CN114732941A - Preparation method of cleaning and antibacterial gel - Google Patents
Preparation method of cleaning and antibacterial gel Download PDFInfo
- Publication number
- CN114732941A CN114732941A CN202210284568.5A CN202210284568A CN114732941A CN 114732941 A CN114732941 A CN 114732941A CN 202210284568 A CN202210284568 A CN 202210284568A CN 114732941 A CN114732941 A CN 114732941A
- Authority
- CN
- China
- Prior art keywords
- gel
- parts
- carbomer
- bacteriocin
- hydrogel
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 238000004140 cleaning Methods 0.000 title claims description 11
- 108010062877 Bacteriocins Proteins 0.000 claims abstract description 27
- 229920001651 Cyanoacrylate Polymers 0.000 claims abstract description 12
- MWCLLHOVUTZFKS-UHFFFAOYSA-N Methyl cyanoacrylate Chemical compound COC(=O)C(=C)C#N MWCLLHOVUTZFKS-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229920001661 Chitosan Polymers 0.000 claims abstract description 10
- 108090000790 Enzymes Proteins 0.000 claims abstract description 9
- 102000004190 Enzymes Human genes 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 239000000243 solution Substances 0.000 claims description 17
- NIXOWILDQLNWCW-UHFFFAOYSA-N Acrylic acid Chemical compound OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 16
- 229920002125 Sokalan® Polymers 0.000 claims description 16
- 229960001631 carbomer Drugs 0.000 claims description 16
- 239000000203 mixture Substances 0.000 claims description 14
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 12
- 230000003385 bacteriostatic effect Effects 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 8
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 7
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- 108010073254 Colicins Proteins 0.000 claims description 6
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- 108010053775 Nisin Proteins 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 238000010257 thawing Methods 0.000 claims description 5
- WHNWPMSKXPGLAX-UHFFFAOYSA-N N-Vinyl-2-pyrrolidone Chemical compound C=CN1CCCC1=O WHNWPMSKXPGLAX-UHFFFAOYSA-N 0.000 claims description 4
- NVNLLIYOARQCIX-MSHCCFNRSA-N Nisin Chemical compound N1C(=O)[C@@H](CC(C)C)NC(=O)C(=C)NC(=O)[C@@H]([C@H](C)CC)NC(=O)[C@@H](NC(=O)C(=C/C)/NC(=O)[C@H](N)[C@H](C)CC)CSC[C@@H]1C(=O)N[C@@H]1C(=O)N2CCC[C@@H]2C(=O)NCC(=O)N[C@@H](C(=O)N[C@H](CCCCN)C(=O)N[C@@H]2C(NCC(=O)N[C@H](C)C(=O)N[C@H](CC(C)C)C(=O)N[C@H](CCSC)C(=O)NCC(=O)N[C@H](CS[C@@H]2C)C(=O)N[C@H](CC(N)=O)C(=O)N[C@H](CCSC)C(=O)N[C@H](CCCCN)C(=O)N[C@@H]2C(N[C@H](C)C(=O)N[C@@H]3C(=O)N[C@@H](C(N[C@H](CC=4NC=NC=4)C(=O)N[C@H](CS[C@@H]3C)C(=O)N[C@H](CO)C(=O)N[C@H]([C@H](C)CC)C(=O)N[C@H](CC=3NC=NC=3)C(=O)N[C@H](C(C)C)C(=O)NC(=C)C(=O)N[C@H](CCCCN)C(O)=O)=O)CS[C@@H]2C)=O)=O)CS[C@@H]1C NVNLLIYOARQCIX-MSHCCFNRSA-N 0.000 claims description 4
- 239000002202 Polyethylene glycol Substances 0.000 claims description 4
- 239000007864 aqueous solution Substances 0.000 claims description 4
- 239000004359 castor oil Substances 0.000 claims description 4
- 235000019438 castor oil Nutrition 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
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- 239000012153 distilled water Substances 0.000 claims description 4
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- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 claims description 4
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- 229940031663 carbomer-974p Drugs 0.000 claims description 3
- JJJFUHOGVZWXNQ-UHFFFAOYSA-N enbucrilate Chemical compound CCCCOC(=O)C(=C)C#N JJJFUHOGVZWXNQ-UHFFFAOYSA-N 0.000 claims description 3
- WVXQYJXDTJWWEA-UHFFFAOYSA-N heptyl 2-cyanoprop-2-enoate Chemical compound CCCCCCCOC(=O)C(=C)C#N WVXQYJXDTJWWEA-UHFFFAOYSA-N 0.000 claims description 3
- 239000000178 monomer Substances 0.000 claims description 3
- 238000012425 Freezing-thawing process Methods 0.000 claims description 2
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- 239000008399 tap water Substances 0.000 claims description 2
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- 238000001816 cooling Methods 0.000 claims 1
- 238000003760 magnetic stirring Methods 0.000 claims 1
- 239000000017 hydrogel Substances 0.000 abstract description 36
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 6
- 239000003242 anti bacterial agent Substances 0.000 description 6
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- LXCFILQKKLGQFO-UHFFFAOYSA-N methylparaben Chemical compound COC(=O)C1=CC=C(O)C=C1 LXCFILQKKLGQFO-UHFFFAOYSA-N 0.000 description 2
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- MSWZFWKMSRAUBD-IVMDWMLBSA-N 2-amino-2-deoxy-D-glucopyranose Chemical compound N[C@H]1C(O)O[C@H](CO)[C@@H](O)[C@@H]1O MSWZFWKMSRAUBD-IVMDWMLBSA-N 0.000 description 1
- 206010067484 Adverse reaction Diseases 0.000 description 1
- 108700042778 Antimicrobial Peptides Proteins 0.000 description 1
- 102000044503 Antimicrobial Peptides Human genes 0.000 description 1
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 description 1
- 208000007190 Chlamydia Infections Diseases 0.000 description 1
- 201000004624 Dermatitis Diseases 0.000 description 1
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- 241000283973 Oryctolagus cuniculus Species 0.000 description 1
- 229930182555 Penicillin Natural products 0.000 description 1
- 239000001888 Peptone Substances 0.000 description 1
- 108010080698 Peptones Proteins 0.000 description 1
- 208000007536 Thrombosis Diseases 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 230000006838 adverse reaction Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 229940088710 antibiotic agent Drugs 0.000 description 1
- 230000008952 bacterial invasion Effects 0.000 description 1
- 235000015278 beef Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229960000686 benzalkonium chloride Drugs 0.000 description 1
- DMSMPAJRVJJAGA-UHFFFAOYSA-N benzo[d]isothiazol-3-one Chemical compound C1=CC=C2C(=O)NSC2=C1 DMSMPAJRVJJAGA-UHFFFAOYSA-N 0.000 description 1
- CADWTSSKOVRVJC-UHFFFAOYSA-N benzyl(dimethyl)azanium;chloride Chemical compound [Cl-].C[NH+](C)CC1=CC=CC=C1 CADWTSSKOVRVJC-UHFFFAOYSA-N 0.000 description 1
- MSWZFWKMSRAUBD-UHFFFAOYSA-N beta-D-galactosamine Natural products NC1C(O)OC(CO)C(O)C1O MSWZFWKMSRAUBD-UHFFFAOYSA-N 0.000 description 1
- 239000003519 biomedical and dental material Substances 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
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- 210000000170 cell membrane Anatomy 0.000 description 1
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- 229960002798 cetrimide Drugs 0.000 description 1
- 108010089807 chitosanase Proteins 0.000 description 1
- 238000003501 co-culture Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
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- 238000007796 conventional method Methods 0.000 description 1
- 125000004093 cyano group Chemical group *C#N 0.000 description 1
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- 230000004060 metabolic process Effects 0.000 description 1
- 239000002207 metabolite Substances 0.000 description 1
- 235000010270 methyl p-hydroxybenzoate Nutrition 0.000 description 1
- 239000004292 methyl p-hydroxybenzoate Substances 0.000 description 1
- 229960002216 methylparaben Drugs 0.000 description 1
- 210000004400 mucous membrane Anatomy 0.000 description 1
- 125000004108 n-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 230000001717 pathogenic effect Effects 0.000 description 1
- 150000002960 penicillins Chemical class 0.000 description 1
- 235000019319 peptone Nutrition 0.000 description 1
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- 230000037048 polymerization activity Effects 0.000 description 1
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- 239000012798 spherical particle Substances 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
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- 230000002195 synergetic effect Effects 0.000 description 1
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- 231100000419 toxicity Toxicity 0.000 description 1
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Classifications
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L26/00—Chemical aspects of, or use of materials for, wound dressings or bandages in liquid, gel or powder form
- A61L26/0009—Chemical aspects of, or use of materials for, wound dressings or bandages in liquid, gel or powder form containing macromolecular materials
- A61L26/0014—Chemical aspects of, or use of materials for, wound dressings or bandages in liquid, gel or powder form containing macromolecular materials obtained by reactions only involving carbon-to-carbon unsaturated bonds
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L26/00—Chemical aspects of, or use of materials for, wound dressings or bandages in liquid, gel or powder form
- A61L26/0061—Use of materials characterised by their function or physical properties
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L26/00—Chemical aspects of, or use of materials for, wound dressings or bandages in liquid, gel or powder form
- A61L26/0061—Use of materials characterised by their function or physical properties
- A61L26/0066—Medicaments; Biocides
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L26/00—Chemical aspects of, or use of materials for, wound dressings or bandages in liquid, gel or powder form
- A61L26/0061—Use of materials characterised by their function or physical properties
- A61L26/008—Hydrogels or hydrocolloids
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
- A61L2300/20—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices containing or releasing organic materials
- A61L2300/252—Polypeptides, proteins, e.g. glycoproteins, lipoproteins, cytokines
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
- A61L2300/20—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices containing or releasing organic materials
- A61L2300/252—Polypeptides, proteins, e.g. glycoproteins, lipoproteins, cytokines
- A61L2300/254—Enzymes, proenzymes
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
- A61L2300/40—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices characterised by a specific therapeutic activity or mode of action
- A61L2300/404—Biocides, antimicrobial agents, antiseptic agents
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
- A61L2300/40—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices characterised by a specific therapeutic activity or mode of action
- A61L2300/412—Tissue-regenerating or healing or proliferative agents
-
- 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
- Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- Materials Engineering (AREA)
- Epidemiology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Dispersion Chemistry (AREA)
- Materials For Medical Uses (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
- Medicinal Preparation (AREA)
Abstract
The invention belongs to the technical field of hydrogel, in particular to a preparation method of clean antibacterial gel, which utilizes the combination of bacteriocin and hydrogel through cyanoacrylate load and is assisted by chitosan enzyme and the like to form the clean antibacterial gel, has good compliance of moisture retention, can be cut, can absorb seepage and permeate gas, has the advantages of promoting the moist healing of wounds, having no adhesion, enabling patients to feel comfortable, obviously relieving the pain feeling and the like, has activity or can promote the release of active substances, thereby accelerating the healing speed of wound surfaces, and the clean antibacterial hydrogel disclosed by the invention shows stable coverage, small displacement, lasting antibacterial property and rapid wound healing capability.
Description
Technical Field
The invention belongs to the technical field of hydrogel materials, and particularly relates to a preparation method of a cleaning and antibacterial gel.
Background
The hydrogel is also called water-containing hydrogel, and is a hydrophilic net-shaped polymer swelling body which can swell in water, absorb and retain a large amount of water and is insoluble in water. Because of high water content, the hydrogel can be randomly shaped, is suitable for wound surfaces of any position, provides necessary conditions for wound healing, and has biocompatibility superior to fiber and film dressings. In addition, the hydrogel is very soft due to a large amount of moisture and is similar to organism tissues, so that adverse reactions can be reduced when the hydrogel is used as a human implant. Therefore, the hydrogel is widely used as an excellent biomedical material, such as a drug carrier, a tissue scaffold, a wound dressing and the like, and can prevent further wound injury and bacterial invasion. The antibacterial hydrogel can meet the requirements of both hydrogel and antibacterial function, and is mainly divided into antibacterial hydrogel containing inorganic nanoparticles, antibacterial hydrogel containing organic antibacterial agents and the like according to the difference between a matrix and the antibacterial agents. For example, silver particles, the conventional method mostly compounds nano silver particles with the implant directly, thereby endowing the implant with an antibacterial function. Taking hydrogel material as an example, after the nano silver ions are directly compounded with the hydrogel material, the nano silver particles have interaction with tissues or cells, but when the concentration of the nano silver particles exceeds a certain range, certain toxicity is generated on the cells and the tissues, and the nano silver particles penetrate or deposit on cell walls, so that the transportation of electrolytes and metabolites is influenced, the interaction with membrane proteins is caused, signal channels are activated, and the proliferation and the contraction of the cells are inhibited. Chinese patent CN2018115319408 discloses an antibacterial hydrogel capable of controllably releasing nano silver ions and a preparation method thereof, and aims to realize long-term slow release of nano silver particles in an implant; for example, chinese patent CN2016104668764 discloses a marine phycocolloid hydrogel and its preparation method, which mainly uses artificially synthesized antibacterial agents, such as antibacterial agents benzisothiazolinone, methylparaben, benzalkonium chloride, cetrimide, etc., however, the hydrogel using the synthesized antibacterial agents has the disadvantages and defects of poor biocompatibility and antibacterial property, and easy skin allergy. From the current research results, in the development of the antibacterial hydrogel, people have great efforts to utilize macromolecules such as polysaccharides and polyethers to prepare the antibacterial hydrogel with complicated structure, complicated method, complicated components and mixing with various antibacterial substances, but neglect the most basic biocompatibility and irritation, for example, although inorganic antibacterial agents such as Ag nanoparticles have good antibacterial property, the biocompatibility limits the wide application of the antibacterial hydrogel on the surface of human skin. In addition, long-term use and abuse of traditional antibiotic antibacterials, such as penicillins and the like, can lead to the development of resistant bacteria. Therefore, those skilled in the art are in need of developing a preparation method of a cleansing antibacterial gel, specifically, a bacteriocin hydrogel is formed by chemically or physically combining bacteriocin and hydrogel.
Disclosure of Invention
In view of the above problems, the present invention aims to provide a preparation method of a clean bacteriostatic gel, and specifically, a bacteriocin hydrogel is formed by chemically or physically combining bacteriocin and hydrogel.
The invention is realized by the following technical scheme:
a preparation method of a cleaning bacteriostatic gel comprises the following operation steps:
(1) adding 45-50 parts by weight of deionized water and 16-18 parts by weight of carbomer into a reaction bottle, magnetically stirring for dissolving, then adjusting the pH of the system to 3.5-4 by using a hydrochloric acid solution with the mass fraction of 5%, slowly dropwise adding 12-15 parts of cyanoacrylate monomer at the stirring speed of 800r/min, and adjusting the pH of the system to 6.8-7.0 by using 0.1mol/L potassium carbonate aqueous solution after 2-3 h to obtain a gel solution;
since the cyano group in the alpha position is a strong electron-withdrawing group, the beta carbon atom is rendered more electropositive, so that it has a great tendency to polymerize, and upon contact with an anion, it is converted from a monomer to a polymer. And then the cyanoacrylate microspheres are introduced into the hydrogel, and the organic rigid particles of the cyanoacrylate microspheres toughen to form a cold-drawing effect, so that the physical and mechanical properties of the hydrogel are further improved. (2) Uniformly mixing the gel solution and the bacteriocin according to the mass ratio of 7-9: 1, and then placing the mixture in a constant-temperature oscillator for oscillation for 2.4 hours; filtering out the hydrogel, cleaning, washing, and drying in an oven at 60 ℃ for 0.5-1 h to obtain the bacteriocin-loaded carbomer gel; the constant temperature oscillator has the advantages of high temperature control precision, uniform temperature distribution, high heating speed and low noise, and can ensure that the bacteriocin is uniformly and rapidly loaded on the carbomer gel.
(3) According to the weight parts, sequentially adding 8-13 parts of glycerol polyethylene glycol hydrogenated castor oil, 36-43 parts of polyvinyl alcohol, 56-61 parts of bacteriocin-loaded carbomer gel, 8-12 parts of polyvidone and 6-8 parts of chitosan enzyme into 690-740 parts of distilled water, stirring, performing ultrasonic defoaming treatment for 40-50 min, and performing freezing-thawing cycle treatment for 5-7 times to obtain the clean antibacterial gel.
Further, in the step (1), the polyvinyl alcohol in the step (3) is one of PVA05-88 or PVA 17-88.
Further, in the step (1), the carbomer is one of carbomer 934P, carbomer 974P and carbomer 1342.
Further, in the step (3), the povidone is one or a mixture of PVPK30 and PVPK 90.
Further, in the step (2), the bacteriocin is one of colicin and nisin or a mixture of the colicin and the nisin.
Bacteriocins are a class of antibacterial substances produced by certain bacteria, and have certain antibacterial action although the action range is narrow. The name of bacteriocin is named according to the species produced, e.g.the bacteriocin produced by E.coli is called colicin.
Further, in the step (3), the cyanoacrylate is one of α -n-butyl cyanoacrylate and α -heptyl cyanoacrylate, or a mixture of both.
Cyanoacrylate, commonly used as an adhesive, was first developed and applied by kodak companies, such as n-butyl α -cyanoacrylate to prepare 504 medical adhesive, which can strongly adhere to body tissues and has a high adhesion speed. Has no toxicity, little reaction to tissues, no thrombosis and simple sterilization.
Further, in the step (3), the operation of the freezing-thawing cycle treatment is to place the mixture into a refrigerator with the temperature of-26 ℃ for cold 24 hours, take the mixture out, thaw the mixture with tap water at room temperature until the temperature reaches 0-2 ℃, and complete the freezing-thawing process.
The invention has the beneficial effects that:
the invention introduces cyanoacrylate microspheres into hydrogel, rigid particles of the cyanoacrylate microspheres toughen to form a cold drawing effect, spherical particles are dispersed in a matrix before drawing, brittle particles yield and deform in the same size with the matrix during drawing to absorb considerable energy, so that the toughness of a blend is improved, the mechanical property of the hydrogel can be enhanced, high tensile strength and better compression property are realized, meanwhile, the loaded bacteriocin provides lasting antibacterial property for the hydrogel and forms a synergistic antibacterial effect with chitosan enzyme, the main antibacterial active ingredients of the clean antibacterial gel prepared by the preparation method disclosed by the invention are bacteriocin and chitosan enzyme, and the gel has multiple medical health-care effects of resisting bacteria, diminishing inflammation, increasing immunity, promoting wound healing, nourishing and repairing mucous membranes and the like, and also has good biocompatibility and biodegradability, is safe and nontoxic, wherein chitosan is a polymer formed by connecting glucosamine through beta-1, 4-bonds, is rich in active groups, can be adsorbed with pathogenic cell membranes and can be coagulated, or penetrate into pathogenic bacteria to disturb metabolism of pathogenic bacteria, thereby exerting broad-spectrum antibacterial effect, not easily generating drug resistance, and having lasting effect, has obvious inhibiting and killing effect on mycoplasma or chlamydia infection, high cyanoacrylate polymerization activity, alkali and very weak water capable of initiating polymerization and being wetted by blood, can be subjected to nontoxic and biochemical depolymerization, has good biodegradability and biocompatibility, can be used as a carrier material to prepare the loaded bacteriocin, and improves the action efficiency of the bacteriocin by means of degradation performance and drug release performance, the cleaning gel with uniform bacteriostatic action is prepared by simple preparation steps through processes of freezing, thawing, defoaming and the like.
Compared with the prior art, the invention has the following advantages:
the invention combines bacteriocin and hydrogel through cyanoacrylate load, and is assisted by chitosan enzyme and the like to form clean antibacterial gel, which has the advantages of good compliance of moisture retention, tailorability, capability of absorbing seepage, permeability of gas, promotion of moist healing of wounds, no adhesion, comfortable feeling of patients, obvious pain relief and the like, and the hydrogel has activity or can promote the release of active substances, so that the healing speed of wound surfaces is accelerated.
Detailed Description
The invention is illustrated by the following specific examples, which are not intended to be limiting.
Example 1
Firstly, adding 50 parts by weight of deionized water and 18 parts by weight of carbomer 974P into a reaction bottle, magnetically stirring for dissolution, then adjusting the pH of the system to 4 by using a hydrochloric acid solution with the mass fraction of 5%, slowly dropwise adding 15 parts of alpha-heptyl cyanoacrylate at the stirring speed of 800r/min, and after 3 hours, adjusting the pH of the system to 7.0 by using 0.1mol/L potassium carbonate aqueous solution to obtain a gel solution;
step two, uniformly mixing the gel solution and bacteriocin colicin according to the mass ratio of 9:1, and then placing the mixture in an SHZ-88 water bath constant temperature oscillator at 30 ℃ for oscillation for 2.4 hours with the oscillation frequency of 100 times; filtering out the hydrogel, cleaning, washing, and drying in an oven at 60 ℃ for 1h to obtain the bacteriocin-loaded carbomer gel;
thirdly, adding 13 parts of glycerol polyethylene glycol hydrogenated castor oil, 43 parts of polyvinyl alcohol PVA05-88, 61 parts of bacteriocin-loaded carbomer gel, 12 parts of povidone PVPK90 and 8 parts of chitosan enzyme into 740 parts of distilled water in sequence by weight, stirring, performing ultrasonic defoaming treatment for 50min, and performing freezing-unfreezing circulation treatment for 7 times to obtain the clean antibacterial gel, wherein the longitudinal tensile strength of the gel is 1.4MPa, the transverse tensile strength of the gel is 1.3MPa, the elongation at break of the gel is 654.3%, the peel strength of the gel at a width of 1cm is 1.2N/cm, and the skin sensitization of the gel is as follows: post-challenge rating of 0, skin irritation: the response stimulation index is 0, and the water vapor transmission rate is 112.5g/m224h, bacteriostatic activity: staphylococcus aureus (ATCC6538) 93.0%, Escherichia coli (ATCC25922) 98.4%, Candida albicans (ATCC10231) 93.0%.
Coli (ATCC25922) MIC colicin 2.69 × 10-4Coli (ATCC25922) MIC chitosanase 2.8X 10-3、FIC＝0.36
Example 2
Firstly, adding 45 parts of deionized water and 16 parts of carbomer 934P into a reaction bottle in parts by weight, magnetically stirring for dissolution, then adjusting the pH of the system to 3.5 by using a hydrochloric acid solution with the mass fraction of 5%, slowly dropwise adding 12 parts of alpha-n-butyl cyanoacrylate at the stirring speed of 800r/min, and adjusting the pH of the system to 6.8 by using 0.1mol/L potassium carbonate aqueous solution after 2 hours to obtain a gel solution;
step two, uniformly mixing the gel solution and bacteriocin nisin according to the mass ratio of 7:1, and then placing the mixture into an SHZ-88 water bath constant-temperature oscillator for oscillation for 2.4 hours with the oscillation frequency of 100 times; filtering out the hydrogel, cleaning, washing, and drying in an oven at 60 ℃ for 0.5h to obtain the carbomer gel loaded with the bacteriocin;
thirdly, sequentially adding 8 parts of glycerol polyethylene glycol hydrogenated castor oil, 36 parts of polyvinyl alcohol PVA05-88, 56 parts of bacteriocin-loaded carbomer gel, 8 parts of povidone PVPK30 and 6 parts of chitosan enzyme into 690 parts of distilled water by weight, stirring, performing ultrasonic defoaming treatment for 40min, and performing freezing-unfreezing cycle treatment for 5 times to obtain the clean antibacterial gel, wherein the longitudinal tensile strength of the clean antibacterial gel is 1.1MPa, the transverse tensile strength of the clean antibacterial gel is 1.0MPa, the elongation at break is 612.7%, the peel strength of the clean antibacterial gel with the width of 1cm is 1.2N/cm, and the skin sensitization is as follows: post-challenge rating of 0, skin irritation: the response stimulation index is 0, and the water vapor transmission rate is 112.5g/m224h, bacteriostatic activity: 95.2% of staphylococcus aureus (ATCC6538), 93.8% of escherichia coli (ATCC25922) and 94.1% of candida albicans (ATCC 10231).
Note: the detection was performed with reference to the following criteria: the bacteriostasis rate test is carried out according to the method in the GB15979-2002 hygienic standard of disposable sanitary products; irritation and skin sensitization test: removing back hair of 10cm × 15cm from two sides of spinal column of animal 24 hr before test, and dripping 0.5ml of test sample leaching solution and control solution onto 2.5cm × 2.5cm absorbent gauze pieces respectively. The gauze pieces soaked with the sample leaching solution and the solvent contrast solution are respectively directly contacted with the skins on both sides of the spine of the rabbit, and then are fixedly attached for 4 hours by using bandages. And removing the patch after the contact period is finished. The tensile strength and elongation at break were determined according to GB/T1040.3-2006. The test sample is a strip with the length of 150mm and the width of 15mm, the distance between the clamps is 100mm, and the test speed is 250 mm/min.
Staphylococcus aureus (ATCC6538) MIC nisin 1.63X 10-5Staphylococcus aureus (ATCC6538) MIC Chitosan enzyme 3.14X 10-3、FIC＝0.27；
And (3) culturing bacteria: transforming the activated bacteriaInoculating to liquid culture medium, culturing at 37 deg.C for 12 hr, centrifuging at 3000r min for 5min, discarding supernatant, and diluting the precipitate with sterilized liquid culture medium to 10%6CFU/mL is used as a test bacterial liquid (beef extract peptone culture medium), the cultured fungal cells are diluted to 2X 10' CFUmL by using a liquid culture medium, 100/AL is taken and put into each experimental hole of a 96-well plate, then 100 mu L of antibacterial peptide with certain concentration is respectively added into each experimental hole, and two groups are set as a control group: one group was 100 μ L of culture medium; the other group is 100 mu L of bacterial liquid, and the bacterial liquid is simultaneously put into an incubator at 28 ℃ for 24 hours. On the basis of small inhibitory concentration (MIC), 4 XMIC antibacterial peptide and 4 XMIC antibiotic are respectively added into each 75/L of experiment holes of a 96-hole micro-culture plate, dilution is carried out in a multiple ratio mode continuously, each original concentration hole is diluted into 20 experiment holes, and then 100/L of bacteria liquid to be detected (10) is added into each experiment hole6CFU/mL), together with two controls: one group is 250/culture solution; the other group is 250L of bacterial liquid, and then the bacterial liquid is put into a constant temperature incubator at 37 ℃ for 12 hours. The Minimum Inhibitory Concentration (MIC) of the antimicrobial peptide and the antibiotic at the time of co-culture was calculated.
Claims (6)
1. The preparation method of the cleaning and bacteriostasis gel is characterized by comprising the following operation steps:
(1) adding 45-50 parts by weight of deionized water and 16-18 parts by weight of carbomer into a reaction bottle, dissolving by magnetic stirring, adjusting the pH of the system to 3.5-4 by using a hydrochloric acid solution with the mass fraction of 5%, slowly dripping 12-15 parts of cyanoacrylate monomer at the stirring speed of 600-800 r/min, and adjusting the pH of the system to 6.8-7.0 by using 0.1mol/L potassium carbonate aqueous solution after 2-3 h to obtain a gel solution;
(2) uniformly mixing the gel solution and the bacteriocin according to the mass ratio of 7-9: 1, and then placing the mixture in a constant-temperature oscillator for oscillation for 2-2.4 hours; filtering out the gel, cleaning, washing, and drying in an oven at 50-60 ℃ for 0.5-1 h to obtain the carbomer gel loaded with the bacteriocin;
(3) according to the weight parts, 8-13 parts of glycerol polyethylene glycol hydrogenated castor oil, 36-43 parts of polyvinyl alcohol, 56-61 parts of bacteriocin-loaded carbomer gel, 8-12 parts of polyvidone and 6-8 parts of chitosan enzyme are sequentially added into 690-740 parts of distilled water, stirred, subjected to ultrasonic defoaming treatment for 40-50 min, subjected to freezing-unfreezing cycle treatment for 5-7 times, and then the clean antibacterial gel is obtained.
2. The method for preparing a cleansing bacteriostatic gel according to claim 1, wherein in the step (3), the polyvinyl alcohol is one of PVA05-88 or PVA17-88, and the povidone is one of PVPK30 or PVPK90 or a mixture of both.
3. The method for preparing a cleansing bacteriostatic gel according to claim 1, characterized in that in the step (1), the carbomer is one of carbomer 934P, carbomer 974P and carbomer 1342.
4. The method for preparing a cleansing bacteriostatic gel according to claim 1, wherein in the step (1), the cyanoacrylate is one of α -n-butyl cyanoacrylate and α -heptyl cyanoacrylate or a mixture of the two.
5. The method for preparing a cleansing bacteriostatic gel according to claim 1, wherein in the step (2), the bacteriocin is one or a mixture of colicin and nisin.
6. The preparation method of a cleaning bacteriostatic gel according to claim 1, characterized in that in the step (3), the freezing-thawing cycle treatment is carried out by putting the gel into a refrigerator of-20 ℃ for cooling for 24h, taking out the gel, thawing the gel with tap water at room temperature until the temperature reaches 0-2 ℃, and then completing a freezing-thawing process.
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| CN101524180A (en) * | 2009-04-22 | 2009-09-09 | 东北农业大学 | Composite microbiological antibiotic and preparation method thereof |
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