Medical eye protection dressing and preparation method thereof
By mixing graphene oxide-oxidized sodium hyaluronate and graphene oxide-trehalose oxide with other ingredients, the medical eye care dressings made improve breathability, solve the problem of insufficient breathability of existing eye care dressings and reduce skin irritating reactions.
Patent Information
- Application Number
- CN202510635654.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-05-16
- Publication Date
- 2025-08-05
- Estimated Expiration
- 2045-05-16
AI Technical Summary
The existing eye protection dressings are insufficient breathability, which leads to poor use and may cause adverse reactions such as itching and redness and swelling of the skin.
Graphene oxide-sodium hyaluronate oxide and graphene oxide-trehalose oxide are mixed with glycerin, Tween-80, polyglutamic acid, disodium edetic acid, calcium chloride and deionized water to form a dilute mucus matrix material, and are filled into a nonwoven aluminum-plastic film bag to make medical eye protection dressings, and the high specific surface area of graphene oxide is used to improve breathability.
It improves the breathability of eye protection dressings, reduces skin irritation, improves the comfort of use, and reduces adverse reactions such as itching and redness and swelling of the skin.
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Figure BDA0005406578130000171 
Figure BDA0005406578130000181
Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of preparation of medical biological dressing materials, and particularly relates to a medical eye-protecting dressing and a preparation method thereof. Background Art
[0002] With the rapid development of modern society, the popularity of electronic products has led to a significant increase in the time people spend using their eyes. Whether it is work, study or entertainment, staring at computer screens, mobile phones and other digital devices for a long time has led to the frequent occurrence of discomfort symptoms such as eye fatigue and dry eyes. Eye fatigue, also known as visual fatigue, is a type of discomfort caused by prolonged use of the eyes. The causes of eye fatigue include: (1) Prolonged use of eyes: Working in front of digital devices for a long time requires continuous focus of the eyes, which leads to eye muscle fatigue and thus eye discomfort; (2) Poor eye environment: Insufficient or excessive light, screen reflection, dry indoor air and other environmental factors will increase the burden on the eyes; (3) Dry eyes: Staring at the screen for a long time will reduce the number of blinks, causing tears to evaporate too quickly, the eyes become dry, and then cause discomfort; (4) Vision problems: Uncorrected vision problems, such as myopia or astigmatism, will cause more eye fatigue when using the eyes; (5) Age factors: As we age, the eye's ability to adjust and secrete tears gradually declines, which can easily lead to visual fatigue. There are currently several ways to relieve eye fatigue: (1) Take regular breaks: Follow the "20-20-20" rule, that is, after looking at the computer screen for 20 minutes, stare at an object 20 feet (about 6 meters) away for at least 20 seconds to relax your eyes; (2) Eye massage: Eye massage can promote blood circulation and relieve tension in the eye muscles; (3) Hot compress: Using a hot compress eye mask or a warm, wet towel on the eyes can relieve eye fatigue and dryness; (4) Artificial tears: Using artificial tears or eye drops can effectively relieve dry eye symptoms and increase eye moisture; (5) Use eye patches: Medical eye patches, as an emerging eye care product, are widely popular because of their convenience, effectiveness and targetedness, and have gradually become a popular choice for relieving eye fatigue and dry eye syndrome.
[0003] Patent CN105363062A discloses a medical hydrogel eye patch. The invention uses carrageenan, konjac gum, calcium chloride, potassium chloride and purified water as raw materials, and obtains the medical hydrogel eye patch by mixing and compounding. The polymer network structure of carrageenan and konjac gum contains a large amount of deionized water. When covered on the eyes, on the one hand, it improves the close fit to the eyes by means of physical cross-linking and chemical cross-linking of calcium ion metal coordination. On the other hand, the polymer network structure contains a large amount of deionized water, which keeps the eyes in a moist environment, which helps to relieve eye discomfort.
[0004] Patent CN113730272A discloses an eye patch with the effect of relieving eye fatigue and its preparation method. The invention mixes moisturizing ingredients, antibacterial ingredients, skin care ingredients and therapeutically active ingredients for relieving visual fatigue to form an eye patch to improve eye problems such as visual fatigue and fatigue of skin cells around the eyes.
[0005] Patent CN117599228A discloses a multifunctional eye dressing patch. The invention stacks a transparent porous permeable layer, an antibacterial drug layer, a first porous permeable layer, an anti-inflammatory drug layer, a second porous permeable layer, an oxygen sustained-release layer and a transparent hydrophobic protective layer in sequence to form an eye dressing patch. It can not only relieve symptoms such as dry eyes and fatigue caused by excessive or unhealthy eye use in daily life, but also achieve the treatment of symptoms such as eye infections and inflammatory reactions through the antibacterial drug layer and the anti-inflammatory drug layer.
[0006] Among the eye patch materials that relieve eye discomfort symptoms such as eye fatigue, dry eyes and soreness, commonly used gelling macromolecular materials such as sodium hyaluronate, sodium alginate, and carrageenan have characteristics such as biocompatibility and will not cause serious irritation to human skin. However, since these macromolecular materials mainly produce gelling properties through hydrogen bond cross-linking and chemical cross-linking, although they improve the adhesion to the skin and make it less likely to fall off naturally, the strong cross-linking also leads to insufficient air permeability of the material. Insufficient air permeability not only affects the feel of use, but also causes adverse phenomena such as itching, redness and swelling of the skin in the eye patch area.
[0007] Therefore, how to improve the air permeability of eye protection dressing is of great significance. Summary of the Invention
[0008] In response to the shortcomings of the prior art, the present invention comprises a thin mucus matrix material obtained by mixing graphene oxide-sodium hyaluronate oxide, graphene oxide-trehalose oxide, glycerol, Tween-80, polyglutamic acid, disodium edetate, calcium chloride, and deionized water, and then filling the mixture into an aluminum-plastic film bag with a non-woven fabric to produce a medical eye protection dressing, thereby resolving the technical problems raised in the background art. Specifically, the technical solution of the present invention includes the following:
[0009] A method for preparing a medical eye-protection dressing, comprising the following steps:
[0010] Mixing graphene oxide-sodium hyaluronate oxide, graphene oxide-trehalose oxide, glycerin, an emulsifier, a moisturizer, a chelating agent, calcium chloride and deionized water to form a thin mucus matrix material;
[0011] The thin mucus matrix material is filled into an aluminum-plastic film bag provided with non-woven fabric and sealed to obtain a medical eye-protecting dressing.
[0012] Furthermore, the preparation method of the graphene oxide-sodium hyaluronate oxide comprises the following steps:
[0013] Sodium hyaluronate and a buffer solution are ultrasonically mixed in a weight ratio of 1:100-150 to form a dispersion, and the dispersion is mixed with sodium periodate and placed in an environment at a temperature of 30±2° C. for oxidation treatment for 3 h to 5 h, followed by dialysis to obtain an oxidized sodium hyaluronate mixture;
[0014] Graphene oxide, an amino crosslinking agent, EDC hydrochloride, and N-hydroxysuccinimide are mixed and dispersed in a weight ratio of 1:10-20:0.5-1:0.5-1, and then stirred and reacted at 25° C.-30° C. for 20 h-22 h to obtain amino-modified graphene oxide;
[0015] The amino-modified graphene oxide and sodium hyaluronate oxide mixture are mixed and dispersed in a weight ratio of 1:50-60, stirred and reacted at 25±2° C. for 20 h to 22 h, and then dried to obtain graphene oxide-sodium hyaluronate oxide.
[0016] Furthermore, the buffer solution comprises an acetate buffer solution with a pH of 6.
[0017] Furthermore, the amino cross-linking agent includes ethylenediamine or 1,3-propylenediamine.
[0018] Furthermore, the preparation method of the graphene oxide-trehalose oxide comprises the following steps:
[0019] After trehalose and deionized water are mixed and dissolved in a weight ratio of 1:10-20, sodium periodate is added and placed in an environment of 30±2°C for oxidation treatment for 4h-6h, followed by dialysis to obtain an oxidized trehalose mixture;
[0020] Graphene oxide, an amino crosslinking agent, EDC hydrochloride, and N-hydroxysuccinimide are mixed and dispersed in a weight ratio of 1:10-20:0.5-1:0.5-1, and then stirred and reacted at 25° C.-30° C. for 20 h-22 h to obtain amino-modified graphene oxide;
[0021] The amino-modified graphene oxide and trehalose oxide mixture are mixed and dispersed in a weight ratio of 1:50-60, stirred and reacted at 25±2° C. for 20 h to 22 h, and then dried to obtain graphene oxide-trehalose oxide.
[0022] Furthermore, the amino cross-linking agent includes ethylenediamine or 1,3-propylenediamine.
[0023] Furthermore, the emulsifier includes Tween-80.
[0024] Furthermore, the moisturizing agent includes γ-polyglutamic acid.
[0025] Furthermore, the chelating agent includes disodium edetate.
[0026] Furthermore, the weight percentages of the graphene oxide-sodium hyaluronate oxide: graphene oxide-trehalose oxide: glycerol: emulsifier: moisturizer: chelating agent: calcium chloride are 0.1% to 0.5%: 1% to 2%: 22% to 25%: 1.6% to 2%: 4% to 7%: 0.1% to 0.2%: 0.008% to 0.01%.
[0027] A medical eye protection dressing prepared by a preparation method of a medical eye protection dressing.
[0028] Compared with the prior art, the present invention has the following beneficial effects:
[0029] The present invention uses sodium hyaluronate, which has strong water absorption, and trehalose, which has high water retention, as the main raw materials. Sodium hyaluronate contains a large number of hydrophilic groups such as carboxyl and hydroxyl groups, which can bind to water molecules through hydrogen bonds, thereby increasing the water content; trehalose has the function of forming a protective film, thereby improving the water retention performance. Sodium hyaluronate and trehalose are first oxidized to obtain functional groups such as aldehyde groups. After oxidation, the adverse effects of poor air permeability of the medical eye dressing obtained by directly mixing the two with other ingredients for gelation can be effectively reduced. The oxidized sodium hyaluronate and oxidized trehalose obtained after oxidation are cross-linked with graphene oxide through amino cross-linking agents, and the graphene oxide is then evenly dispersed on the oxidized sodium hyaluronate and oxidized trehalose to obtain graphene oxide-oxidized sodium hyaluronate and graphene oxide-oxidized trehalose, respectively. Graphene oxide has excellent biosafety and is well-suited for use as a pharmaceutical carrier. Its high specific surface area and pores improve the breathability of eye dressings, reducing adverse reactions such as itching and redness caused by prolonged, airtight dressings. Finally, a thin mucus matrix material obtained by mixing graphene oxide-sodium hyaluronate oxide, graphene oxide-trehalose oxide, glycerol, Tween-80, polyglutamic acid, disodium edetate, calcium chloride, and deionized water is poured into an aluminum-plastic film bag lined with non-woven fabric to produce a medical eye dressing. DETAILED DESCRIPTION
[0030] The following will clearly and completely describe the technical solutions of the present invention through the embodiments of the present invention. Obviously, the embodiments described are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without making any creative efforts shall fall within the scope of protection of the present invention.
[0031] Unless otherwise specified, the raw materials and reagents used in the present invention are commercially available or can be prepared by known methods.
[0032] Preparation Example 1:
[0033] The preparation method of graphene oxide-sodium hyaluronate oxide specifically includes the following steps:
[0034] Weigh 1 part by weight of sodium hyaluronate and add it to 100 parts by weight of acetate buffer with a pH of 6, then place it in an ultrasonic disperser and disperse and mix it at an ultrasonic power of 300W for 15 minutes. After the ultrasonic mixing is completed, take out the dispersion, and then slowly add 0.5 times the weight of sodium hyaluronate sodium periodate to the dispersion and mix and stir, then immediately place it in a dark environment, control the oxidation temperature to 28°C, and time the oxidation treatment for 3 hours. After the oxidation treatment is completed, add 2 times the weight of sodium periodate in ethylene glycol to quench and terminate the oxidation reaction. The reaction solution is then poured into a dialysis bag with a molecular weight cutoff of 3.5kDa, and dialyzed with deionized water to remove small molecular impurities such as sodium periodate and ethylene glycol to obtain an oxidized sodium hyaluronate mixture;
[0035] 1 part by weight of graphene oxide was added to anhydrous acetone and dispersed and mixed at an ultrasonic power of 300W for 15 minutes. Then 0.5 parts by weight of EDC hydrochloride and 0.5 parts by weight of N-hydroxysuccinimide were added and stirred for pre-activation for 1 hour. After the pre-activation, 10 parts by weight of ethylenediamine crosslinker was added to the activated mixture and the temperature was controlled to 25°C. Then, the mixture was stirred at a stirring speed of 200r / min for 20 hours. After the reaction was completed, the solid particles were collected by filtration, rinsed with ethyl acetate, ethanol and deionized water in sequence, and placed in a vacuum drying oven to dry to constant weight to obtain amino-modified graphene oxide;
[0036] Weigh 1 part by weight of amino-modified graphene oxide and 50 parts by weight of sodium hyaluronate oxide, mix and stir until uniformly dispersed. Then, stir at 200 rpm and 25 ± 2°C for 20 hours. After the reaction, filter and dry the mixture to obtain graphene oxide-sodium hyaluronate oxide.
[0037] Preparation Example 2:
[0038] The preparation method of graphene oxide-sodium hyaluronate oxide specifically includes the following steps:
[0039] Weigh 1 part by weight of sodium hyaluronate and add it to 120 parts by weight of acetate buffer with a pH of 6, then place it in an ultrasonic disperser and disperse and mix it at an ultrasonic power of 300W for 15 minutes. After the ultrasonic mixing is completed, take out the dispersion, and then slowly add 0.7 times the weight of sodium hyaluronate sodium periodate to the dispersion and mix and stir, then immediately place it in a dark environment, control the oxidation temperature to 30°C, and time the oxidation treatment for 3 hours. After the oxidation treatment is completed, add 2 times the weight of sodium periodate in ethylene glycol to quench and terminate the oxidation reaction. The reaction solution is then poured into a dialysis bag with a molecular weight cutoff of 3.5kDa, and dialyzed with deionized water to remove small molecular impurities such as sodium periodate and ethylene glycol to obtain an oxidized sodium hyaluronate mixture;
[0040] 1 part by weight of graphene oxide was added to anhydrous acetone and dispersed and mixed at an ultrasonic power of 300W for 15 minutes. Then 0.7 parts by weight of EDC hydrochloride and 0.7 parts by weight of N-hydroxysuccinimide were added and stirred for pre-activation for 1 hour. After the pre-activation, 14 parts by weight of ethylenediamine crosslinker was added to the activated mixture and the temperature was controlled to 25°C. Then, the mixture was stirred at a stirring speed of 200r / min for 20 hours. After the reaction was completed, the solid particles were collected by filtration, rinsed with ethyl acetate, ethanol and deionized water in sequence, and placed in a vacuum drying oven to dry to constant weight to obtain amino-modified graphene oxide;
[0041] Weigh 1 part by weight of amino-modified graphene oxide and 54 parts by weight of sodium hyaluronate oxide, mix and stir until uniformly dispersed. Then, stir at 200 rpm and maintain a temperature of 25 ± 2°C for 21 hours. After the reaction, filter and dry the mixture to obtain graphene oxide-sodium hyaluronate oxide.
[0042] Preparation Example 3:
[0043] The preparation method of graphene oxide-sodium hyaluronate oxide specifically includes the following steps:
[0044] Weigh 1 part by weight of sodium hyaluronate and add it to 140 parts by weight of acetate buffer with a pH of 6, then place it in an ultrasonic disperser and disperse and mix it at an ultrasonic power of 400W for 15 minutes. After the ultrasonic mixing is completed, take out the dispersion, and then slowly add 0.9 times the weight of sodium hyaluronate sodium periodate to the dispersion and mix and stir, then immediately place it in a dark environment, control the oxidation temperature to 30°C, and time the oxidation treatment for 4 hours. After the oxidation treatment is completed, add 2 times the weight of sodium periodate in ethylene glycol to quench and terminate the oxidation reaction. The reaction solution is then poured into a dialysis bag with a molecular weight cutoff of 3.5kDa, and dialyzed with deionized water to remove small molecular impurities such as sodium periodate and ethylene glycol to obtain an oxidized sodium hyaluronate mixture;
[0045] 1 part by weight of graphene oxide was added to anhydrous acetone and dispersed and mixed at an ultrasonic power of 400W for 15 minutes. Then 0.9 parts by weight of EDC hydrochloride and 0.9 parts by weight of N-hydroxysuccinimide were added and stirred for pre-activation for 1 hour. After the pre-activation, 18 parts by weight of 1,3-propylenediamine crosslinker was added to the activated mixture and the temperature was controlled to 30°C. Then, the mixture was stirred at a stirring speed of 300r / min for 21 hours. After the reaction was completed, the solid particles were collected by filtration, rinsed with ethyl acetate, ethanol and deionized water in sequence, and placed in a vacuum drying oven to dry to constant weight to obtain amino-modified graphene oxide;
[0046] Weigh 1 part by weight of amino-modified graphene oxide and 58 parts by weight of sodium hyaluronate oxide, mix and stir until uniformly dispersed. Then, stir at 300 rpm and a temperature of 25 ± 2°C for 21 hours. After the reaction, filter and dry the mixture to obtain graphene oxide-sodium hyaluronate oxide.
[0047] Preparation Example 4:
[0048] The preparation method of graphene oxide-sodium hyaluronate oxide specifically includes the following steps:
[0049] Weigh 1 part by weight of sodium hyaluronate and add it to 150 parts by weight of acetate buffer with a pH of 6, then place it in an ultrasonic disperser and disperse and mix it at an ultrasonic power of 400W for 15 minutes. After the ultrasonic mixing is completed, take out the dispersion, and then slowly add 1 times the weight of sodium hyaluronate sodium periodate to the dispersion and mix and stir, then immediately place it in a dark environment, control the oxidation temperature to 32°C, and time the oxidation treatment for 5 hours. After the oxidation treatment is completed, add 2 times the weight of sodium periodate in ethylene glycol to quench and terminate the oxidation reaction. The reaction solution is then poured into a dialysis bag with a molecular weight cutoff of 3.5kDa, and dialyzed with deionized water to remove small molecular impurities such as sodium periodate and ethylene glycol to obtain an oxidized sodium hyaluronate mixture;
[0050] 1 part by weight of graphene oxide was added to anhydrous acetone and dispersed and mixed at an ultrasonic power of 400W for 15 minutes. Then 1 part by weight of EDC hydrochloride and 1 part by weight of N-hydroxysuccinimide were added and stirred for pre-activation for 1 hour. After the pre-activation, 20 parts by weight of 1,3-propylenediamine crosslinker was added to the activated mixture and the temperature was controlled to 30°C. Then, the mixture was stirred at a stirring speed of 300r / min for 22 hours. After the reaction was completed, the solid particles were collected by filtration, rinsed with ethyl acetate, ethanol and deionized water in sequence, and placed in a vacuum drying oven to dry to constant weight to obtain amino-modified graphene oxide;
[0051] Weigh 1 part by weight of amino-modified graphene oxide and 60 parts by weight of sodium hyaluronate oxide, mix and stir until uniformly dispersed. Then, stir at 300 rpm and a temperature of 25 ± 2°C for 22 hours. After the reaction, filter and dry the mixture to obtain graphene oxide-sodium hyaluronate oxide.
[0052] Preparation Example 5:
[0053] The preparation method of graphene oxide-sodium hyaluronate oxide specifically includes the following steps:
[0054] Weigh 1 part by weight of sodium hyaluronate and add it to 150 parts by weight of acetate buffer with a pH of 6, then place it in an ultrasonic disperser and disperse and mix it at an ultrasonic power of 400W for 15 minutes. After the ultrasonic mixing is completed, take out the dispersion, and then slowly add 1 times the weight of sodium hyaluronate sodium periodate to the dispersion and mix and stir, then immediately place it in a dark environment, control the oxidation temperature to 35°C, and time the oxidation treatment for 7 hours. After the oxidation treatment is completed, add 2 times the weight of sodium periodate in ethylene glycol to quench and terminate the oxidation reaction. The reaction solution is then poured into a dialysis bag with a molecular weight cutoff of 3.5kDa, and dialyzed with deionized water to remove small molecular impurities such as sodium periodate and ethylene glycol to obtain an oxidized sodium hyaluronate mixture;
[0055] The rest of the process was the same as that in Preparation Example 4.
[0056] Preparation Example 6:
[0057] The preparation method of graphene oxide-sodium hyaluronate oxide specifically includes the following steps:
[0058] The 1,3-propylenediamine cross-linking agent in Preparation Example 4 was replaced with 1,2-propylenediamine cross-linking agent, and the rest of the process remained the same as Preparation Example 4.
[0059] Preparation Example 7:
[0060] The preparation method of graphene oxide-trehalose oxide specifically includes the following steps:
[0061] Weigh 1 part by weight of trehalose and add it to 10 parts by weight of deionized water, and stir at a speed of 400r / min until it is completely dissolved. Then slowly add 0.5 times the weight of trehalose sodium periodate to the trehalose solution and mix and stir, then immediately place it in a dark environment, control the oxidation temperature to 28°C, and time the oxidation treatment for 4 hours. After the oxidation treatment is completed, add 2 times the weight of sodium periodate in ethylene glycol to quench and terminate the oxidation reaction. Then pour the reaction solution into a dialysis bag with a molecular weight cutoff of 3.5kDa, and dialyze with deionized water to remove small molecular impurities such as sodium periodate and ethylene glycol to obtain an oxidized trehalose mixture;
[0062] 1 part by weight of graphene oxide was added to anhydrous acetone and dispersed and mixed at an ultrasonic power of 300W for 15 minutes. Then 0.5 parts by weight of EDC hydrochloride and 0.5 parts by weight of N-hydroxysuccinimide were added and stirred for pre-activation for 1 hour. After the pre-activation, 10 parts by weight of ethylenediamine crosslinker was added to the activated mixture and the temperature was controlled to 25°C. Then, the mixture was stirred at a stirring speed of 200r / min for 20 hours. After the reaction was completed, the solid particles were collected by filtration, rinsed with ethyl acetate, ethanol and deionized water in sequence, and placed in a vacuum drying oven to dry to constant weight to obtain amino-modified graphene oxide;
[0063] Weigh 1 part by weight of amino-modified graphene oxide and 50 parts by weight of trehalose oxide, mix and stir until uniformly dispersed. Then, stir at 200 r / min and maintain a temperature of 25 ± 2°C for 20 hours. After the reaction, filter and dry the mixture to obtain graphene oxide-trehalose oxide.
[0064] Preparation Example 8:
[0065] The preparation method of graphene oxide-trehalose oxide specifically includes the following steps:
[0066] Weigh 1 part by weight of trehalose and add it to 14 parts by weight of deionized water, and stir at a speed of 400r / min until it is completely dissolved. Then slowly add 0.7 times the weight of trehalose sodium periodate to the trehalose solution and mix and stir, then immediately place it in a dark environment, control the oxidation temperature to 30°C, and time the oxidation treatment for 4 hours. After the oxidation treatment is completed, add 2 times the weight of sodium periodate in ethylene glycol to quench and terminate the oxidation reaction. Then pour the reaction solution into a dialysis bag with a molecular weight cutoff of 3.5kDa, and dialyze with deionized water to remove small molecular impurities such as sodium periodate and ethylene glycol to obtain an oxidized trehalose mixture;
[0067] 1 part by weight of graphene oxide was added to anhydrous acetone and dispersed and mixed at an ultrasonic power of 300W for 15 minutes. Then 0.7 parts by weight of EDC hydrochloride and 0.7 parts by weight of N-hydroxysuccinimide were added and stirred for pre-activation for 1 hour. After the pre-activation, 14 parts by weight of ethylenediamine crosslinker was added to the activated mixture and the temperature was controlled to 25°C. Then, the mixture was stirred at a stirring speed of 200r / min for 20 hours. After the reaction was completed, the solid particles were collected by filtration, rinsed with ethyl acetate, ethanol and deionized water in sequence, and placed in a vacuum drying oven to dry to constant weight to obtain amino-modified graphene oxide;
[0068] Weigh 1 part by weight of amino-modified graphene oxide and 54 parts by weight of trehalose oxide, mix and stir until uniformly dispersed. Then, stir at 200 r / min and maintain a temperature of 25 ± 2°C for 21 hours. After the reaction, filter and dry the mixture to obtain graphene oxide-trehalose oxide.
[0069] Preparation Example 9:
[0070] The preparation method of graphene oxide-trehalose oxide specifically includes the following steps:
[0071] Weigh 1 part by weight of trehalose and add it to 18 parts by weight of deionized water, and stir at a speed of 400r / min until it is completely dissolved. Then slowly add 0.9 times the weight of trehalose sodium periodate to the trehalose solution and mix and stir, then immediately place it in a dark environment, control the oxidation temperature to 30°C, and time the oxidation treatment for 5 hours. After the oxidation treatment is completed, add 2 times the weight of sodium periodate in ethylene glycol to quench and terminate the oxidation reaction. Then pour the reaction solution into a dialysis bag with a molecular weight cutoff of 3.5kDa, and dialyze with deionized water to remove small molecular impurities such as sodium periodate and ethylene glycol to obtain an oxidized trehalose mixture;
[0072] 1 part by weight of graphene oxide was added to anhydrous acetone and dispersed and mixed at an ultrasonic power of 400W for 15 minutes. Then 0.9 parts by weight of EDC hydrochloride and 0.9 parts by weight of N-hydroxysuccinimide were added and stirred for pre-activation for 1 hour. After the pre-activation, 18 parts by weight of 1,3-propylenediamine crosslinker was added to the activated mixture and the temperature was controlled to 30°C. Then, the mixture was stirred at a stirring speed of 300r / min for 21 hours. After the reaction was completed, the solid particles were collected by filtration, rinsed with ethyl acetate, ethanol and deionized water in sequence, and placed in a vacuum drying oven to dry to constant weight to obtain amino-modified graphene oxide;
[0073] Weigh 1 part by weight of amino-modified graphene oxide and 58 parts by weight of trehalose oxide, mix and stir until uniformly dispersed. Then, stir at 200 r / min and maintain a temperature of 25 ± 2°C for 21 hours. After the reaction, filter and dry the mixture to obtain graphene oxide-trehalose oxide.
[0074] Preparation Example 10:
[0075] The preparation method of graphene oxide-trehalose oxide specifically includes the following steps:
[0076] Weigh 1 part by weight of trehalose and add it to 20 parts by weight of deionized water, and stir at a speed of 400r / min until it is completely dissolved. Then slowly add 1 times the weight of trehalose sodium periodate to the trehalose solution and mix and stir, then immediately place it in a dark environment, control the oxidation temperature to 32°C, and time the oxidation treatment for 6 hours. After the oxidation treatment is completed, add 2 times the weight of sodium periodate in ethylene glycol to quench and terminate the oxidation reaction. Then pour the reaction solution into a dialysis bag with a molecular weight cutoff of 3.5kDa, and dialyze with deionized water to remove small molecular impurities such as sodium periodate and ethylene glycol to obtain an oxidized trehalose mixture;
[0077] 1 part by weight of graphene oxide was added to anhydrous acetone and dispersed and mixed at an ultrasonic power of 400W for 15 minutes. Then 1 part by weight of EDC hydrochloride and 1 part by weight of N-hydroxysuccinimide were added and stirred for pre-activation for 1 hour. After the pre-activation, 20 parts by weight of 1,3-propylenediamine crosslinker was added to the activated mixture and the temperature was controlled to 30°C. Then, the mixture was stirred at a stirring speed of 300r / min for 22 hours. After the reaction was completed, the solid particles were collected by filtration, rinsed with ethyl acetate, ethanol and deionized water in sequence, and placed in a vacuum drying oven to dry to constant weight to obtain amino-modified graphene oxide;
[0078] Weigh 1 part by weight of amino-modified graphene oxide and 60 parts by weight of trehalose oxide, mix and stir until uniformly dispersed. Then, stir at 200 r / min and maintain a temperature of 25 ± 2°C for 22 hours. After the reaction, filter and dry the mixture to obtain graphene oxide-trehalose oxide.
[0079] Preparation Example 11:
[0080] The preparation method of graphene oxide-trehalose oxide specifically includes the following steps:
[0081] Weigh 1 part by weight of trehalose and add it to 20 parts by weight of deionized water, and stir at a speed of 400r / min until it is completely dissolved. Then slowly add 1 times the weight of trehalose sodium periodate to the trehalose solution and mix and stir, then immediately place it in a dark environment, control the oxidation temperature to 35°C, and time the oxidation treatment for 7 hours. After the oxidation treatment is completed, add 2 times the weight of sodium periodate in ethylene glycol to quench and terminate the oxidation reaction. Then pour the reaction solution into a dialysis bag with a molecular weight cutoff of 3.5kDa, and dialyze with deionized water to remove small molecular impurities such as sodium periodate and ethylene glycol to obtain an oxidized trehalose mixture;
[0082] The rest of the process was the same as in Preparation Example 10.
[0083] Preparation Example 12:
[0084] The preparation method of graphene oxide-trehalose oxide specifically includes the following steps:
[0085] The 1,3-propylenediamine cross-linking agent in Preparation Example 10 was replaced with 1,2-propylenediamine cross-linking agent, and the rest of the process remained the same as Preparation Example 10.
[0086] Example 1:
[0087] A method for preparing a medical eye protection dressing specifically comprises the following steps:
[0088] According to weight percentage, 0.1% of the graphene oxide-sodium hyaluronate oxide obtained in Preparation Example 1, 1% of the graphene oxide-trehalose oxide obtained in Preparation Example 7, and 50% deionized water were mixed, heated to 55°C, and stirred until uniformly dispersed. Subsequently, 22% glycerol, 1.6% Tween-80, 4% γ-polyglutamic acid, 0.1% disodium edetate, and 0.008% calcium chloride powder were added and continued to mix and stir for 10 minutes. Deionized water was then added to bring the volume to 100%, and the mixture was finally defoamed in a vacuum drying oven and cooled to room temperature to form a thin mucus matrix material.
[0089] In a room temperature environment, the dilute mucus matrix material is filled into an aluminum-plastic film bag provided with non-woven fabric, and then sealed to complete the preparation of the medical eye dressing.
[0090] Example 2:
[0091] A method for preparing a medical eye protection dressing specifically comprises the following steps:
[0092] According to weight percentage, 0.2% of the graphene oxide-sodium hyaluronate oxide obtained in Preparation Example 2, 1.4% of the graphene oxide-trehalose oxide obtained in Preparation Example 8, and 50% deionized water were mixed, heated to 55°C, and stirred until uniformly dispersed. Subsequently, 23% glycerol, 1.7% Tween-80, 5% γ-polyglutamic acid, 0.1% disodium edetate, and 0.009% calcium chloride powder were added and continued to mix and stir for 10 minutes. Deionized water was then added to bring the total to 100%. Finally, the mixture was defoamed in a vacuum drying oven and cooled to room temperature to form a thin mucus matrix material.
[0093] In a room temperature environment, the dilute mucus matrix material is filled into an aluminum-plastic film bag provided with non-woven fabric, and then sealed to complete the preparation of the medical eye dressing.
[0094] Example 3:
[0095] A method for preparing a medical eye protection dressing specifically comprises the following steps:
[0096] According to weight percentage, 0.4% of the graphene oxide-sodium hyaluronate oxide obtained in Preparation Example 3, 1.8% of the graphene oxide-trehalose oxide obtained in Preparation Example 9, and 50% deionized water were mixed, heated to 55°C, and stirred until uniformly dispersed. Subsequently, 24% glycerol, 1.9% Tween-80, 6% γ-polyglutamic acid, 0.2% disodium edetate, and 0.01% calcium chloride powder were added and continued to mix and stir for 10 minutes. Deionized water was then added to bring the volume to 100%, and the mixture was finally defoamed in a vacuum drying oven and cooled to room temperature to form a thin mucus matrix material.
[0097] In a room temperature environment, the dilute mucus matrix material is filled into an aluminum-plastic film bag provided with non-woven fabric, and then sealed to complete the preparation of the medical eye dressing.
[0098] Example 4:
[0099] A method for preparing a medical eye protection dressing specifically comprises the following steps:
[0100] According to weight percentage, 0.5% of the graphene oxide-sodium hyaluronate oxide obtained in Preparation Example 4, 2% of the graphene oxide-trehalose oxide obtained in Preparation Example 10, and 50% deionized water were mixed, heated to 55°C, and stirred until uniformly dispersed. Subsequently, 25% glycerol, 2% Tween-80, 7% γ-polyglutamic acid, 0.2% disodium edetate, and 0.01% calcium chloride powder were added and continued to mix and stir for 10 minutes. Deionized water was then added to bring the volume to 100%, and the mixture was finally defoamed in a vacuum drying oven and cooled to room temperature to form a thin mucus matrix material.
[0101] In a room temperature environment, the dilute mucus matrix material is filled into an aluminum-plastic film bag provided with non-woven fabric, and then sealed to complete the preparation of the medical eye dressing.
[0102] Comparative Example 1:
[0103] A method for preparing a medical eye protection dressing specifically comprises the following steps:
[0104] According to weight percentage, 0.5% of the graphene oxide-sodium hyaluronate oxide obtained in Preparation Example 5, 2% of the graphene oxide-trehalose oxide obtained in Preparation Example 11, and 50% deionized water were mixed, heated to 55°C, and stirred until uniformly dispersed. Subsequently, 25% glycerol, 2% Tween-80, 7% γ-polyglutamic acid, 0.2% disodium edetate, and 0.01% calcium chloride powder were added and continued to mix and stir for 10 minutes. Deionized water was then added to bring the volume to 100%, and the mixture was finally defoamed in a vacuum drying oven and cooled to room temperature to form a thin mucus matrix material.
[0105] In a room temperature environment, the dilute mucus matrix material is filled into an aluminum-plastic film bag provided with non-woven fabric, and then sealed to complete the preparation of the medical eye dressing.
[0106] Comparative Example 2:
[0107] A method for preparing a medical eye protection dressing specifically comprises the following steps:
[0108] According to weight percentage, 0.5% of the graphene oxide-sodium hyaluronate oxide obtained in Preparation Example 6, 2% of the graphene oxide-trehalose oxide obtained in Preparation Example 12, and 50% deionized water were mixed, heated to 55°C, and stirred until uniformly dispersed. Subsequently, 25% glycerol, 2% Tween-80, 7% γ-polyglutamic acid, 0.2% disodium edetate, and 0.01% calcium chloride powder were added and continued to mix and stir for 10 minutes. Deionized water was then added to bring the volume to 100%, and the mixture was finally defoamed in a vacuum drying oven and cooled to room temperature to form a thin mucus matrix material.
[0109] In a room temperature environment, the dilute mucus matrix material is filled into an aluminum-plastic film bag provided with non-woven fabric, and then sealed to complete the preparation of the medical eye dressing.
[0110] Comparative Example 3:
[0111] A method for preparing a medical eye protection dressing specifically comprises the following steps:
[0112] Mix 0.5% sodium hyaluronate, 2% trehalose, and 50% deionized water, heating to 55°C and stirring until uniformly dispersed. Then, add 25% glycerol, 2% Tween-80, 7% γ-polyglutamic acid, 0.2% disodium edetate, and 0.01% calcium chloride powder, and continue stirring for 10 minutes. Deionized water is then added to bring the volume to 100%. Finally, the mixture is degassed in a vacuum drying oven and cooled to room temperature to form a thin mucus matrix material.
[0113] In a room temperature environment, the dilute mucus matrix material is filled into an aluminum-plastic film bag provided with non-woven fabric, and then sealed to complete the preparation of the medical eye dressing.
[0114] Comparative Example 4:
[0115] A method for preparing a medical eye protection dressing specifically comprises the following steps:
[0116] According to weight percentage, 0.5% of the graphene oxide-sodium hyaluronate oxide obtained in Preparation Example 4, 2% of the graphene oxide-trehalose oxide obtained in Preparation Example 10, and 50% deionized water were mixed, heated to 55°C, and stirred until uniformly dispersed. Subsequently, 25% glycerol, 2% Tween-80, 0.2% disodium edetate, and 0.01% calcium chloride powder were added and continued to mix and stir for 10 minutes. Deionized water was then added to bring the volume to 100%, and the mixture was finally defoamed in a vacuum drying oven and cooled to room temperature to form a thin mucus matrix material.
[0117] In a room temperature environment, the dilute mucus matrix material is filled into an aluminum-plastic film bag provided with non-woven fabric, and then sealed to complete the preparation of the medical eye dressing.
[0118] (1) Adhesion performance verification
[0119] After removing the anti-stick protective layer from the medical eye protection dressings prepared in Examples 1 to 4 and Comparative Examples 1 to 4, the dressings were adhered to the surface of fresh pigskin, respectively. Then, a tensile adhesion test was performed using a universal testing machine at 25±2°C. The adhesion strength when the medical eye protection dressing was completely detached was used as the final adhesion strength value. The results are shown in Table 1 below.
[0120] Table 1 Adhesion properties
[0121] Sources Adhesion strength (kPa) Example 1 42.80 Example 2 49.53 Example 3 56.07 Example 4 58.23 Comparative Example 1 4.58 Comparative Example 2 110.41 Comparative Example 3 55.14 Comparative Example 4 5.91
[0122] (2) Air permeability test:
[0123] The anti-adhesive protective layer of the medical eye protection dressings prepared in Examples 1 to 4 and Comparative Examples 1 to 4 was removed, and the air permeability was tested using a fully automatic air permeability meter according to ASTM D 737. The test area was 20 cm 2 , the test pressure is 100Pa, and the results are shown in Table 2 below.
[0124] Table 2 Air permeability
[0125] Sources Air permeability (mm / s) Example 1 5.1 Example 2 5.8 Example 3 6.3 Example 4 6.6 Comparative Example 1 6.2 Comparative Example 2 0.8 Comparative Example 3 1.1 Comparative Example 4 6.4
[0126] (3) Skin irritation test:
[0127] The anti-sticking protective layers of the medical eye dressings prepared in Examples 1 to 4 and Comparative Examples 1 to 4 were torn off and applied to the upper and lower eyelids of experimental mice. After 1 hour, the shedding of the medical eye dressings, the ease of removal, and the redness and swelling of the eyelids after removal of the medical eye dressings were observed. The results are shown in Table 3 below.
[0128] Table 3 Irritation test
[0129]
[0130]
[0131] The following conclusions can be drawn from the test results in Tables 1 to 3 above:
[0132] (1) Through Examples 1 to 4, it can be found that the medical eye protection dressing prepared by mixing the graphene oxide-sodium hyaluronate oxide and graphene oxide-trehalose oxide constructed by the present invention with other additives and then filling them into an aluminum-plastic film bag configured with non-woven fabric has low skin irritation and good adhesion and breathability.
[0133] (2) It can be found from Comparative Example 1 that the prepared medical eye protection dressing has good air permeability during the performance test, but has low adhesion strength. This may be because in this system, further increasing the degree of oxidation of sodium hyaluronate and trehalose may lead to the breakage of glycosidic bonds, and the aldehyde groups produced by oxidation may compete with the original carboxyl and hydroxyl groups to bind to water molecules, weakening the stability of the hydrogen bond network, and thus resulting in poor adhesion of the finally prepared medical eye protection dressing to the skin, which is not conducive to use.
[0134] (3) It can be found from Comparative Example 2 that the prepared medical eye protection dressing has high adhesion strength and poor air permeability during performance testing. This may be because in this system, the two amino groups of the 1,2-propylenediamine crosslinker are located on adjacent carbon atoms of propane, the molecular structure is compact, and the steric hindrance is small. This proximity enhances the synergistic effect of the amino groups, making it easier for the amino groups to undergo multi-point cross-linking reactions with the target functional groups to form a denser three-dimensional network structure. However, the highly dense three-dimensional network structure is not conducive to the air permeability of the material. As a result, the medical eye protection dressing finally prepared not only has poor air permeability, but also the improvement of adhesion performance will cause pain and other irritation to the skin when removing the medical eye protection dressing, which is not conducive to use.
[0135] (4) Comparative Example 3 shows that although the prepared medical eye protection dressing has good adhesion performance, it has poor air permeability and is prone to causing adverse reactions such as redness and swelling on the skin during use. This may be because the cross-linked network structure formed by sodium hyaluronate and trehalose through their own hydrogen bond cross-linking and chemical cross-linking is too dense, which makes it difficult to achieve good air permeability under the formulation of this system, making it unfavorable for use.
[0136] (5) Comparative Example 4 shows that the medical eye protection dressing prepared without adding the moisturizing agent γ-polyglutamic acid has good air permeability but low adhesion strength during performance testing. This may be because in this system, after hyaluronic acid and trehalose are oxidized, their own structures are damaged by oxidation, resulting in low adhesion performance. Although glycerol has a certain moisturizing effect, the hydroxyl groups in the glycerol structure have poor coordination and cross-linking effects on metal ions and calcium ions compared to functional groups such as carboxyl and amino groups on γ-polyglutamic acid, which leads to poor adhesion strength.
[0137] The embodiments described above provide a detailed description of the technical solutions and beneficial effects of the present invention. It should be understood that the above descriptions are merely specific embodiments of the present invention and are not intended to limit the present invention. Various changes and modifications may be made to the present invention without departing from the spirit and scope of the present invention, and such changes and modifications fall within the scope of the present invention as claimed.
Claims
1. A method for preparing a medical eye-protecting dressing, characterized in that: The preparation method comprises the following steps: Mixing graphene oxide-sodium hyaluronate oxide, graphene oxide-trehalose oxide, glycerin, an emulsifier, a moisturizer, a chelating agent, calcium chloride and deionized water to form a thin mucus matrix material; The thin mucus matrix material is filled into an aluminum-plastic film bag provided with non-woven fabric and sealed to obtain a medical eye-protecting dressing.
2. The method for preparing a medical eye protection dressing according to claim 1, characterized in that: The preparation method of the graphene oxide-sodium hyaluronate oxide comprises the following steps: Sodium hyaluronate and a buffer solution are ultrasonically mixed in a weight ratio of 1:100-150 to form a dispersion, and the dispersion is mixed with sodium periodate and placed in an environment at a temperature of 30±2° C. for oxidation treatment for 3 h to 5 h, followed by dialysis to obtain an oxidized sodium hyaluronate mixture; Graphene oxide, an amino crosslinking agent, EDC hydrochloride, and N-hydroxysuccinimide are mixed and dispersed in a weight ratio of 1:10-20:0.5-1:0.5-1, and then stirred and reacted at 25° C.-30° C. for 20 h-22 h to obtain amino-modified graphene oxide; The amino-modified graphene oxide and sodium hyaluronate oxide mixture are mixed and dispersed in a weight ratio of 1:50-60, stirred and reacted at 25±2° C. for 20 h to 22 h, and then dried to obtain graphene oxide-sodium hyaluronate oxide.
3. The method for preparing a medical eye-protecting dressing according to claim 2, characterized in that: The amino cross-linking agent includes ethylenediamine or 1,3-propylenediamine.
4. The method for preparing a medical eye-protecting dressing according to claim 1, characterized in that: The preparation method of the graphene oxide-trehalose oxide comprises the following steps: After trehalose and deionized water are mixed and dissolved in a weight ratio of 1:10-20, sodium periodate is added and placed in an environment of 30±2°C for oxidation treatment for 4h-6h, followed by dialysis to obtain an oxidized trehalose mixture; Graphene oxide, an amino crosslinking agent, EDC hydrochloride, and N-hydroxysuccinimide are mixed and dispersed in a weight ratio of 1:10-20:0.5-1:0.5-1, and then stirred and reacted at 25° C.-30° C. for 20 h-22 h to obtain amino-modified graphene oxide; The amino-modified graphene oxide and trehalose oxide mixture are mixed and dispersed in a weight ratio of 1:50-60, stirred and reacted at 25±2° C. for 20 h to 22 h, and then dried to obtain graphene oxide-trehalose oxide.
5. The method for preparing a medical eye-protecting dressing according to claim 4, characterized in that: The amino cross-linking agent includes ethylenediamine or 1,3-propylenediamine.
6. The method for preparing a medical eye-protecting dressing according to claim 1, characterized in that: The weight percentages of the graphene oxide-sodium hyaluronate oxide: graphene oxide-trehalose oxide: glycerol: emulsifier: moisturizer: chelating agent: calcium chloride are 0.1% to 0.5%: 1% to 2%: 22% to 25%: 1.6% to 2%: 4% to 7%: 0.1% to 0.2%: 0.008% to 0.01%.
7. A medical eye protection dressing, characterized in that: The medical eye protection dressing is prepared by the preparation method of a medical eye protection dressing according to any one of claims 1 to 7.
Citation Information
Patent Citations
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KR102660445B1
Biodegradable graphene oxide biocomposite fibrous membrane, preparation method and uses thereof
US20200330641A1
