KR20020034481A - Charcoal filled hydrogels dressings and process for preparing thereof by irradiation - Google Patents

Abstract

PURPOSE: Provided is a hydrated gel dressing with charcoal filled which freezes and thaws or exposes hydrated gel dressing to radiation with charcoal added to synthetic polymer so that it lowers viscosity and controls swelling, gel strength and gelation easily. CONSTITUTION: In the hydrated gel dressing with charcoal filled which is prepared by containing 2-40wt% of charcoal on a basis of 100wt% of synthetic polymer wherein 10-90wt% of polyvinyl alcohol and 10-90wt% of polyvinyl pyrrolidone, the production process of the hydrated gel dressing with charcoal filled comprises the steps of: (i) freezing and thawing aqueous polymer solution in a mold and shaping firstly-gelated hydrated gel in a sheet form; and (ii) exposing the firstly-gelated hydrated gel to radiation to perform second gelation.

Description

Charcoal filled hydrogels dressings and process for preparing coconut by irradiation}

The present invention relates to a hydrogel dressing, specifically, a charcoal-filled hydrogel dressing composed of polyvinyl alcohol, polyvinylpyrrolidone and charcoal and a polymer aqueous solution are lyophilized to form a sheet, and then irradiated with radiation to prepare a hydrogel dressing. It relates to a charcoal-filled hydrogel dressing and its preparation method using radiation.

Severe burn treatment ultimately results in the transplantation of fibroblast tissue from a patient that has been autografted or cultured in vitro. Usually, considerable time is required to perform such a procedure, and thus, a burn dressing is used to prevent infection within a short time until the procedure, and the burn dressing must meet the following conditions. It must be able to absorb fluids well, to prevent infection from bacteria, and to be easily attached to wounds or skin. In addition, transparency and oxygen permeability should be good, drug control should be possible, handling should be easy, storage and sterilization should be possible.

Hydrogels have been proposed as the most promising ones which can satisfy the above conditions. It is known that hydrogel has more than 90% water content, so that it is used temporarily for the purpose of skin regeneration which requires burn treatment or wet condition continuously. It has affinity with blood, body fluids and biological tissues and is used in wound dressing, contact lenses and cartilage.

The hydrogel has a three-dimensional network and can function at several tens of times its own weight. Generally, hydrogels are synthetic polymers such as polyvinylpyrrolidone, polyethylene oxide, polyhydroxyethyl methacrylate, polyvinyl alcohol, gelatin, agar, alginate, collagen, and recently gaining popularity. It is produced by a combination of natural polymers such as chitosan and synthetic polymers and natural polymers. Hydrogels containing hydrophilic functional groups such as carboxyl groups (-COOH), amino groups (-CONH ₂ ), and sulfonic acid groups (-SO ₃ H) in the polymer mainly function by hydrogen bonding, capillary and osmotic pressure when they come into contact with moisture. It forms a covalent structure between the polymer chains, with some electrostatic and lipophilic interactions, and keeps swelling without dissolving in water. As a result, the polymer hydrogel can absorb moisture and retain the mechanical properties and shape of the polymer.

Hydrogels are prepared by chemical methods, by irradiation and by lyolysis.

The chemical method is a conventional method of cross-linking reactions having a three-dimensional network structure using a cross-linking agent and initiator such as formaldehyde and glutaaldehyde in the polymer can be easily induced cross-linking reaction, but the toxicity after cross-linking reaction There is a disadvantage in that the chemical crosslinking agent and initiator present must be removed as it remains.

The method using radiation is a method of irradiating a polymer with radiation to crosslink it, and there is no need to remove residual crosslinking agent or initiator after crosslinking as compared with chemical method, and it is capable of both sterilization and crosslinking at the same time. In addition, there is no need to apply heat in the cross-linking process, it is possible to cross-link even in a cooled state, and there is a feature that can freely adjust the physical properties by controlling the radiation dose without changing the composition.

Freezing and thawing mainly freezes polymers containing hydroxyl groups such as polyvinyl alcohol at low temperature and then thaws at room temperature to induce physical crosslinking reaction. Since the freezing and thawing method does not use a crosslinking agent and an initiator, there is no need to worry about the toxicity of the crosslinking agent and the initiator remaining after the crosslinking reaction, but there is a difficulty in using the physical crosslinking as time passes.

Recently, researches are being made on the application of medical hydrogels to medical treatments including wound dressings by preparing polymer hydrogels by irradiation.

Attempts have been made to use polyvinylpyrrolidone, which is nontoxic and has excellent physical properties, as a dressing for wound healing. According to the publication published by Yoshii et al. (Radiation Physics and Chemistry, 55, 1999, 133-138), animal studies on rats showed that polyvinylpyrrolidone hydrogels had low strength and higher adhesion than needed to treat wounds. It has been described that there is a problem that some of the polyvinylpyrrolidone remains in the wound when the polyvinylpyrrolidone hydrogel dressing is removed from the wound. However, even if the strength of the material is high, there is a possibility that the material may stick to the wound by the chemical interaction between the material and the protein.

US Patent No. 4,871,490 describes a technique for preparing a wound dressing using a radiation crosslinking method without using a chemical crosslinking agent. Polyvinylpyrrolidone hydrogel was prepared by mixing agar and polyethylene oxide with polyvinylpyrrolidone and irradiating it with radiation to crosslink it. U.S. Patent No. 5,480,717 provides a technique for producing a hydrogel by casting a polyvinylpyrrolidone aqueous solution on a polymer film attached to the pressure-sensitive adhesive and irradiation. In the patent, polyvinylpyrrolidone has a number average molecular weight of 200,000 to 400,000, and an epidermal layer was prepared on the surface of the polyvinylpyrrolidone to prevent the hydrogel from breaking due to evaporation of water. However, the prepared wound dressings still do not solve the problem of polyvinylpyrrolidone remaining in the wound when removing the dressing as described above.

As a result of various attempts to solve the adhesive problem of polyvinylpyrrolidone, US Pat. No. 5,389,376 shows that the polyvinylpyrrolidone solution is tackled when irradiated with polyvinylpyrrolidone to give more tackiness to be used as an adhesive. For this purpose, a method of preparing a medical pressure-sensitive adhesive was proposed by irradiating an aqueous solution of polyglycerol with polyvinylpyrrolidone. In addition, US Pat. No. 6,022,330 describes a technique for irradiating a nonwoven fabric and then graft copolymerizing N-isopropyl acrylamide to prevent the nonwoven fabric from sticking to the wound. In addition, Japanese Patent Application Laid-open No. 10-118174 deals with a technique of mixing polyethylene and ethylene-vinyl acetate copolymer, foaming using a radiation technique, and using it as a bandage. However, there still remains a problem that the wound dressing prepared by the various methods adheres to the skin or has a negligible therapeutic effect.

Therefore, the present inventors have attempted a multi-faceted study to apply to the dressing for wound treatment using a hydrogel, as a result of using a charcoal-filled hydrogel containing powdered charcoal to increase the wound healing effect on polyvinyl alcohol and polyvinylpyrrolidone synthetic polymer. In order to propose and use as a dressing for wound treatment, the polymer solution was prepared by freezing thawing and irradiation, and the prepared hydrogel dressing was excellent in ductility and strength, and it was possible to control stickiness of unreacted polymer remaining on the surface. The present invention was completed by knowing that the treatment effect can be increased by introducing deodorization (adsorption), humidity control, air purification function, filtration function, and reducing function as a wound treatment dressing as charcoal is contained.

It is an object of the present invention to provide a method for producing a hydrogel dressing for wound treatment and a hydrogel dressing prepared by the method.

1 is a schematic diagram of a rotating device used for gamma irradiation;

2 is a graph showing the relationship between the gel strength of the hydrogel according to the amount of charcoal and gamma-irradiation,

3 is a graph showing the relationship between the gelation rate of the hydrogel according to the amount of charcoal and gamma-irradiation,

4 is a graph showing the relationship between the swelling degree of the hydrogel according to the amount of charcoal and gamma-irradiation,

5 is a graph showing the swelling degree change of the hydrogel with respect to time,

6 is a graph showing the change in gel strength of hydrogel with respect to time,

7 is a graph showing the control effect of Staphylococcus aureus bacteria on charcoal-filled hydrogel;

8 is a graph showing the control effect of Pseudomonas aeruginosa bacteria of charcoal-filled hydrogel.

In order to achieve the above object, the present invention provides a hydrogel dressing consisting of polyvinyl alcohol, polyvinylpyrrolidone and charcoal.

In addition, the present invention provides a use of charcoal-filled hydrogel as a wound dressing.

In addition, in the present invention

1) freezing and melting the aqueous aqueous polymer solution in a mold to mold the first gelled hydrogel into a sheet form (step 1);

2) It provides a method for producing a hydrogel dressing comprising the step (step 2) of performing a second gelation by irradiating the sealed sheet of step 2 to radiation.

Hereinafter, the present invention will be described in detail.

The present invention provides a hydrogel dressing consisting of polyvinyl alcohol, polyvinylpyrrolidone and charcoal.

Hydrogel can function several tens of times its own weight. It is composed of polymer of 3D network structure, and it must maintain mechanical properties and shape while absorbing or drying water, and must control gel strength and swelling properly. . In particular, in order to manufacture a hydrogel for wound treatment such as burns using a polymer, the final physical properties should be designed by appropriately selecting the type and molecular weight of the polymer and increasing the compatibility between the used and mixed polymers so that phase separation does not occur.

In the hydrogel dressing of the present invention, a synthetic polymer is prepared by mixing polyvinyl alcohol and polyvinylpyrrolidone, and the hydrogel is prepared by adding charcoal to the hydrogel dressing, and when applied as a dressing for wound treatment, the wound is treated by the self-cleaning action of charcoal. Can increase the effect. In particular, the charcoal-filled hydrogel dressing containing the composition physically crosslinks polyvinyl alcohol through freeze-thawing and induces chemical crosslinking of polyvinylpyrrolidone through irradiation.

Polyvinyl alcohol is attracting attention as a medical polymer because of its excellent mechanical and thermal strength as a representative water-soluble polymer. Polyvinyl alcohol has a three-dimensional network structure through hydrogen bonds between molecules due to intramolecular hydroxyl groups, so that a large amount of water can be swelled upon contact with moisture. In the present invention, the number average molecular weight of 85,000 to 146,000 is the best physical properties, when the molecular weight is less than the above can not obtain the gel strength available as a dressing for wound treatment, if the molecular weight is excessive other mechanical properties This decreases. Physically crosslinking is possible by repeatedly freezing and thawing polyvinyl alcohol at low temperature and thawing at room temperature. As a result, handling before irradiation is easy and the strength of the hydrogel dressing is finally improved.

Polyvinylpyrrolidone has a biocompatibility as a water-soluble polymer, such as polyvinyl alcohol, has been widely used as a biomaterial including plasma for several decades, and recently, studies have been actively conducted as a vitreous substitute for the eye. Since polyvinylpyrrolidone has oxygen and nitrogen in its molecules to form hydrogen bonds with water molecules, it can contain a lot of water in a three-dimensional network structure, which is suitable for making hydrogels. In the present invention, it is preferable to use a number average molecular weight of 200,000 to 1,300,000, and in this case, when the molecular weight is less than the above, the viscosity of the polymer solution is very low so that it is easy to prepare an aqueous polymer solution, but the gelation rate and gel strength when prepared by hydrogel dressing There is a low problem, and if the molecular weight is excessive, it is difficult to prepare a high concentration of aqueous polymer solution and mechanical properties are lowered is not preferred.

In particular, the present invention produces a hydrogel dressing containing various effects and effects of charcoal by introducing charcoal into the aqueous polymer solution. Charcoal can adsorb pathogenic bacteria to inhibit infection and growth of bacteria in the wound, and can absorb odors from the wound.

The charcoal-filled hydrogel dressing of the present invention prepares a synthetic polymer in which 10 to 90% by weight of polyvinyl alcohol and 10 to 90% by weight of polyvinylpyrrolidone are prepared, and a synthetic polymer comprising the polyvinyl alcohol and polyvinylpyrrolidone. It is prepared by containing 2 to 40 parts by weight of charcoal, preferably 7 to 25 parts by weight, based on 100 parts by weight. At this time, if the content of the charcoal is less than the above range, the effect of the charcoal is insignificant and excessively, the gel strength and gelation rate of the prepared charcoal-filled hydrogel dressing are lowered, which is not suitable as a wound dressing.

Therefore, the charcoal-filled hydrogel dressing containing polyvinyl alcohol, polyvinylpyrrolidone and charcoal is prepared to be 5 to 40% by weight (solid content) in an aqueous solution, and preferably 10 to 25% by weight. If the solid content is less than the above range, it is not possible to obtain a gel strength that can be used as a dressing when prepared as a hydrogel dressing, and when excessive, the viscosity of the aqueous polymer solution is so large that it is difficult to prepare a sheet form in the manufacturing step of the hydrogel, which is not preferable.

Charcoal filled hydrogel dressing of the present invention is used as a dressing for wound healing.

Charcoal-filled hydrogel of the present invention has a three-dimensional network structure and can be easily applied to the human body by using polyvinyl alcohol and polyvinylpyrrolidone having physical properties similar to those of biological tissues and excellent biocompatibility. Appropriate adhesiveness and flexibility for use in wound healing, absorbing pathogenic bacteria, absorbing body fluids, preventing infection from bacteria, easy attachment to wounds and skin, transparency, ease of handling, storage and sterilization As it is improved, it is suitably used for wound dressings.

According to an embodiment of the present invention, as a result of the control effect on Staphylococcus aureus and Pseudomonas aeruzinosa, bacteria that can occur in human skin, the bacterial strain is more than 50% by charcoal-filled hydrogel of the present invention. It can be seen that the decrease. In addition, as a result of examining the treatment effect on the wound using rats, it was found that it showed excellent treatment effect, and the toxicity test on the human skin showed no side effects such as blister or itching at all.

In addition, the hydrogel dressing of the present invention

1) freezing and melting the aqueous aqueous polymer solution in a mold to mold the first gelled hydrogel into a sheet form (step 1);

2) Prepared through a step (step 2) of performing a second gelation by irradiating the sealed primary gelled hydrogel of step 1 to the radiation.

Each step will be described below.

In step 1, a water-soluble aqueous polymer solution is injected into a mold and lyophilized to prepare a sheet-type primary hydrogel.

Freeze thawing is carried out by freezing the aqueous aqueous polymer solution at -5 to -100 ° C for 5 minutes to 4 hours and thawing at 5 to 50 ° C for 30 minutes to 2 hours. do. The primary gelled hydrogel prepared through the freeze-thawing process is physically crosslinked and is very easy to handle in subsequent steps. In addition, the polymer aqueous solution is more preferably left in the mold to freeze bubbles before freezing and thawing.

The water-soluble polymer is a synthetic polymer such as polyvinylpyrrolidone, polyethylene oxide, polyhydroxyethyl methacrylate, polyvinyl alcohol, gelatin, agar (agar), alginate, collagen, chitosan alone Or compounds thereof.

In particular, it is prepared using polyvinyl alcohol and polyvinylpyrrolidone as a water-soluble polymer for use as a dressing for wound healing, and more preferably, charcoal is added to increase the wound healing effect. At this time, when the number average molecular weight of polyvinyl alcohol is large, it is difficult to dissolve in water at room temperature. In step 1, it is preferable to dissolve the polyvinyl alcohol and polyvinylpyrrolidone by mixing in an autoclave of about 120 ° C. .

Step 2 completes the present invention by preparing a hydrogel dressing by irradiating the sealed primary gelled hydrogel of step 1 with radiation to perform secondary gelation (step 2).

The radiation is irradiated at 5 to 100 kGy, preferably 25 to 100 kGy, using ordinary gamma rays (γ-rays) or electron beams (β-rays). Irradiation can crosslink the polymer and sterilize the hydrogel. At this time, if the radiation dose is less than the above range, the crosslinking is insufficient. Therefore, the physical properties such as the gel strength of the polymer hydrogel are lowered. There is a problem of increased water absorption and flexibility, but easily broken.

The prepared hydrogel dressing is sealed with a packaging material for use as a product. The sealing step may be performed after any one of steps 1 and 2, and preferably, the first hydrogel in the form of sheet 1 is sealed with a conventional packaging material, and then irradiated to prepare a hydrogel dressing. At this time, the packaging material that can be used may be a polymer film, such as polyethylene, polypropylene, polyvinyl chloride, nylon, polyester, aluminum foil, or a laminate of aluminum and a polymer film.

As described above, the water-soluble polymer was used to induce a physical crosslinking through freeze-thawing and a chemical crosslinking structure through irradiation to prepare a char-filled hydrogel. Unlike the case of using only radiation, the repeated operation and freezing method according to the present invention can control the stickiness of the remaining unreacted polymer while providing different ductility and strength, and irradiating without using a crosslinking agent. By crosslinking the polymer material and sterilization at the same time can be solved problems such as toxicity by the residual initiator or crosslinking agent.

For example, polyvinyl alcohol and polyvinylpyrrolidone are used as water-soluble polymers, and a charcoal-filled hydrogel dressing was prepared through the above steps by preparing an aqueous polymer solution including charcoal in order to enhance the wound healing effect. According to an embodiment of the present invention, it can be seen that the charcoal-filled hydrogel has good mechanical properties with increasing swelling over time, and shows a tendency of increasing gel strength due to evaporation of water and a low concentration of polymer. It can be seen that the gel strength remains almost constant. In addition, since it contains a large amount of water, the hydrogel was not broken due to evaporation of water even after 14 days without adding a secondary epidermal layer to prevent moisture, and the strength of the gel did not decrease. Such charcoal-filled hydrogel dressing of the present invention exhibits a great difference from the conventional hydrogel dressing in which the mechanical strength drops sharply after swelling.

Hereinafter, the present invention will be described in more detail with reference to Examples.

However, the following examples are illustrative of the present invention, and the content of the present invention is not limited by the examples.

Example 1 Preparation of Charcoal Filled Hydrogel Dressing

Charcoal-filled hydrogel dressing was prepared by varying the amount of charcoal and radiation dose contained in the hydrogel as follows.

Polyvinyl alcohol (number average molecular weight 85,000 to 146,000, manufactured by Aldrich) and polyvinylpyrrolidone (number average molecular weight of 1.3 million, manufactured by Aldrich) were used at a ratio of 6: 4 (charcoal). 5, 10, 15 and 20 parts by weight were added to 100 parts by weight of the synthetic polymer made of polyvinylpyrrolidone, respectively. A polymer aqueous solution containing polyvinyl alcohol-polyvinylpyrrolidone-charcoal was prepared by dissolving in distilled water such that the weight ratio of polymer solids including charcoal was 15% by weight. Each of the polymer aqueous solutions was poured into a Petri dish mold 4 mm high and placed in a clean room for 24 hours to remove bubbles. Subsequently, frozen at −40 ° C. for 1 hour and thawed at room temperature for 1 hour (run once). After the freeze-thawing process, the polymer aqueous solution was prepared in the form of a sheet, and then packaged in a polyethylene bag . The charcoal-filled hydrogel dressing was prepared by irradiating gamma rays of 10, 20, 30, 40 or 50 kGy using the rotating apparatus of FIG . Prepared.

Example 2 Gel Strength of Charcoal Filled Hydrogel Dressing

In order to measure the gel strength of the charcoal-filled hydrogel dressing according to the amount of charcoal contained in the hydrogel and the radiation dose, the following experiment was carried out.

The charcoal-filled hydrogel prepared in Example 1 was made into a specimen with a thickness of 3.5 mm and a width of 20 cm ² to measure the strength using a texture analyzer (Texture-Analyzer), the strength was calculated by the following equation (1).

Gel strength (gcm) = weighting force when destroyed (FB) x increased distance until destruction (DB)

The gel strength of the charcoal filled hydrogel dressing calculated by Equation 1 is shown in FIG. 2, and according to FIG. 2, the gel strength of the hydrogel dressing was generally increased as the radiation dose was increased and decreased with increasing char content. There was a tendency. However, the gel strength of the hydrogel is 50 ~ 400 g · cm is suitable to use as a wound dressing material, the char-filled hydrogel dressing prepared in Example 1 can be suitably used as a dressing for wound treatment.

Example 3 Gelation Rate of Charcoal Filled Hydrogel Dressing

In order to determine the gelation rate of the charcoal-filled hydrogel dressing according to the amount of charcoal contained in the hydrogel and the radiation dose, the following experiment was carried out.

The charcoal filled hydrogel dressing of Example 1 irradiated with gamma rays of 10, 20 or 30 kGy and the charcoal filled hydrogel dressing without gamma irradiation were taken out of a polyethylene bag and soaked in distilled water for 48 hours to dissolve and dissolve the uncrosslinked portions. The undiluted portion was put in a vacuum oven, dried at 60 ° C. for 48 hours, and the weight (W _d ) was measured. The gel content was calculated by Equation 2 below.

The gelation rate of the charcoal-filled hydrogel dressing calculated by Equation 2 is shown in FIG. 3. According to FIG . 3 , the gelation rate of the hydrogel prepared by freeze-thawing without simply irradiating gamma-rays was very low as 50%, but gamma-rays. It can be seen that the gelation rate increases as the irradiation dose increases, and it can be seen that there is almost no change in the gelation rate according to the char content.

Example 4 Swelling Degree of Charcoal Filled Hydrogel Dressing According to Charcoal Content and Radiation Dose

In order to determine the swelling degree of the charcoal-filled hydrogel dressing according to the amount of charcoal contained in the hydrogel and the radiation dose, the following experiment was carried out.

The hydrogel dressing prepared in Example 1 was taken out of a polyethylene bag and immersed in distilled water for 48 hours, and then wiped off the water on the surface with cellulose paper. Then, the weight (W _s ) was measured and put in a vacuum oven for 48 hours at 60 ° C. After drying, the weight (W _d ) was measured. Swelling was calculated by the following equation.

The swelling degree of the charcoal filled hydrogel dressing calculated by Equation 3 is shown in FIG . 4 , and according to FIG. 4 , the swelling degree of the charcoal filled hydrogel dressing showed little change in the char content and the swelling degree decreased as the radiation dose increased. Could. This decrease in swelling degree is due to the increase in the crosslinking density of the hydrogel dressing as the radiation dose increases, thereby decreasing the water absorption.

Example 5 Swelling Degree of Charcoal Filled Hydrogel Dressing with Time

In order to determine the degree of swelling over time of the polymer hydrogel, the following experiment was performed.

In the aqueous polymer solution, polyvinyl alcohol and polyvinylpyrrolidone were prepared alone or mixed with synthetic polymer and char with synthetic polymer. As the single polymer, 15% by weight of polyvinyl alcohol and 15% by weight of polyvinylpyrrolidone were used. As the synthetic polymer, polyvinyl alcohol (9% by weight) and polyvinylpyrrolidone (6% by weight) were mixed. An aqueous solution was used. In addition, the aqueous polymer solution containing 5, 10 parts by weight of charcoal based on 100 parts by weight of the synthetic polymer of Example 1 was used. Hydrogel dressings were prepared in the same manner as in Example 1 using each of the prepared aqueous polymer solutions, and the irradiation was performed at 30 kGy dose using gamma rays.

It was measured by the degree of swelling with time for each of the samples to the equation (3) shown in Figure 5 the results. According to FIG. 5 , the degree of swelling suddenly increased between 4 and 5 hours, and almost no change after 20 hours.

Example 6 Gel Strength of Charcoal Filled Hydrogel Dressing with Time

In order to determine the change in gel strength with time of hydrogel dressing, the following experiment was performed.

Each of the hydrogel dressings of Example 5 was fabricated into specimens having a thickness of 3.5 mm and a width of 20 cm 2 in order to measure gel strength and measured using a tissue analyzer. Each of the polymer hydrogel dressings was immersed in distilled water, and gel strength was measured according to the change of time. The gel strength was calculated by Equation 1 and is shown in FIG. 6 .

As can be seen in FIG. 6 , the gel strength of the polymer hydrogel dressing began to decrease suddenly between 4 and 5 hours with little change after 20 hours. In the case of polyvinylpyrrolidone, it can be seen that the decrease in gel strength is too large from 4 to 5 hours later, and thus is not suitable as a dressing material.

Preparation Example 1 Preparation of Bacteria Culture Medium

Bacteria that can develop on human skin (Staphylococcus aureus (S. aureus; Staphylococcus aureus) and Pseudomonas aeruginosa (P. aeruginosa; In order to determine the control effect on rust bacillus)), a bacterial culture medium was prepared by the following method.

Staphylococcus aureus and Pseudomonas aeruginosa were taken once with sterile platinum and then 100 ml of the pre-prepared culture 3 g of beet extract, peptone 5 g, 1,000 mL of distilled water] and then strain was incubated for 20 hours in a 37 ℃ incubator. Agar medium for Staphylococcus aureus was placed in 1 L of 146.5 g of Chapman agar, and autoclaved at 121 ° C. for 15 minutes and poured into Petri dish in clean hood for about 1/3 to 20 minutes. Then, it was hardened and then dried in an oven at 37 ° C. for 2-3 hours to prepare. Agar medium using Pseudomonas aerugino was prepared as described above in 1 g of 45 g of GSP agar.

Experimental Example 7 Control of Bacteria by Charcoal Filled Hydrogel Dressing

To determine the bacterial control effect of the hydrogel dressing with or without charcoal was measured in the following way.

Hydrogel dressing is a synthetic aqueous polymer solution of polyvinyl alcohol and polyvinylpyrrolidone of Example 1 in a weight ratio of 6: 4, and a polymer aqueous solution containing 10, 20 parts by weight of charcoal to 100 parts by weight of the synthetic polymer It was prepared by irradiation with gamma radiation at a 30 kGy dose.

Bacterial control effects of hydrogel dressings, with or without charcoal, may be associated with bacteria that may occur on human skin (Staphylococcus aureus)S. aureus; Staphylococcus aureus) and Pseudomonas aeruginosa (P. aeruginosa; The control effect on the bacterium) was examined.

9 ml of the culture solution was added to the test tube, and 1 ml of the above-described microbial solution was collected and mixed. Then, 1 g of a polymer hydrogel containing char and a polymer hydrogel containing no char was added and incubated with shaking at 37 ° C. and 150 rpm in an incubator. I was. After incubation, 1 ml of the culture solution was taken from the tube, diluted in 10 ml of 9 ml dilution water, and mixed using vortex, and then diluted 1 ² times by diluting 10 ml. Repeat this dilution up to 10 ⁸ ~ 10 ²³ times, take 0.1 ㎖ from each dilution of the bacteria solution, drop it on agar medium and apply evenly using sterile glass rod and incubate in incubator for 2-5 days at 37 ℃ incubator It was confirmed.

FIG. 7 shows the control effect of the polymer hydrogel containing charcoal on Staphylococcus aureus bacteria, and FIG . 8 shows the control effect on Pseudomonas aeruji bacteria. As can be seen in Figures 7 and 8 , the polymer hydrogel containing char is larger than the polymer hydrogel containing no char, so the adsorption of pathogenic bacteria by char is reduced by about 1/2 of the bacteria in the solution used in the experiment. It could be confirmed.

Example 7 Wound Healing Effect of Charcoal Filled Hydrogel Dressing

In order to use as a dressing for wound healing of polymer hydrogel, experimental white rats were examined for wound healing.

The epidermis was removed from the back of the experimental white rat weighing 150-200 g in a circular shape of 1.3 cm in diameter and wounded. On one wound, the hydrogel dressings of Examples 1 and 4 with a thickness of 3 mm and a size of 1.5 × 1.5 cm were attached to the white rats belonging to each group, and on the other wound 1.5 × 1.5 cm commercial vaseline gauze Constraints). On top of this, 2 × 2 cm Tegaderm (3M company) and sutures were fixed to the wounds, respectively, and the treatment progress was observed. The hydrogel and vaseline gauze were changed every three days. The experimental results are shown in Table 1 below.

Hydrogel composition Healing period Healing state Characteristic a PVA / PVP 10 to 11 days Good Excellent Healing Power b PVA / PVP / Charcoal 10 to 11 days Good Very good healing power c PVP 10-12 days usually No PVP traces on the wound d Vaseline gauze More than 14 days Bad Vaseline residue in the wound a: Synthetic polymer hydrogel comprising a weight ratio of polyvinyl alcohol / polyvinylpyrrolidone 6: 4b: Hydrogel containing 10 parts by weight of charcoal based on 100 parts by weight of synthetic polymer (PVA + PVP) c: Polyvinylpyrrolidone alone Hydrogel d: Vaseline Gauze of Sungkwang Pharm.

As can be seen in Table 1 , the wound was almost healed after about 14 days, but the healing rate of the wound with the hydrogel dressing appeared faster. Vaseline gauze dries relatively quickly and clings to the wound. The polyvinylpyrrolidone hydrogel dressings adhered slightly to the wound but the overall healing effect was much better than the gauze, and the hydrogel dressing made of polyvinyl alcohol and polyvinylpyrrolidone and an aqueous solution containing charcoal in the composition was applied to the wound. It didn't stick at all and was still more hydrated over time than other hydrogel dressings. On the other hand, charcoal added hydrogel had the best therapeutic effect and hemostatic effect in a short time.

Example 8 Skin Toxicity Test of Charcoal Filled Hydrogel Dressing

In order to use charcoal-filled hydrogel dressing for wound treatment, toxicity and side effects on human skin were performed as follows.

10 parts by weight of charcoal based on 100 parts by weight of the synthetic polymer of Example 1 was applied to the skin of a human arm 1.5 × 1.5 cm 2 using a charcoal-filled hydrogel dressing prepared by irradiation with gamma rays of 30 kGy (test 10 people) We examined the toxicity and side effects of the skin.

Hydration gel dressing for wound treatment according to the present invention has no side effects such as blistering or itching on the skin for 15 days after application of charcoal-filled hydrogel dressing. It was confirmed that it does not cause.

As described above, according to the present invention, hydrogel dressings containing charcoal in synthetic polymers of polyvinyl alcohol and polyvinylpyrrolidone were prepared by freeze-thawing and irradiation. Charcoal-filled hydrogel dressing prepared by the present invention has a low adhesiveness of stickiness and can easily control the gel strength, gelation rate and swelling degree according to the radiation dose. In particular, as charcoal is filled, it has the effect of absorbing body fluids and preventing infection from bacteria and improves the control of bacteria, thereby increasing the effect of wound healing. Charcoal-filled hydrogel dressing according to the present invention is easy to adhere to wounds and skin, transparency, handling, storage and sterilization can be suitably used as a dressing for wound treatment.

Claims (9)

Charcoal filled hydrogel dressing, characterized in that consisting of 2 to 40 parts by weight of charcoal based on 100 parts by weight of synthetic polymers consisting of 10 to 90% by weight of polyvinyl alcohol and 90 to 10% by weight of polyvinylpyrrolidone. The charcoal filled hydrogel dressing of claim 1, wherein the polyvinyl alcohol has a number average molecular weight of 85,000 to 146,000. The charcoal filled hydrogel dressing according to claim 1, wherein the polyvinylpyrrolidone has a number average molecular weight of 200,000 to 1,300,000. The charcoal-filled hydrogel dressing according to claim 1, wherein the hydrogel has a solid content of 5 to 40% by weight. A wound dressing applied to skin regeneration treatment using the charcoal-filled hydrogel dressing of claim 1. 1) freezing and melting the aqueous aqueous polymer solution in a mold to mold the first gelled hydrogel into a sheet form (step 1); 2) A method of producing a hydrogel dressing comprising the step (step 2) of performing a second gelation by irradiating the sealed primary gelled hydrogel of step 2 to radiation. The method of claim 6, wherein the aqueous aqueous solution of polymer is polyvinyl alcohol or polyvinylpyrrolidone. The method of claim 6, wherein the freeze-thawing of step 1 is repeated 1 to 10 times at a freezing temperature of -5 to-100 ° C and a thawing temperature of 5 to 50 ° C. The method of claim 6, wherein the irradiation in step 3 is gamma rays (γ-rays) or electron beams (β-rays), and the dose is 5 to 100 kGy.