropyl methylcellulose into the ethanol solution under the stirring state, stirring until the hydroxypropyl methylcellulose is completely dissolved, then adding ammonia water into the stirrer to adjust the pH value of the dissolved solution to 8.7, and marking as mixed solution a;
A2. 26g of 3- (2-aminoethylamino) propyl-methyldimethoxysilane and 230g of 60% ethanol solution are weighed and added into a stirrer to be mixed for 15min, and the mixture is marked as mixed solution b;
A3. adding the mixed solution a into a water bath reactor, regulating and controlling the temperature of the mixed solution a to be 45 ℃, controlling the rotating speed to be 300rpm after the temperature is constant, slowly dropwise adding the mixed solution b into the mixed solution a, controlling the dropwise adding time to be 20min, generating a gel substance in the reactor, transferring the reaction solution into a centrifugal machine, centrifuging for 10min, leading out the solution on the upper layer, and taking out the gel on the lower layer to obtain a prefabricated gel;
A4. placing the preformed gel in a freeze dryer, setting the temperature of a cold trap at-20 ℃, freeze-drying for 24h, taking out the freeze-dried hard gel, placing the freeze-dried hard gel in a high-speed blade type crusher, and crushing until the particle size is about 0.2mm to obtain the aminated cellulose gel particles.
Step two, preparing an antibacterial agent:
B1. stirring 28g of sodium aescinate and 250g of 80% ethanol solution by mass until the sodium aescinate and the ethanol solution are completely dissolved, dropwise adding an acetic acid solution to adjust the pH value of the solution to 5, then slowly adding sodium alginate, stirring until the viscosity of the solution is 800cP, increasing the viscosity to facilitate full aeration reaction, installing an aeration pipe in the solution, placing the solution in an ultraviolet irradiation device, introducing ozone into the mixed solution at the wavelength of 100-200nm at the ultraviolet ray vacuum ultraviolet ray rate of 0.18vvm for 80min, and oxidizing hydroxymethyl on the sodium aescinate molecule to prepare an oxidizing solution;
B2. adjusting pH of the oxidation solution to about 7 with ammonia water, vacuumizing to-0.1 MPa at 80 deg.C, rotary steaming under reduced pressure for 40min, taking out rotary steaming product, placing into a freeze drier, setting cold trap temperature to-20 deg.C, and freeze drying for 24 hr to obtain the antibacterial agent.
Step three, preparing medical antibacterial hydrogel:
s1, weighing 275g of aminated cellulose gel particles, 5g of commercially available carboxymethyl chitosan, 30g of antibacterial agent and 40g of commercially available SAP (super absorbent Polymer) micro powder (with the nominal fineness of 100 meshes), adding the raw materials into a powder mixer, mixing for 15min, transferring into a water bath reaction kettle, adding 8.6L of ethanol solution with the mass fraction of 30%, stirring and mixing uniformly, heating in a water bath to 65 ℃, keeping the temperature in the water bath for 20min, generating gelatinous substances again, and filtering out the gel to obtain a gel matrix;
s2, placing the gel matrix into a mold, flatly paving, controlling the thickness to be about 5mm, then transferring the mold and the gel matrix into a reduced pressure distillation kettle, vacuumizing to-0.1 MPa, controlling the temperature to be 80 ℃, carrying out reduced pressure rotary evaporation for 50min, removing partial water and ethanol to enable the gel matrix to be in a solidified state, then taking out and placing the gel matrix into a roller mill, controlling the roller temperature to be 60 ℃ and the roller interval to be 2mm, rolling the gel matrix in the solidified state into a sheet shape, and then punching to obtain a gel sheet;
and S3, cutting the gel sheet into a designed size, and then soaking in a PBS (phosphate buffer solution) for 10min to obtain the medical antibacterial hydrogel.
The medical antibacterial hydrogel prepared in the embodiment 1 to the embodiment 3 is prepared into an oblate cylindrical test sample with the diameter of 10mm, a material testing machine is adopted to test the mechanical property, after the test is finished, a stress-strain curve of each sample is drawn, the maximum strain and the maximum compressive stress are measured and calculated, and the specific test data are shown in the table 1:
TABLE 1
| Maximum strain/% | Maximum compressive stress/kPa | |
| Example 1 | 68.7 | 82.1 |
| Example 2 | 69.2 | 86.5 |
| Example 3 | 71.7 | 95.3 |
As can be seen from the data in Table 1, the medical antibacterial hydrogel prepared by the invention has good capability of resisting external force damage and deformation under the action of external force, and is suitable for gel dressing.
The medical antibacterial hydrogel prepared in the embodiments 1 to 3 is prepared into an oblate cylindrical sample with the diameter of 25mm, a rotational rheometer is used for rheological property test, the angular frequency scanning range is set to be 1rad/s-10rad/s, the change values of the storage modulus and the loss modulus along with the angular frequency in the test process are recorded through software, and specific test data are shown in table 2:
TABLE 2
As can be seen from the data in Table 2, the medical antibacterial hydrogel prepared by the invention has a storage modulus of more than 1.59kPa, a storage modulus much higher than a loss modulus, and shows good viscoelasticity.
The medical antibacterial hydrogel prepared in example 1 to example 3 was subjected to bacteriostatic test by the bacteriostatic ring method, using staphylococcus aureus and escherichia coli as test strains, and the strains were cultured and diluted to 1 x 10p 6 And (2) smearing the P/mL bacterial liquid on an agar plate, culturing for 12 hours in an incubator at 37 ℃, then taking the medical antibacterial hydrogel to prepare samples with the diameter of 5mm, respectively placing the samples on the agar plate, placing the samples in the incubator again for culturing for 12 hours, taking out the samples, and measuring the diameter of the antibacterial ring, wherein specific test data are shown in Table 3:
TABLE 3
As can be seen from the data in Table 3, the medical antibacterial hydrogel prepared by the invention has good bacteriostatic and bactericidal effects on staphylococcus aureus and escherichia coli.
Based on the test data in table 3, the medical antibacterial hydrogel prepared in example 2 was used as a sample, the method for the bacteriostasis test and staphylococcus aureus were used to perform a long-term bacteriostasis test, the bacteriostasis diameter was measured in 12 hours as one period, and the specific test data are shown in table 4:
TABLE 4
| 12h | 24h | 36h | 48h | 60h | 72h | |
| Diameter/mm of bacteriostatic ring | 14.1 | 17.5 | 17.8 | 17.2 | 16.7 | 15.9 |
As can be seen from the data in Table 4, the medical antibacterial hydrogel prepared in the embodiment 2 of the invention has stable and effective antibacterial effect within 72 h.
Based on the test data, the medical antibacterial hydrogel prepared in example 2 is used as a sample to perform a wash-resistant performance test, the sample is taken and repeatedly soaked in medical alcohol for 5 hours, then washed with PBS buffer solution, and then prepared into a sample, and a bacteriostasis test is performed according to the method of the bacteriostasis test, wherein the specific test data are shown in table 5:
TABLE 5
| Number of immersion times | 1 time of | 2 times (one time) | 3 times of | 4 times (twice) |
| Diameter/mm of bacteriostatic ring | 13.6 | 12.9 | 11.2 | 9.7 |
As can be seen from the data in Table 5, the medical antibacterial hydrogel prepared in the embodiment 2 of the invention still has good antibacterial ability after being soaked and washed repeatedly for 4 times, and can be repeatedly used in drainage dressings, so that the pain of patients in the dressing change process is reduced, and the working strength of medical staff is reduced.
In the description of the specification, reference to the description of "one embodiment," "an example," "a specific example" or the like means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is illustrative and explanatory only, and it will be appreciated by those skilled in the art that various modifications, additions and substitutions can be made to the embodiments described without departing from the scope of the invention as defined in the appended claims.
Claims (7)
1. The medical antibacterial hydrogel is characterized by comprising 40-55 parts of aminated cellulose gel particles, 1-5 parts of carboxymethyl chitosan, 3-6 parts of antibacterial agent and 1-8 parts of SAP micro powder;
the aminated cellulose gel particles are prepared by the following steps:
step A1: dissolving hydroxypropyl methylcellulose in ethanol solution, and dropwise adding ammonia water to adjust pH value of the solution to 8.2-8.7 to obtain mixed solution a;
step A2: diluting 3- (2-aminoethylamino) propyl methyldimethoxysilane with ethanol solution to obtain mixed solution b;
step A3: heating the mixed solution a to 38-45 ℃ in a stirring water bath, keeping stirring, dropwise adding the mixed solution b, controlling the reaction time to be 20-40min, centrifuging the reaction solution, and taking the lower-layer gel to obtain a prefabricated gel;
step A4: and (3) freeze-drying the preformed gel for 24h, taking out and crushing to prepare the aminated cellulose gel particles.
2. The medical antibacterial hydrogel according to claim 1, wherein the mass ratio of the hydroxypropyl methylcellulose to the 3- (2-aminoethylamino) propyl methyldimethoxysilane is 1.
3. The medical antibacterial hydrogel according to claim 1, wherein the particle size of the aminated cellulose gel particles is 0.2-1mm.
4. The medical antibacterial hydrogel according to claim 1, wherein the antibacterial agent is prepared by the following steps:
step B1: dissolving sodium aescinate in ethanol solution, adjusting pH of the solution to 5 with acetic acid, adding sodium alginate to adjust viscosity of the solution to 500-800cP at room temperature, and introducing ozone into the mixed solution under ultraviolet irradiation to obtain an oxidation solution;
and step B2: adjusting pH of the oxidation solution to 7 with ammonia water, rotary steaming under reduced pressure, and freeze drying to obtain antibacterial agent.
5. The medical antibacterial hydrogel according to claim 4, wherein the ultraviolet wavelength of the ultraviolet radiation is 100-300nm.
6. The medical antibacterial hydrogel according to claim 5, wherein the ozone is introduced at a rate of 0.18 to 0.25vvm for 60 to 80min.
7. The preparation method of the medical antibacterial hydrogel according to claim 1, characterized by comprising the following steps:
step S1: uniformly mixing the aminated cellulose gel particles, carboxymethyl chitosan, an antibacterial agent and SAP micro powder, adding an ethanol solution, continuously mixing, then carrying out water bath heat preservation at 58-65 ℃ for 20-30min, and filtering the reaction liquid to prepare a gel matrix;
step S2: placing the gel matrix into a mold, flatly paving the matrix in the mold, then forming the matrix and the mold in a reduced pressure distillation kettle, then rolling out the matrix for forming, and then punching to obtain a gel sheet;
and step S3: and cutting the gel sheet, and then soaking the gel sheet in a PBS (phosphate buffer solution) to obtain the medical antibacterial hydrogel.
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