CN114984305A - Novel antibacterial film-forming liquid medical dressing and preparation method thereof - Google Patents
Novel antibacterial film-forming liquid medical dressing and preparation method thereof Download PDFInfo
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- 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
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- 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
- A61L26/0004—Chemical aspects of, or use of materials for, wound dressings or bandages in liquid, gel or powder form containing inorganic materials
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- 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
- A61L26/0023—Polysaccharides
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- 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
- A61L26/0057—Ingredients of undetermined constitution or reaction products thereof
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- 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
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- 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
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- 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
- A61L2400/00—Materials characterised by their function or physical properties
- A61L2400/12—Nanosized materials, e.g. nanofibres, nanoparticles, nanowires, nanotubes; Nanostructured surfaces
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- 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
Abstract
The invention discloses a novel bacteriostatic film-forming liquid medical dressing, which comprises the following raw materials: the film forming material comprises D-limonene, dopamine-graphene oxide, a functionalized halloysite nanotube, benzyl alcohol, castor oil, camphor, isopropyl palmitate, clove oil and an organic solvent. In addition, a preparation method of the liquid medical dressing is also disclosed. The film formed by the liquid medical dressing has optimized mechanical strength, and meanwhile, the air permeability and the antibacterial performance are not basically damaged.
Description
Technical Field
The invention belongs to the technical field of medical dressing; relates to a novel bacteriostatic film-forming liquid medical dressing and a preparation method thereof.
Background
Skin is an important component of the human body, and when skin is damaged, wound healing is a complex biological process involving hemostasis, inflammation, cell proliferation, scarring and epidermal and other tissue regeneration.
An important means of treating skin wounds is treatment with medical dressings. At present, the medical dressings are mainly divided into traditional medical dressings, synthetic medical dressings and biological medical dressings. The medical dressings can play a role in temporary protection when used for treating skin wounds in the fields of dermatology, respiratory department and the like, avoid or control wound infection and provide a healing environment suitable for the body surfaces of the wounds.
The traditional medical dressing mainly comprises gauze and artificial synthetic fiber, and the medical dressing has the characteristics of wound surface protection, certain absorption capacity on wound exudates, simple manufacture, low cost and the like. But also has the defects of poor hemostatic effect, easy drying, easy re-wound during replacement, easy bacterial invasion and infection after soaking and the like.
Synthetic medical dressings are further classified into film dressings (nylon, polyurethane, polylactic acid, and the like), foam sponges (polyvinyl alcohol foam, silicone rubber foam, polyurethane foam, and the like), hydrogel dressings (sodium carboxymethyl cellulose, for example), hydrocolloid dressings, and alginate dressings. The synthetic medical dressings have various advantages and disadvantages, and proper medical dressings are selected to treat wounds according to different degrees and different positions of the damaged skin.
The biological medical dressing mainly comprises chitosan and derivatives thereof, collagen, hyaluronic acid, silk protein and the like. The biological medical dressing has the advantages of good biocompatibility, no side effect, good air permeability, capability of providing environmental protection, avoiding invasion and infection of bacteria, effectively reducing the damage to the granulation tissue during replacement and the like.
Chinese patent application publication CN104056299A discloses a liquid wound-protecting film and a preparation method thereof. The liquid wound protection film comprises the following components in percentage by mass: 5 to 20 percent of nitrocotton, 50 to 80 percent of isoamyl acetate, 10 to 30 percent of butyl acetate, 5 to 10 percent of castor oil, 0.1 to 1 percent of clove oil and 0.5 to 2 percent of thyme oil. The liquid wound protecting film provided by the invention does not contain alcohol, and has no pricking feeling when in use; the natural analgesic and bacteriostatic components are added, so that the safety is higher. The product is easy and convenient to use, and the formed film has flexibility, good adherence, and no easy shedding, and has effects of relieving pain, inhibiting bacteria, preventing water, and promoting wound healing.
Chinese patent application publication CN105999360A discloses a biological bacteriostatic film-forming liquid medical dressing and a preparation method thereof, which comprises the following components in parts by weight: 110-20 parts of cellulose ether; 5-30 parts of polyacrylate; 150-200 parts of ethanol; 10-30 parts of butyl acetate; 10-20 parts of ethyl acetate; 0.5-1.5 parts of camphor; 5-10 parts of castor oil; 1-5 parts of polydimethylsiloxane; 0.1-0.3 part of antibacterial nano particles. After being applied, the ointment has the effects of easing pain, astringing, inhibiting bacteria, promoting wound healing and the like on the wound surface; the isolation performance is good, bacteria and foreign matters can be prevented from being soaked into the wound, bacteria and fungi on the surface of the wound surface can be killed, infection is reduced, and meanwhile, the waterproof performance is good; the coating film is suitable for the wound surfaces with different sizes, shapes and positions, the coating film has certain elasticity, and the coated position can move freely; no allergy and drug resistance and high safety; no obvious irritation; is convenient to carry and use.
Chinese patent application publication CN114306729A discloses a medical dressing of biological antibacterial film-forming liquid, which comprises a film-forming material, a bactericide and an organic solvent; the liquid medical dressing further comprises dopamine-graphene oxide. The film-forming material is selected from the group consisting of cellulose nitrate and octyl alpha-cyanoacrylate in combination. In addition, a preparation method of the biological antibacterial film-forming liquid medical dressing is also disclosed. Compared with the prior art, the antibacterial film-forming liquid medical dressing has better air permeability and antibacterial property.
In further research, the inventor finds that the mechanical strength of the bacteriostatic film-forming liquid medical dressing is poor. In order to further optimize the mechanical strength performance, a small amount of reinforcing material is usually required to be added into the film-forming material, but the mechanical strength performance is enhanced, and meanwhile, the air permeability of the medical dressing is generally reduced, and the bacteriostatic performance can also be influenced.
Disclosure of Invention
The invention aims to provide a novel bacteriostatic film-forming liquid medical dressing which has optimized mechanical strength and does not basically damage air permeability and bacteriostatic performance and a preparation method thereof.
In order to achieve the above object, in one aspect, the technical solution adopted by the present invention is as follows: a novel bacteriostatic film-forming liquid medical dressing comprises the following raw materials:
60-90 parts of a film forming material;
10-30 parts of D-limonene;
30-50 parts of dopamine-graphene oxide;
20-28 parts of a functionalized halloysite nanotube;
45-75 parts of benzyl alcohol;
10-30 parts of castor oil;
2-8 parts of camphor;
10-30 parts of isopropyl palmitate;
0.5-2 parts of clove oil;
600 portions and 900 portions of organic solvent.
The liquid medical dressing is characterized in that the functionalized halloysite nanotubes are obtained by functionally modifying treated halloysite nanotubes by gamma- (2, 3-epoxypropoxy) propyltrimethoxysilane.
The liquid medical dressing provided by the invention is characterized in that the weight ratio of the treated halloysite nanotubes to gamma- (2, 3-glycidoxy) propyl trimethoxy silane is 1: (1.5-2.5).
In a specific embodiment, the weight ratio of the treated halloysite nanotubes to gamma- (2, 3-glycidoxy) propyltrimethoxysilane is 1: 2.
the liquid medical dressing according to the present invention, wherein the functional modification conditions are: the reaction time is 4-12h at 80-100 ℃.
In a specific embodiment, the functionalization modification conditions are: the reaction time is 8h at 90 ℃.
The liquid medical dressing is characterized in that the treated halloysite nanotubes are obtained by reacting halloysite nanotubes in 1-3M HCl solution at 60-90 ℃ for 2-6 h.
In a specific embodiment, the treated halloysite nanotubes are obtained by reacting halloysite nanotubes in 2M HCl at 75 ℃ for 4 hours.
The liquid medical dressing provided by the invention is characterized in that the inner diameter of the halloysite nanotube is 10-30 nm; the outer diameter is 50-70 nm; the length is 1-3 mu m; specific surface area 64m 2 (ii)/g; the pore volume is 1.26-1.34 mL/g.
The liquid medical dressing according to the present invention, wherein the film-forming material is selected from a combination of nitrocellulose and octyl alpha-cyanoacrylate; and/or the weight ratio of the cellulose nitrate to the octyl alpha-cyanoacrylate is (1.5-2.5): 1.
in one specific embodiment, the weight ratio of cellulose nitrate to octyl alpha-cyanoacrylate is 2: 1.
the liquid medical dressing according to the present invention, wherein the cellulose nitrate has an N content of 10 to 12%.
In a specific embodiment, the cellulose nitrate has an N content of 11.0%.
The liquid medical dressing provided by the invention is prepared by the following steps of: adding 1 part of graphite oxide into 100 and 300 parts of deionized water, and ultrasonically stirring for 0.2-2h at the temperature of 0-10 ℃ to obtain a graphene oxide suspension; adding 1-5 parts of dopamine hydrochloride, and adjusting the pH value to 8.0-10.0; stirring and reacting for 12-72h at 50-70 ℃; centrifuging, washing with water for 1-5 times, and vacuum drying.
In a specific embodiment, the dopamine-graphene oxide is prepared as follows: adding 1 part of graphite oxide into 200 parts of deionized water, and ultrasonically stirring for 0.5h at the temperature of 5 ℃ to obtain a graphene oxide suspension; adding 3 parts of dopamine hydrochloride, and adjusting the pH value to 9.0; stirring and reacting for 24 hours at the temperature of 60 ℃; centrifuging, washing with water for 1-5 times, and vacuum drying.
The liquid medical dressing according to the present invention, wherein the organic solvent is selected from a mixture of ethanol, ethyl acetate and butyl acetate; and/or the weight ratio of the three is (2.4-2.8): (1.6-2.0): 1.
in a specific embodiment, the weight ratio of the three is 2.56: 1.86: 1.
in another aspect, the invention provides a preparation method of the novel bacteriostatic film-forming liquid medical dressing, wherein the method comprises the following steps:
adding the film-forming material with the formula amount into an organic solvent, and mixing and stirring; adding D-limonene, benzyl alcohol, castor oil, isopropyl palmitate and clove oil, mixing and stirring; under the stirring condition, adding dopamine-graphene oxide powder, functionalized halloysite nanotubes and camphor, and carrying out ultrasonic stirring to obtain the novel antibacterial film-forming liquid medical dressing.
Compared with the prior art, the film formed by the novel bacteriostatic film-forming liquid medical dressing has optimized mechanical strength, and does not basically damage the air permeability and bacteriostatic performance.
Detailed Description
It must be noted that, as used in this specification and the appended claims, the singular forms "a," "an," and "the" include both one and more than one (i.e., two, including two) unless the context clearly dictates otherwise.
Unless otherwise indicated, the numerical ranges in this disclosure are approximate and thus may include values outside of the stated ranges. The numerical ranges may be stated herein as from "about" one particular value, and/or to "about" another particular value. When such a range is expressed, another aspect includes from the one particular value and/or to the other particular value. Similarly, when values are expressed as approximations, by use of the antecedent "about," it will be understood that the particular value forms another aspect. It will be further understood that the endpoints of each of the numerical ranges are significant both in relation to the other endpoint, and independently of the other endpoint.
Reference in the specification and concluding claims to parts by weight of a particular element or component in a composition or article refers to the weight relationship between that element or component and any other elements or components in the composition or article, expressed as parts by weight.
In the present invention, unless specifically indicated to the contrary, or implied from the context or customary practice in the art, all solutions referred to herein are aqueous solutions; when the solute of the aqueous solution is a liquid, all fractions and percentages are by volume and the volume percentages of a component are based on the total volume of the composition or product in which it is contained; when the solute of the aqueous solution is a solid, all fractions and percentages are by weight, and the weight percentages of a component are based on the total weight of the composition or product in which the component is included.
References to "comprising," "including," "having," and similar terms in this specification are not intended to exclude the presence of any optional components, steps or procedures, whether or not any optional components, steps or procedures are specifically disclosed. In order to avoid any doubt, all methods claimed through use of the term "comprising" may include one or more additional steps, apparatus parts or components and/or materials unless stated to the contrary. In contrast, the term "consisting of … …" excludes any component, step, or procedure not specifically recited or recited. Unless otherwise specified, the term "or" refers to the listed members individually as well as in any combination.
Furthermore, the contents of any referenced patent or non-patent document in this application are incorporated by reference in their entirety, especially with respect to definitions disclosed in the art (where not inconsistent with any definitions specifically provided herein) and general knowledge.
In the present invention, parts are parts by weight unless otherwise indicated, temperatures are all expressed in degrees celsius or at ambient temperature, and pressures are at or near atmospheric. The room temperature means 20-30 ℃. There are many variations and combinations of reaction conditions (e.g., component concentrations, desired solvents, solvent mixtures, temperatures, pressures, and other reaction ranges) as well as conditions that can be used to optimize the purity and yield of the product obtained by the process. Only reasonable routine experimentation will be required to optimise such process conditions.
In the present invention, untreated halloysite nanotubes were purchased from Sigma-Aldrich; the inner diameter of the halloysite nanotube is 10-30 nm; the outer diameter is 50-70 nm; the length is 1-3 mu m; specific surface area 64m 2 (ii)/g; the pore volume is 1.26-1.34 mL/g.
Example 1
The novel bacteriostatic film-forming liquid medical dressing comprises the following raw materials:
50 parts of nitrocellulose (N% = 11.0%);
25 parts of alpha-octyl cyanoacrylate;
20 parts of D-limonene;
40 parts of dopamine-graphene oxide;
24 parts of functionalized halloysite nanotubes;
60 parts of benzyl alcohol;
20 parts of castor oil;
5 parts of camphor;
20 parts of isopropyl palmitate;
1 part of clove oil;
359 parts of ethanol;
260 parts of ethyl acetate;
and 140 parts of butyl acetate.
The preparation method of the dopamine-graphene oxide powder comprises the following steps: adding 1 part of graphite oxide into 200 parts of deionized water, and ultrasonically stirring for 0.5h at the temperature of 5 ℃ to obtain a graphene oxide suspension. Adding 3 parts of dopamine hydrochloride, and adjusting the pH value to 9.0; the reaction was stirred at 60 ℃ for 24 h. Centrifuging, washing with water for 3 times, and vacuum drying.
The preparation method of the functionalized halloysite nanotube comprises the following steps: according to the weight ratio of 1 g: 10mL of halloysite nanotubes (inner diameter of 10-30nm, outer diameter of 50-70nm, length of 1-3 μm, and specific surface area of 64 m) 2 (ii)/g; pore volume 1.26-1.34 mL/g) was placed in 2M HCl solution and reacted at 75 ℃ for 4 h. And (4) carrying out solid-liquid separation, washing with deionized water, and carrying out vacuum drying to obtain the treated halloysite nanotube. Then according to the volume ratio of 1:15, gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane (KH-560) and toluene are mixed evenly, treated halloysite nanotubes with the weight of 1/2 which is equivalent to the weight of KH-560 are added, ultrasonic treatment is carried out to ensure that the mixture is dispersed evenly, and reflux reaction is carried out for 8 hours at the temperature of 90 ℃. Centrifuging for many times, washing by using methylbenzene, and drying in vacuum to obtain the functionalized halloysite nanotube.
The preparation method of the novel antibacterial film-forming liquid medical dressing comprises the following steps: adding the cellulose nitrate and the octyl alpha-cyanoacrylate into ethanol, ethyl acetate and butyl acetate, mixing and stirring; adding D-limonene, benzyl alcohol, castor oil, isopropyl palmitate and clove oil, mixing and stirring; under the stirring condition, adding dopamine-graphene oxide powder, functionalized halloysite nanotubes and camphor, and carrying out ultrasonic stirring for 0.5h to obtain the novel antibacterial film-forming liquid medical dressing.
Comparative example 1
Chinese patent application publication CN114306729A example 1.
Comparative example 2
The bacteriostatic film-forming liquid medical dressing comprises the following raw materials:
50 parts of nitrocellulose (N% = 11.0%);
25 parts of octyl alpha-cyanoacrylate;
20 parts of D-limonene;
40 parts of dopamine-graphene oxide;
24 parts of a functionalized halloysite nanotube;
60 parts of benzyl alcohol;
20 parts of castor oil;
5 parts of camphor;
20 parts of isopropyl palmitate;
1 part of clove oil;
359 parts of ethanol;
260 parts of ethyl acetate;
and 140 parts of butyl acetate.
The preparation method of the dopamine-graphene oxide powder comprises the following steps: adding 1 part of graphite oxide into 200 parts of deionized water, and ultrasonically stirring for 0.5h at the temperature of 5 ℃ to obtain a graphene oxide suspension. Adding 3 parts of dopamine hydrochloride, and adjusting the pH value to 9.0; the reaction was stirred at 60 ℃ for 24 h. Centrifuging, washing with water for 3 times, and vacuum drying.
The preparation method of the functionalized halloysite nanotube comprises the following steps: uniformly mixing gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane (KH-560) and toluene according to the volume ratio of 1:15, and adding halloysite nanotubes (10-30 nm in inner diameter, 50-70nm in outer diameter, 1-3 μm in length and 64m in specific surface area, wherein the weight of the halloysite nanotubes is 1/2 in weight of KH-560 2 (iv) g; pore volume 1.26 to 1.34 mL/g), evenly dispersing by ultrasonic, and carrying out reflux reaction for 8 hours at the temperature of 90 ℃. Centrifuging for many times, washing by using methylbenzene, and drying in vacuum to obtain the functionalized halloysite nanotube.
The preparation method of the bacteriostatic film-forming liquid medical dressing comprises the following steps: adding the cellulose nitrate and the octyl alpha-cyanoacrylate into ethanol, ethyl acetate and butyl acetate, mixing and stirring; adding D-limonene, benzyl alcohol, castor oil, isopropyl palmitate and clove oil, mixing and stirring; under the stirring condition, adding dopamine-graphene oxide powder, functionalized halloysite nanotubes and camphor, and ultrasonically stirring for 0.5h to obtain the antibacterial film-forming liquid medical dressing.
Comparative example 3
The bacteriostatic film-forming liquid medical dressing comprises the following raw materials:
50 parts of nitrocellulose (N% = 11.0%);
25 parts of alpha-octyl cyanoacrylate;
20 parts of D-limonene;
40 parts of dopamine-graphene oxide;
24 parts of treated halloysite nanotubes;
60 parts of benzyl alcohol;
20 parts of castor oil;
5 parts of camphor;
20 parts of isopropyl palmitate;
1 part of clove oil;
359 parts of ethanol;
260 parts of ethyl acetate;
and 140 parts of butyl acetate.
The preparation method of the dopamine-graphene oxide powder comprises the following steps: adding 1 part of graphite oxide into 200 parts of deionized water, and ultrasonically stirring for 0.5h at the temperature of 5 ℃ to obtain a graphene oxide suspension. Adding 3 parts of dopamine hydrochloride, and adjusting the pH value to 9.0; the reaction was stirred at 60 ℃ for 24 h. Centrifuging, washing with water for 3 times, and vacuum drying.
Meridian pointThe preparation method of the halloysite nanotube comprises the following steps: according to the weight ratio of 1 g: 10mL of halloysite nanotubes (inner diameter of 10-30nm, outer diameter of 50-70nm, length of 1-3 μm, and specific surface area of 64 m) 2 (ii)/g; pore volume 1.26-1.34 mL/g) was placed in 2M HCl solution and reacted at 75 ℃ for 4 h. And (4) carrying out solid-liquid separation, washing with deionized water, and carrying out vacuum drying to obtain the treated halloysite nanotube.
The preparation method of the bacteriostatic film-forming liquid medical dressing comprises the following steps: adding the cellulose nitrate and the octyl alpha-cyanoacrylate into ethanol, ethyl acetate and butyl acetate according to the formula ratio, and mixing and stirring; adding D-limonene, benzyl alcohol, castor oil, isopropyl palmitate and clove oil, mixing and stirring; and adding dopamine-graphene oxide powder, the treated halloysite nanotube and camphor under stirring, and ultrasonically stirring for 0.5h to obtain the antibacterial film-forming liquid medical dressing.
Performance testing
The bacteriostatic film-forming liquid medical dressing of example 1 and comparative examples 2-3 was applied to a wound surface according to the weight ratio of 1 g: adding 10mL of the medical dressing film into a mixed solvent of ethanol and ethyl acetate with the volume ratio of 1.4:1, and volatilizing the solvent to obtain the antibacterial film-forming liquid medical dressing film. Using the unit area (cm) of the film passing in the unit time (h) 2 ) Evaluation of moisture vapor quality (mg), i.e., moisture vapor Permeability (MVTR) of the film 2 H). The air permeability of comparative example 1 was directly determined by the test data of example 1 of chinese patent application publication CN 114306729A.
The tensile strength and the elongation at break of the bacteriostatic film-forming liquid medical dressing film of the example 1 and the comparative examples 1 to 3 are measured by a tensile testing machine. The tensile strength is the ratio of the force borne by the film at the moment of tensile failure to the area of the film, and the parameter is a standard for evaluating the maximum tensile force which can be borne by the medical dressing; and the elongation at break is the ratio of the elongation length of the film at the moment of tensile fracture to the initial length of the film, and is a standard for evaluating the toughness of the medical dressing. The tensile strength and elongation at break of comparative example 1 were measured in the same manner.
Test example 1 and comparative examples 2-3 antimicrobial film-forming liquid medical dressings were tested against E.coli and S.aureusThe performance of the bacterium. Coli and s.aureus were cultured for 2d at 35 ℃ using nutrient broth. Selecting a certain amount of bacterial colony, fully scattering the bacterial colony in physiological saline, and adjusting the concentration of bacterial suspension to 5 multiplied by 10 6 cfu/mL. A100 mm culture dish is added with 20mL of dissolved nutrient agar culture solution, and the mixture is solidified to prepare a culture medium plate. And uniformly coating the bacterial suspension on a culture medium flat plate to obtain a bacterial-containing flat plate. Experimental groups 10 mu L of the medical dressing of the bacteriostatic film-forming liquid in example 1 and comparative examples 2-3 are respectively taken on a bacteria-containing flat plate, and 8mm sterile blank filter paper sheets are covered after dripping, wherein the blank groups adopt the sterile blank filter paper sheets with the diameter of 8 mm. Culturing for 72h at 37 ℃ in a water-proof constant-temperature incubator, observing the size of each inhibition zone and recording the diameter of each inhibition zone. The antibacterial performance of comparative example 1 was directly determined by the test data of example 1 of chinese patent application publication CN 114306729A.
The results are shown in Table 1.
TABLE 1
As can be seen from Table 1, compared with comparative examples 1-3, the film formed by the novel bacteriostatic film-forming liquid medical dressing of example 1 of the invention has optimized mechanical strength, and meanwhile, the air permeability and bacteriostatic performance are not substantially damaged.
Furthermore, it should be understood that various changes, substitutions, deletions, modifications or adjustments may be made by those skilled in the art after reading the disclosure of the present invention, and such equivalents are also within the scope of the invention as defined in the appended claims.
Claims (10)
1. The novel bacteriostatic film-forming liquid medical dressing is characterized by comprising the following raw materials in formula:
60-90 parts of a film forming material;
10-30 parts of D-limonene;
30-50 parts of dopamine-graphene oxide;
20-28 parts of a functionalized halloysite nanotube;
45-75 parts of benzyl alcohol;
10-30 parts of castor oil;
2-8 parts of camphor;
10-30 parts of isopropyl palmitate;
0.5-2 parts of clove oil;
600 portions and 900 portions of organic solvent.
2. The liquid medical dressing of claim 1, wherein the functionalized halloysite nanotubes are obtained from treated halloysite nanotubes that have been functionally modified using gamma- (2, 3-glycidoxy) propyltrimethoxysilane.
3. The liquid medical dressing of claim 2, wherein the weight ratio of the treated halloysite nanotubes to gamma- (2, 3-glycidoxy) propyltrimethoxysilane is 1: (1.5-2.5).
4. The liquid medical dressing of claim 2, wherein the functionalization modification conditions are: the reaction time is 4-12h at 80-100 ℃.
5. The liquid medical dressing according to claim 2, wherein the treated halloysite nanotubes are obtained by reacting halloysite nanotubes in 1-3M HCl solution at 60-90 ℃ for 2-6 h.
6. The liquid medical dressing of claim 5, wherein the halloysite nanotubes have an inner diameter of 10-30 nm; the outer diameter is 50-70 nm; the length is 1-3 mu m; specific surface area 64m 2 (ii)/g; the pore volume is 1.26-1.34 mL/g.
7. The liquid medical dressing of claim 1, wherein the film-forming material is selected from the group consisting of a combination of nitrocellulose and octyl alpha-cyanoacrylate; and/or the weight ratio of the cellulose nitrate to the octyl alpha-cyanoacrylate is (1.5-2.5): 1; and/or the N content of the nitrocellulose is 10-12%.
8. The liquid medical dressing of claim 1, wherein the dopamine-graphene oxide is prepared by the following method: adding 1 part of graphite oxide into 100 and 300 parts of deionized water, and ultrasonically stirring for 0.2-2h at the temperature of 0-10 ℃ to obtain a graphene oxide suspension; adding 1-5 parts of dopamine hydrochloride, and adjusting the pH value to 8.0-10.0; stirring and reacting for 12-72h at 50-70 ℃; centrifuging, washing with water for 1-5 times, and vacuum drying.
9. The liquid medical dressing according to claim 1, wherein the organic solvent is selected from the group consisting of a mixture of ethanol, ethyl acetate and butyl acetate; and/or the weight ratio of the three is (2.4-2.8): (1.6-2.0): 1.
10. a method for preparing a novel bacteriostatic film-forming liquid medical dressing according to any one of claims 1-9, wherein the method comprises the following steps:
adding the film-forming material with the formula amount into an organic solvent, and mixing and stirring; adding D-limonene, benzyl alcohol, castor oil, isopropyl palmitate and clove oil, mixing and stirring; under the condition of stirring, adding dopamine-graphene oxide powder, functionalized halloysite nanotubes and camphor, and ultrasonically stirring to obtain the novel bacteriostatic film-forming liquid medical dressing.
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| CN117017840A (en) * | 2023-09-20 | 2023-11-10 | 广东时尚女孩生物科技有限公司 | Gel based on long-acting antibacterial function and preparation method thereof |
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