A hydrogel dressing and a method of making the same
Patent Information
- Application Number
- CN202610361242.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2026-03-24
- Publication Date
- 2026-10-30
- Estimated Expiration
- 2046-03-24
AI Technical Summary
[0004]为了解决现有技术中蜂蜜敷料易于结晶的问题,本发明提供一种水凝胶敷料,该水凝胶敷料通过引入蜂蜜-普鲁兰多糖复配抗结晶体系抑制葡萄糖分子重排结晶,解决了现有技术中蜂蜜敷料易于结晶的问题
本发明提供的水凝胶敷料,通过引入普鲁兰多糖与蜂蜜多重氢键网络,利用空间位阻效应有效抑制葡萄糖分子重排析出,显著抑制蜂蜜结晶;避免了传统蜂蜜敷料因结晶产生的颗粒感,提升了敷料与皮肤接触的舒适度。
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Abstract
Description
Technical Field
[0001] This invention relates to the field of medical dressing technology, and more particularly to a hydrogel dressing and its preparation method. Background Technology
[0002] Honey, as a natural antibacterial substance, is widely used in medical dressings due to its broad-spectrum antibacterial properties and healing-promoting effects. However, as a supersaturated sugar solution, honey's glucose is prone to crystallization, leading to a grainy texture and reduced comfort in the dressing. Repeated melting can also produce hydroxymethylfurfural, which destroys the active ingredients and irritates the skin.
[0003] Therefore, how to inhibit honey crystallization in dressings is a technical problem that urgently needs to be solved. Summary of the Invention
[0004] To address the problem of easy crystallization in existing honey dressings, this invention provides a hydrogel dressing that introduces a honey-pullulan polysaccharide complex anti-crystallization system to inhibit glucose molecule rearrangement and crystallization, thus solving the problem of easy crystallization in existing honey dressings.
[0005] The technical solution adopted by this invention to solve its technical problem is: A hydrogel dressing includes a functional layer; the functional layer is formed by UV curing of a mixture of raw materials; wherein, by weight, the mixture comprises the following components: 20-30 parts of UV-curable monomer; Crosslinking agent 0.10-0.22 parts; Viscosity modifier 1.0-1.5 parts; 12-22 parts of moisturizer; 25-35 parts honey; Pullulan 0.05-0.3 parts; Photoinitiator 0.10-0.25 parts; Water 23-27 parts.
[0006] Optionally, the honey is selected from at least one of Manuka honey, buckwheat honey, wax tree honey, Jala honey, Marie honey, stingless bee honey, Scrophularia honey, Gallnut honey, Fennel honey, and wolfberry honey.
[0007] Optionally, the honey is Manuka honey.
[0008] Optionally, the UV-curable monomer is N,N-dimethylacrylamide.
[0009] Optionally, the crosslinking agent is N,N-methylenebisacrylamide.
[0010] Optionally, the viscosity modifier is sodium carboxymethyl cellulose.
[0011] Optionally, the moisturizer is glycerin.
[0012] Optionally, the photoinitiator is selected from at least one of photoinitiator 2959, photoinitiator 1173, photoinitiator 184, photoinitiator TPO-L, and photoinitiator 819.
[0013] Optionally, it may also include a substrate layer stacked with the functional layer; the substrate layer is a mesh fabric.
[0014] Another object of the present invention is to provide a method for preparing the hydrogel dressing as described above, comprising the following steps: S1: Add the viscosity modifier to water under stirring according to the formula amount to obtain solution A; S2: Pullulan was added to water under stirring to obtain solution B; S3: Mix the solution A, the solution B, honey, humectant and the remaining water, and stir at 30-40°C to obtain mixture C; S4: Mix the UV-curable monomer, crosslinking agent, and photoinitiator to obtain mixture D; S5: Mix the mixture C with the mixture D to obtain mixture E; S6: Coat the mixture E onto the release film, lay the mesh fabric flat and adhere it tightly, and cure with UV to obtain the hydrogel dressing.
[0015] The beneficial effects of this invention are: The hydrogel dressing provided by this invention introduces pullulan polysaccharide and honey multiple hydrogen bond network, which effectively inhibits glucose molecule rearrangement and precipitation by utilizing steric hindrance effect, and significantly inhibits honey crystallization; it avoids the grainy feeling caused by crystallization in traditional honey dressings and improves the comfort of the dressing in contact with the skin. Detailed Implementation
[0016] The present invention will now be described in further detail. The embodiments described below are exemplary and intended to explain the present invention, and should not be construed as limiting the present invention. All other embodiments obtained by those skilled in the art based on the embodiments of the present invention without inventive effort are within the scope of protection of the present invention.
[0017] To address the problem of easy crystallization in existing honey dressings, this invention provides a hydrogel dressing comprising a functional layer; the functional layer is formed by UV curing of a mixture of raw materials; wherein, by weight, the mixture comprises the following components: 20-30 parts of UV-curable monomer; Crosslinking agent 0.10-0.22 parts; Viscosity modifier 1.0-1.5 parts; 12-22 parts of moisturizer; 25-35 parts honey; Pullulan 0.05-0.3 parts; Photoinitiator 0.10-0.25 parts; Water 23-27 parts.
[0018] In this mixture, honey exhibits multiple antibacterial mechanisms; the specific mechanisms are as follows: (1) High osmotic pressure effect: The sugar content in honey is as high as about 80%, which forms a hyperosmotic environment, causing bacterial cells to dehydrate and undergo plasmolysis, thus inhibiting their growth and reproduction; (2) Hydrogen peroxide generation: Glucose oxidase in honey catalyzes the generation of hydrogen peroxide from glucose in a diluted state, which destroys the bacterial cell membrane structure; (3) Methylglyoxal (MGO) specific antibacterial: The high concentration of MGO in Manuka honey can penetrate the bacterial cell membrane, interfere with its metabolic pathway, and produce an irreversible bactericidal effect.
[0019] To inhibit honey crystallization, this invention introduces pullulan polysaccharide; this pullulan polysaccharide serves as a core anti-crystallization and functional synergistic component, achieving a dual effect: (1) Anti-crystallization mechanism: Pullulan is a water-soluble linear polysaccharide. A large number of hydroxyl groups in the molecule can form multiple hydrogen bonds with water molecules and glucose molecules in honey, reducing the mobility and precipitation rate of glucose molecules. At the same time, its linear long chain molecules will form steric hindrance in the honey system, hindering the aggregation of glucose molecules and the formation of crystal nuclei, thus inhibiting crystallization from the source.
[0020] (2) Protection and sustained release of active ingredients: Pullulan is a linear polysaccharide molecule. Its numerous hydroxyl groups can form multiple hydrogen bonds with water molecules and active ingredients in honey, constructing a stable molecular network in the functional layer of the dressing. This network can effectively slow down the release rate of antibacterial active substances (such as hydrogen peroxide, methylglyoxal, etc.) from honey to the wound, avoiding rapid loss at one time, and achieving a continuous and stable supply of antibacterial ingredients, thereby prolonging the effective antibacterial time of the dressing.
[0021] (3) Functional enhancement mechanism: Pullulan has excellent film-forming properties, which can form a dense and breathable film on the surface of the dressing, reduce the evaporation of wound moisture and the loss of honey active ingredients, and improve the long-lasting moisturizing effect of the dressing; at the same time, pullulan forms a large number of hydrogen bonds with sugar molecules in honey, which enhances the cohesion and cross-linking density of the hydrogel network, and improves its mechanical strength and structural stability.
[0022] During the UV curing process, the photoinitiator rapidly generates active free radicals under UV light, initiating the cross-linking polymerization of the UV-curing monomers and cross-linking agents, thus achieving rapid curing of the functional layer. A viscosity modifier adjusts the viscosity of the functional layer system, ensuring uniform spreading of the mixture on the PET release film during preparation and avoiding performance differences caused by uneven coating. The humectant, on the one hand, works synergistically with pullulan and the viscosity modifier to enhance the system's moisturizing ability, creating a moist healing environment for the wound; on the other hand, it increases the flexibility of the hydrogel, preventing discomfort caused by the dressing's brittleness and improving its adhesion to the skin.
[0023] The hydrogel dressing provided by this invention introduces pullulan polysaccharide and honey multiple hydrogen bond network, which effectively inhibits glucose molecule rearrangement and precipitation by utilizing steric hindrance effect, and significantly inhibits honey crystallization; it avoids the grainy feeling caused by crystallization in traditional honey dressings and improves the comfort of the dressing in contact with the skin.
[0024] To balance the physicochemical stability and clinical performance of the dressing, the present invention further preferably includes the following components by weight: 23-28 parts of UV-curable monomer; Crosslinking agent 0.15-0.20 parts; Viscosity modifier 1.2-1.4 parts; 15-20 parts of moisturizer; 28-33 parts honey; Pullulan 0.1-0.25 parts; Photoinitiator 0.15-0.22 parts; Water 23-27 parts.
[0025] Specifically, the honey of this invention is preferably selected from at least one of Manuka honey, buckwheat honey, wax tree honey, Jala honey, Marie honey, stingless bee honey, Scrophularia honey, Gallnut honey, Fennel honey, and wolfberry honey; and is further preferably Manuka honey, and preferably has a Manuka factor (UMF) ≥ 8+.
[0026] The preferred UV-curing monomer of this invention is N,N-dimethylacrylamide (DMAA), which has high double bond reactivity and low steric hindrance in its molecular structure, good compatibility with reducing sugars and polyphenols in honey, and the resulting polymer has a moderate glass transition temperature, ensuring that the dressing is in a soft gel state at body temperature and has moderate cohesion.
[0027] The preferred crosslinking agent is N,N-methylenebisacrylamide (BIS), whose bisacrylamide structure can form a dense but elastic three-dimensional network with DMAA. If its dosage is less than 0.10 parts, the gel strength is insufficient and it is easy to swell and break. If it is more than 0.22 parts, the network is too dense, which inhibits the slow release of honey active ingredients and reduces water vapor permeability.
[0028] DMAA and BIS, as the core monomers and crosslinking agents of the UV curing system, rapidly form a three-dimensional network crosslinking structure under the action of photoinitiators and UV light, fixing active ingredients and functional components such as honey and pullulan polysaccharide in the three-dimensional network and preventing component loss; at the same time, the three-dimensional network structure has good swelling properties, which can lock in moisture and further improve the moisturizing performance of the dressing.
[0029] The preferred viscosity modifier of this invention is sodium carboxymethyl cellulose (CMC), whose anionic properties form weak coordination with organic acids and metal ions in honey, effectively suppressing stringing and splashing in the high-sugar system during stirring and coating.
[0030] The preferred moisturizer of this invention is glycerin, whose triol structure forms a strong hydrogen bond network with water molecules, and works synergistically with glucose / fructose in honey to achieve dual moisturizing.
[0031] In this invention, glycerin acts as both a humectant and a plasticizer. On the one hand, it works synergistically with pullulan and CMC to enhance the system's moisturizing ability and create a moist healing environment for the wound. On the other hand, it increases the flexibility of the hydrogel, avoiding discomfort caused by the dressing's brittleness and improving its adhesion to the skin.
[0032] The preferred photoinitiator of this invention is selected from at least one of photoinitiator 2959, photoinitiator 1173, photoinitiator 184, photoinitiator TPO-L, and photoinitiator 819; further, the preferred photoinitiator of this invention is photoinitiator 2959, which has a high molar absorptivity at a dominant wavelength of 365 nm, non-toxic fragments, does not yellow, and has no photosensitizing quenching effect with flavonoids in honey.
[0033] This photoinitiator rapidly generates active free radicals under UV light, initiating the cross-linking polymerization of DMAA and BIS, achieving rapid curing of the functional layer. The curing process is gentle, produces no harmful substances, and does not damage the activity of honey and pullulan polysaccharides.
[0034] Traditional honey dressings often use foam or film substrates, which suffer from poor adhesion and insufficient moisturizing properties. Therefore, this invention preferably includes a substrate layer stacked on top of the functional layer in the hydrogel dressing, and more preferably, this substrate layer is a mesh fabric.
[0035] Sodium carboxymethyl cellulose (CMC) in the functional components of this invention acts as both a viscosity modifier and a binder. On the one hand, it adjusts the viscosity of the functional layer system to ensure uniform spreading of the mixture on the PET release film and avoid performance differences caused by uneven coating. On the other hand, it enhances the bonding force between the hydrogel and the medical mesh substrate, prevents the functional layer from falling off during use, and improves the structural stability of the dressing.
[0036] The broad-spectrum mesh substrate selected in this invention is suitable for different wound needs. Its porous structure ensures the breathability of the dressing, avoiding infection and delayed healing caused by heat and stuffiness. At the same time, the flexible structure of the mesh can deform with the contour of the skin, improving the fit to the wound and reducing the feeling of foreign body during use.
[0037] The hydrogel dressing provided by this invention uses a mesh fabric as a substrate and loads a honey-pullulan polysaccharide complex anti-crystallization system onto a hydrogel carrier. Pullulan polysaccharide, with its unique linear polysaccharide structure, forms a multi-hydrogen bond network with glucose and fructose in honey. On the one hand, it inhibits glucose molecule rearrangement and crystallization through steric hindrance; on the other hand, it forms a continuous and dense protective film, enhancing the film-forming and moisturizing properties of the dressing. At the same time, the synergistic hydrogen bonding effect of the complex system enhances the mechanical strength of the hydrogel network. The components are fixed by a UV curing process, and the honey activity is preserved through low-temperature operation throughout the process, taking into account both the physicochemical stability and clinical performance of the dressing.
[0038] Currently, to address the issue of honey crystallization in dressings, heat treatment and physical methods such as ultrafiltration and ultrasound are commonly used. However, heat treatment reduces the antibacterial activity of honey, while ultrafiltration and ultrasound methods involve high equipment costs. This invention employs a low-temperature process to protect the activity and ensure antibacterial efficacy. Specifically, it uses a UV curing process, operating entirely at low temperatures, avoiding the damage to the active ingredients in honey caused by heat treatment. This preserves the natural broad-spectrum antibacterial properties and healing-promoting effects of honey, ensuring the bioactivity of the dressing.
[0039] In summary, this invention utilizes pullulan's film-forming properties and UV-cured three-dimensional cross-linked structure to dual-lock antibacterial components, preventing loss and significantly extending the effective antibacterial time of the dressing. This provides long-lasting antibacterial protection for the wound, solving the problems of easy loss of antibacterial components and short-lasting efficacy in traditional honey dressings. The synergistic hydrogen bonding between pullulan and honey strengthens the cohesion of the hydrogel network. Combined with the cross-linking and thickening effects of N,N-dimethylacrylamide (DMAA) and sodium carboxymethyl cellulose (CMC), the mechanical strength, extensibility, and structural integrity of the functional layer are improved, enhancing the mechanical properties and structural stability of the hydrogel. Pullulan forms a continuous and dense protective film in the system, enhancing the film-forming properties of the dressing on the wound surface. Combined with moisturizing ingredients such as glycerin, it effectively locks in moisture, maintains a moist wound environment, and promotes wound healing. In addition, the use of mesh fabric as the base layer and composite hydrogel functional layer not only utilizes the high moisturizing properties of hydrogel to provide a moist healing environment, but also ensures the breathability of the dressing through the mesh structure of the mesh fabric, thus optimizing the dressing structure and taking into account both fit and breathability.
[0040] Another object of the present invention is to provide a method for preparing the hydrogel dressing as described above, the method comprising the following steps: S1: Add the viscosity modifier to water under stirring according to the formula amount to obtain solution A; Specifically, in this step, an accurate amount of sodium carboxymethyl cellulose (CMC) is slowly added to purified water under high-speed shear stirring, and stirring is continued to ensure that the sodium carboxymethyl cellulose (CMC) is completely dissolved, resulting in a transparent, viscous, homogeneous solution A. S2: Pullulan was added to water under stirring to obtain solution B; In this step, an accurate amount of pullulan is slowly added to purified water with stirring, and the stirring is continued to ensure that the pullulan is completely dissolved, resulting in a clear and homogeneous solution B. S3: Mix solution A, solution B, honey, humectant and remaining water, and stir at 30-40℃ to obtain mixture C; In this step, accurately measured amounts of solution A, solution B, honey, glycerin, and the remaining purified water are mixed and stirred at 30-40°C until smooth and homogeneous to obtain mixture C. S4: Mix the UV-curable monomer, crosslinking agent, and photoinitiator to obtain mixture D; In this step, accurately measured amounts of N,N-dimethylacrylamide (DMAA), N,N-methylenebisacrylamide (BIS), and photoinitiator are stirred and dissolved until colorless and transparent to obtain mixture D; S5: Mix mixture C with mixture D to obtain mixture E; In this step, mixture C and mixture D are stirred until they are in a homogeneous state without particles to obtain mixture E; S6: Apply mixture E onto the release film, lay the mesh fabric flat and adhere it tightly, and cure with UV to obtain the hydrogel dressing; In this step, mixture E is coated onto the silicone side of the PET release film, a mesh is laid flat and tightly adhered, and curing is completed using a mercury lamp UV curing machine; the hydrogel is removed from the mold and cut into predetermined sizes using the mold; the cut hydrogel sheets are placed in sterile packaging bags, sealed, and sterilized to obtain the final product.
[0041] The method for preparing hydrogel dressings provided by this invention introduces pullulan polysaccharide and honey into a multiple hydrogen bond network, effectively inhibiting glucose molecule rearrangement and precipitation by utilizing steric hindrance effect, and significantly inhibiting honey crystallization; it avoids the grainy feel caused by crystallization in traditional honey dressings and improves the comfort of the dressing in contact with the skin.
[0042] To make the above-mentioned objects, features and advantages of the present invention more apparent and understandable, specific embodiments of the present invention will be described in detail below with reference to the accompanying drawings. Example 1
[0043] This embodiment provides a method for preparing a hydrogel dressing, including the following steps: S1: Take 18.0 parts by weight of purified water and slowly add 1.2 parts of sodium carboxymethyl cellulose (CMC) while stirring at 600 r / min. Continue stirring until completely dissolved to obtain a transparent and viscous solution A. S2: Take 5.0 parts of purified water, and slowly add 0.2 parts of pullulan polysaccharide while stirring at 400 r / min. Continue stirring until completely dissolved to obtain a transparent solution B; S3: Mix solution A from step S1, solution B from step S2, 30 parts of Manuka honey (UMF 10+), 18 parts of glycerol, and the remaining purified water (2.22 parts), and stir at 30-40℃ and 400r / min until smooth and uniform to obtain mixture C; S4: Mix 25 parts of N,N-dimethylacrylamide (DMAA), 0.18 parts of N,N-methylenebisacrylamide (BIS), and 0.2 parts of photoinitiator 2959, and stir until completely dissolved to obtain mixture D; S5: Mix mixture C with mixture D, and stir at 400 r / min under light-protected conditions until uniform and free of particles to obtain mixed raw material E; S6: Evenly coat the mixed raw material E onto the silicone-containing surface of the PET release film to a thickness of 1.5mm. Then, lay a polyester fiber mesh flat on top of the mixed raw material E and gently press it to ensure complete impregnation and adhesion. Place it in a UV curing machine equipped with a mercury lamp and irradiate it for 45 seconds at 100W power and a curing distance of 15cm to complete curing, thus obtaining a composite hydrogel with an attached functional layer. S7: Cut the cured composite hydrogel into 10cm×10cm sizes using a mold, seal it in a sterile packaging bag, and sterilize it by irradiation to obtain the final product. Example 2
[0044] This embodiment provides a method for preparing a hydrogel dressing, including the following steps: S1: Take 20.0 parts by weight of purified water and slowly add 1.4 parts of sodium carboxymethyl cellulose (CMC) while stirring at 600 r / min. Continue stirring until completely dissolved to obtain a transparent and viscous solution A. S2: Take 4.0 parts of purified water, and slowly add 0.15 parts of pullulan polysaccharide while stirring at 400 r / min. Continue stirring until completely dissolved to obtain a transparent solution B; S3: Mix solution A from step S1, solution B from step S2, 28 parts of Manuka honey (UMF 10+), 16 parts of glycerol, and the remaining purified water (2.03 parts), and stir at 30-40℃ and 400r / min until smooth and uniform to obtain mixture C; S4: Mix 28 parts of N,N-dimethylacrylamide (DMAA), 0.20 parts of N,N-methylenebisacrylamide (BIS) and 0.22 parts of photoinitiator 2959, and stir until completely dissolved to obtain mixture D; S5: Mix mixture C with mixture D, and stir at 400 r / min under light-protected conditions until uniform and free of particles to obtain mixed raw material E; S6: Evenly coat the mixed raw material E onto the silicone-containing surface of the PET release film to a thickness of 1.5mm. Then, lay a polyester fiber mesh flat on top of the mixed raw material E and gently press it to ensure complete impregnation and adhesion. Place it in a UV curing machine equipped with a mercury lamp and irradiate it for 45 seconds at 100W power and a curing distance of 15cm to complete curing, thus obtaining a composite hydrogel with an attached functional layer. S7: Cut the cured composite hydrogel into 10cm×10cm sizes using a mold, seal it in a sterile packaging bag, and sterilize it by irradiation to obtain the final product. Example 3
[0045] This embodiment provides a method for preparing a hydrogel dressing, including the following steps: S1: Take 15.0 parts by weight of purified water and slowly add 1.0 part of sodium carboxymethyl cellulose (CMC) to it while stirring at 600 r / min. Continue stirring until completely dissolved to obtain a transparent and viscous solution A. S2: Take 5.0 parts of purified water, and slowly add 0.25 parts of pullulan polysaccharide while stirring at 400 r / min. Continue stirring until completely dissolved to obtain a transparent solution B; S3: Mix solution A from step S1, solution B from step S2, 32 parts of Manuka honey (UMF 10+), 20 parts of glycerol, and the remaining purified water (3.45 parts), and stir at 30-40℃ and 400r / min until smooth and uniform to obtain mixture C; S4: Mix 23 parts of N,N-dimethylacrylamide (DMAA), 0.15 parts of N,N-methylenebisacrylamide (BIS) and 0.15 parts of photoinitiator 2959, and stir until completely dissolved to obtain mixture D; S5: Mix mixture C with mixture D, and stir at 400 r / min under light-protected conditions until uniform and free of particles to obtain mixed raw material E; S6: Evenly coat the mixed raw material E onto the silicone-containing surface of the PET release film to a thickness of 1.5mm. Then, lay a polyester fiber mesh flat on top of the mixed raw material E and gently press it to ensure complete impregnation and adhesion. Place it in a UV curing machine equipped with a mercury lamp and irradiate it for 45 seconds at 100W power and a curing distance of 15cm to complete curing, thus obtaining a composite hydrogel with an attached functional layer. S7: Cut the cured composite hydrogel into 10cm×10cm sizes using a mold, seal it in a sterile packaging bag, and sterilize it by irradiation to obtain the final product. Example 4
[0046] This embodiment provides a method for preparing a hydrogel dressing, including the following steps: S1: Take 18.0 parts by weight of purified water and slowly add 1.2 parts of sodium carboxymethyl cellulose (CMC) to it while stirring at 600 r / min. Continue stirring until completely dissolved to obtain a transparent and viscous solution A. S2: Take 5.0 parts of purified water, and slowly add 0.05 parts of pullulan polysaccharide while stirring at 400 r / min. Continue stirring until completely dissolved to obtain a transparent solution B; S3: Mix solution A from step S1, solution B from step S2, 30 parts of Manuka honey (UMF 10+), 18 parts of glycerol, and the remaining purified water (2.37 parts), and stir at 30-40℃ and 400r / min until smooth and uniform to obtain mixture C; S4: Mix 25 parts of N,N-dimethylacrylamide (DMAA), 0.18 parts of N,N-methylenebisacrylamide (BIS), and 0.2 parts of photoinitiator 2959, and stir until completely dissolved to obtain mixture D; S5: Mix mixture C with mixture D, and stir at 400 r / min under light-protected conditions until uniform and free of particles to obtain mixed raw material E; S6: Evenly coat the mixed raw material E onto the silicone-containing surface of the PET release film to a thickness of 1.5mm. Then, lay a polyester fiber mesh flat on top of the mixed raw material E and gently press it to ensure complete impregnation and adhesion. Place it in a UV curing machine equipped with a mercury lamp and irradiate it for 45 seconds at 100W power and a curing distance of 15cm to complete curing, thus obtaining a composite hydrogel with an attached functional layer. S7: Cut the cured composite hydrogel into 10cm×10cm sizes using a mold, seal it in a sterile packaging bag, and sterilize it by irradiation to obtain the final product. Example 5
[0047] This embodiment provides a method for preparing a hydrogel dressing, including the following steps: S1: Take 18.0 parts by weight of purified water and slowly add 1.2 parts of sodium carboxymethyl cellulose (CMC) to it while stirring at 600 r / min. Continue stirring until completely dissolved to obtain a transparent and viscous solution A. S2: Take 5.0 parts of purified water, and slowly add 0.2 parts of pullulan polysaccharide while stirring at 400 r / min. Continue stirring until completely dissolved to obtain a transparent solution B; S3: Mix solution A from step S1, solution B from step S2, 30 parts buckwheat honey, 18 parts glycerol, and the remaining purified water (2.22 parts), and stir at 30-40℃ and 400r / min until smooth and uniform to obtain mixture C; S4: Mix 25 parts of N,N-dimethylacrylamide (DMAA), 0.18 parts of N,N-methylenebisacrylamide (BIS), and 0.2 parts of photoinitiator 2959, and stir until completely dissolved to obtain mixture D; S5: Mix mixture C with mixture D, and stir at 400 r / min under light-protected conditions until uniform and free of particles to obtain mixed raw material E; S6: Evenly coat the mixed raw material E onto the silicone-containing surface of the PET release film to a thickness of 1.5mm. Then, lay a polyester fiber mesh flat on top of the mixed raw material E and gently press it to ensure complete impregnation and adhesion. Place it in a UV curing machine equipped with a mercury lamp and irradiate it for 45 seconds at 100W power and a curing distance of 15cm to complete curing, thus obtaining a composite hydrogel with an attached functional layer. S7: Cut the cured composite hydrogel into 10cm×10cm sizes using a mold, seal it in a sterile packaging bag, and sterilize it by irradiation to obtain the final product.
[0048] In this invention, all comparative examples are compared with Example 1.
[0049] Comparative Example 1 This comparative example provides a method for preparing a hydrogel dressing, comprising the following steps: S1: Take 18.0 parts by weight of purified water and slowly add 1.2 parts of sodium carboxymethyl cellulose (CMC) while stirring at 600 r / min. Continue stirring until completely dissolved to obtain a transparent and viscous solution A. S2: Mix solution A from step S1, 30 parts of Manuka honey (UMF 10+), 18 parts of glycerol, and the remaining purified water (7.42 parts), and stir at 30-40℃ and 400r / min until smooth and uniform to obtain mixture B; S3: Mix 25 parts of N,N-dimethylacrylamide (DMAA), 0.18 parts of N,N-methylenebisacrylamide (BIS) and 0.2 parts of photoinitiator 2959, and stir until completely dissolved to obtain mixture C; S4: Mix mixture B with mixture C, and stir at 400 r / min under light-protected conditions until uniform and free of particles to obtain mixed raw material D; S5: Evenly coat the mixed raw material D onto the silicone-containing surface of the PET release film to a thickness of 1.5 mm. Then, lay a polyester fiber mesh flat on top of the mixed raw material D and gently press it to ensure complete impregnation and adhesion. Place it in a UV curing machine equipped with a mercury lamp and irradiate it for 45 seconds at 100W power and a curing distance of 15cm to complete curing, thus obtaining a composite hydrogel with an attached functional layer. S6: Cut the cured composite hydrogel into 10cm×10cm sizes using a mold, seal it in a sterile packaging bag, and sterilize it by irradiation to obtain the final product.
[0050] Comparative Example 2 This comparative example provides a method for preparing a hydrogel dressing, comprising the following steps: S1: Take 5.0 parts by weight of purified water and slowly add 0.2 parts of pullulan polysaccharide to it while stirring at 400 r / min. Continue stirring until completely dissolved to obtain a transparent solution A. S2: Mix solution A from step S1, 30 parts of Manuka honey (UMF 10+), 18 parts of glycerol, and the remaining purified water (2.22 parts), and stir at 30-40℃ and 400r / min until smooth and uniform to obtain mixture B; S3: Mix 25 parts of N,N-dimethylacrylamide (DMAA), 0.18 parts of N,N-methylenebisacrylamide (BIS) and 0.2 parts of photoinitiator 2959, and stir until completely dissolved to obtain mixture C; S4: Mix mixture B with mixture C, and stir at 400 r / min under light-protected conditions until uniform and free of particles to obtain mixed raw material D; S5: Evenly coat the mixed raw material D onto the silicone-containing surface of the PET release film to a thickness of 1.5 mm. Then, lay a polyester fiber mesh flat on top of the mixed raw material D and gently press it to ensure complete impregnation and adhesion. Place it in a UV curing machine equipped with a mercury lamp and irradiate it for 45 seconds at 100W power and a curing distance of 15cm to complete curing, thus obtaining a composite hydrogel with an attached functional layer. S6: Cut the cured composite hydrogel into 10cm×10cm sizes using a mold, seal it in a sterile packaging bag, and sterilize it by irradiation to obtain the final product.
[0051] Comparative Example 3 This comparative example provides a method for preparing a hydrogel dressing, comprising the following steps: S1: Take 18.0 parts by weight of purified water and slowly add 1.2 parts of sodium carboxymethyl cellulose (CMC) while stirring at 600 r / min. Continue stirring until completely dissolved to obtain a transparent and viscous solution A. S2: Take 5.0 parts of purified water, and slowly add 0.2 parts of pullulan polysaccharide while stirring at 400 r / min. Continue stirring until completely dissolved to obtain a transparent solution B; S3: Mix solution A from step S1, solution B from step S2, 30 parts of Manuka honey (UMF 10+), 18 parts of glycerol, and the remaining purified water (2.22 parts), and stir at 30-40℃ and 400r / min until smooth and uniform to obtain mixture C; S4: Mix 25 parts of N,N-dimethylacrylamide (DMAA), 0.18 parts of N,N-methylenebisacrylamide (BIS), and 0.2 parts of photoinitiator 2959, and stir until completely dissolved to obtain mixture D; S5: Mix mixture C with mixture D, and stir at 400 r / min under light-protected conditions until uniform and free of particles to obtain mixed raw material E; S6: The mixed raw material E is evenly coated on the silicone-containing surface of the PET release film with a coating thickness of 1.5mm. It is then placed in a UV curing machine equipped with a mercury lamp and irradiated for 45 seconds at a power of 100W and a curing distance of 15cm to complete the curing and obtain a composite hydrogel with a functional layer attached. S7: Cut the cured composite hydrogel into 10cm×10cm sizes using a mold, seal it in a sterile packaging bag, and sterilize it by irradiation to obtain the final product.
[0052] Comparative Example 4 This comparative example provides a method for preparing a hydrogel dressing, comprising the following steps: S1: Take 18.0 parts by weight of purified water and slowly add 1.2 parts of sodium carboxymethyl cellulose (CMC) while stirring at 600 r / min. Continue stirring until completely dissolved to obtain a transparent and viscous solution A. S2: Take 5.0 parts of purified water, and slowly add 0.2 parts of pullulan polysaccharide while stirring at 400 r / min. Continue stirring until completely dissolved to obtain a transparent solution B; S3: Mix solution A from step S1, solution B from step S2, 30 parts of Manuka honey (UMF 10+), 18 parts of glycerol, and the remaining purified water (2.22 parts), and stir at 30-40℃ and 400r / min until smooth and uniform to obtain mixture C; S4: Mix 25 parts of N,N-dimethylacrylamide (DMAA), 0.18 parts of N,N-methylenebisacrylamide (BIS), and 0.2 parts of thermal initiator (ammonium persulfate), and stir until completely dissolved to obtain mixture D; S5: Mix mixture C with mixture D, and stir at 400 r / min under light-protected conditions until uniform and free of particles to obtain mixed raw material E; S6: Coat the mixed raw material E evenly on the silicone-containing surface of the PET release film with a coating thickness of 1.5mm. Then lay the polyester fiber mesh flat on the mixed raw material E and gently press it to make it completely impregnated and adhered. S7: Place the coated sample in a constant temperature drying oven and heat it at 80°C for 30 minutes to crosslink it and form a hydrogel functional layer. S8: Cut the cured composite hydrogel into 10cm×10cm sizes using a mold, seal it in a sterile packaging bag, and sterilize it by irradiation to obtain the final product.
[0053] The stability, antibacterial properties, tensile strength, water content, and water vapor transmission rate of the hydrogel dressings prepared in the above embodiments and comparative examples were tested using the following methods: 1. Product stability: The stability of the hydrogel dressings in the above embodiments and comparative examples was tested to observe their crystallization. Considering that honey is prone to crystallization below 25℃, the hydrogel dressings prepared in each embodiment and comparative example were placed in a room at 0-25℃ and 60%±5% humidity. The sample morphology and whether crystallization occurred were observed at specified time points. The test results are shown in Table 1.
[0054] 2. Antibacterial performance test: The inhibition rate of Staphylococcus aureus and Escherichia coli at 24 hours and 168 hours was tested according to GB / T 20944.3-2008 standard. The test results are shown in Table 2.
[0055] 3. Tensile strength: Tested according to ASTM D5035-11 (2019), the longitudinal and transverse tensile values at fracture were recorded, three sets of parallel tests were conducted, the average value was calculated and recorded, and the test results are shown in Table 2.
[0056] 4. Moisture content: After removing the packaging, store the product under constant temperature and humidity conditions (temperature 25℃±2℃, humidity 60%±5%) for 72 hours, and then conduct the test according to the method specified in General Chapter 0831 of the 2020 edition of the Chinese Pharmacopoeia. Three parallel tests were conducted, and the average value was calculated and recorded. The test results are shown in Table 2.
[0057] 5. Water vapor transmission rate: The 24-hour water vapor transmission rate was tested according to the method specified in 3.3 "Water vapor transmission rate of wound dressings in liquid contact" of YY / T 0471.2-2004. The test results are shown in Table 2.
[0058] Table 1 Table 2 As can be seen from the data in the table above, the hydrogel dressings prepared in the various embodiments of the present invention have excellent antibacterial properties and excellent antibacterial durability, and are stable and not prone to crystallization.
[0059] Compared with Example 1, Comparative Example 1 did not add pullulan, so it could not form a multiple hydrogen bond network with glucose and fructose in honey. It had no steric hindrance effect to inhibit glucose molecule rearrangement and crystallization, and could not build a stable molecular network to lock in antibacterial components. Glucose molecules easily aggregated and precipitated to form crystal nuclei. Although the initial antibacterial properties were good, the crystallization stability decreased significantly and the antibacterial durability was poor. At the same time, the cohesion of the hydrogel network was insufficient, and the mechanical strength and moisturizing properties were also significantly reduced.
[0060] Compared to Example 1, Comparative Example 2, without the addition of sodium carboxymethyl cellulose (CMC), cannot adjust the viscosity of the functional layer system, leading to uneven spreading during the coating process and resulting in inconsistent product thickness. Furthermore, the lack of the thickening synergistic effect of CMC significantly reduces the overall mechanical strength of the dressing.
[0061] Compared to Example 1, Comparative Example 3 did not use a mesh fabric as the substrate layer; it was molded solely with a hydrogel functional layer. Without the flexible support of the mesh fabric, the tensile strength of the hydrogel itself decreased significantly. Simultaneously, it lost the air permeability advantage of the porous structure of the mesh fabric, resulting in a substantial reduction in water vapor permeability.
[0062] Compared with Example 1, Comparative Example 4 did not use photoinitiator and UV curing process, but instead used thermal initiator and 80°C heating crosslinking process. High temperature treatment will destroy natural active ingredients such as glucose oxidase and methylglyoxal in honey, resulting in a significant reduction in the broad-spectrum antibacterial properties of honey, and a significant decrease in both initial and long-term antibacterial performance.
[0063] Based on the above-described preferred embodiments of the present invention, and through the foregoing description, those skilled in the art can make various changes and modifications without departing from the inventive concept. The technical scope of this invention is not limited to the contents of the specification, but must be determined according to the scope of the claims.
Claims
1. A hydrogel dressing, characterized in that, Includes a functional layer; the functional layer is formed by UV curing of a mixture of raw materials; wherein, by weight, the mixture comprises the following components: 20-30 parts of UV-curable monomer; Crosslinking agent 0.10-0.22 parts; Viscosity modifier 1.0-1.5 parts; 12-22 parts of moisturizer; 25-35 parts honey; Pullulan 0.05-0.3 parts; Photoinitiator 0.10-0.25 parts; Water 23-27 parts.
2. The hydrogel dressing as described in claim 1, characterized in that, The honey is selected from at least one of the following: Manuka honey, buckwheat honey, wax tree honey, Jala honey, Marie honey, stingless bee honey, Scrophularia honey, Gallnut honey, Fennel honey, and Goji berry honey.
3. The hydrogel dressing as described in claim 2, characterized in that, The honey in question is Manuka honey.
4. The hydrogel dressing as described in claim 1, characterized in that, The UV-curable monomer is N,N-dimethylacrylamide.
5. The hydrogel dressing as described in claim 1, characterized in that, The crosslinking agent is N,N-methylenebisacrylamide.
6. The hydrogel dressing as described in claim 1, characterized in that, The viscosity modifier is sodium carboxymethyl cellulose.
7. The hydrogel dressing as described in claim 1, characterized in that, The moisturizer is glycerin.
8. The hydrogel dressing as described in claim 1, characterized in that, The photoinitiator is selected from at least one of photoinitiator 2959, photoinitiator 1173, photoinitiator 184, photoinitiator TPO-L, and photoinitiator 819.
9. The hydrogel dressing according to any one of claims 1-8, characterized in that, It also includes a substrate layer stacked with the functional layer; the substrate layer is a mesh fabric.
10. A method for preparing a hydrogel dressing as described in any one of claims 1-9, characterized in that, Includes the following steps: S1: Add the viscosity modifier to water under stirring according to the formula amount to obtain solution A; S2: Pullulan was added to water under stirring to obtain solution B; S3: Mix the solution A, the solution B, honey, humectant and the remaining water, and stir at 30-40°C to obtain mixture C; S4: Mix the UV-curable monomer, crosslinking agent, and photoinitiator to obtain mixture D; S5: Mix the mixture C with the mixture D to obtain mixture E; S6: Coat the mixture E onto the release film, lay the mesh fabric flat and adhere it tightly, and cure with UV to obtain the hydrogel dressing.
Citation Information
Patent Citations
Preparation method of hydrogel dressing containing honey
CN108404202A