KR20180006784A - Cellulose based wound dressing with antimicirobial filler and manufacturing method thereof - Google Patents

Abstract

The present invention relates to a method for manufacturing a wound dressing by mixing carboxymethyl cellulose with antimicrobial carbon complex without a toxic cross-linking agent and a catalyst for cross-linking and irradiating radiation. Accordingly, a wound dressing, which is harmless to a wound part, is easy to manufacture and shows high degree of cross-linking, absorption and wound healing power, can be manufactured.

Description

[0001] The present invention relates to a high-functional cellulose wound dressing containing an antimicrobial composition and a method for producing the same,

The present invention relates to a high-functional cellulose wound dressing containing an antimicrobial composition and a method for producing the same, and more particularly to a carboxymethylcellulose (CMC) cellulose derivative, which is obtained by heat-treating a powdery activated carbon impregnated with a silver nitrate solution, And then crosslinking by irradiation with radiation to form a hydrogel-like wound dressing.

Generally, a living organism has a property of defending itself to a certain extent and attempting self-healing when a defective site occurs in the body (living body). Particularly, when the defective portion of the living body is skin, the biocompatibility of the cover material to be used is strictly required, and the highly sensitive condition should be satisfied. Wound dressings are used to assist in the treatment of wounds and burns. They help protect the affected area temporarily until the damaged skin is recovered, helping to regenerate the skin through absorption of exudates, bleeding or loss of fluids and infection. Natural and synthetic polymer materials are used as the material to be used. The type of covering material can be classified into film type, foam type, hydration gel type, hydrocolloid type and the like depending on the product form. The film type covering material is a dressing material with a semi-permeable adhesive, which protects the wound area from bacterial infection and maintains a wet environment And it is used by applying film and adhesive of various materials. In the case of foam-type dressing material, it has an excellent absorbing power and evaporation power as compared with other covering materials, so it is suitable for deep wounds having a large amount of effusion, expands after absorbing the effusion, and compresses the wound to reduce swelling around the wound. The hydrated gel-type covering material is excellent in the ability to absorb exudates discharged from wounds due to many pores and micro spaces, and has good oxygen permeability, so that it can exhibit excellent tissue regeneration ability not only for covering materials but also for vascular grafts and tissue engineering supports.

The polyurethane foam dressing material is the mainstream wet wrinkle covering material and the hydrocolloid type covering material is used for the wound having a relatively small amount of exudate. However, since the coverage of the covering material tends to be lowered, development of a wound covering material having a higher added value . As a high value added wound dressing material, a dressing material for promoting the absorption of exudates and a dressing material for infectious wound dressing containing a silver ingredient having an antibacterial action are representative, and the high therapeutic efficacy of the antibacterial dressing material is attracting attention. These highly functional antimicrobial coatings exhibit excellent properties in the wound healing ability of infections, but their selling prices are excessively high, and thus there is a growing need for high-performance / low-cost therapeutic dressings having antimicrobial properties from cheap raw materials through cheap processes.

An object of the present invention is to provide a method for manufacturing a wound dressing material which is non-toxic and easy to manufacture by radiation irradiation in order to solve the above-mentioned problems.

Another object of the present invention is to provide a wound dressing which is manufactured by a method of manufacturing a wound dressing material which is non-toxic and easy to manufacture by irradiation, and which is effective for wound healing composed of carboxymethylcellulose / antibacterial carbon composite gel.

To achieve these and other advantages and in accordance with the purpose of the present invention,

(1) a step of immersing activated carbon in an aqueous solution of silver precursor salt to adsorb silver ions on activated carbon;

(2) heat treating the activated carbon in the step (1) to produce an antimicrobial carbon composite;

(3) adding the antimicrobial carbon composite prepared in step (2) to a mixture of carboxymethylcellulose (CMC) and distilled water;

(4) irradiating and cross-linking the mixed solution of step (3) with radiation;

(5) drying the carboxymethyl cellulose and the antimicrobial carbon composite gel prepared in the step (4), thereby producing a wound dressing which is non-toxic, easy to manufacture and effective in wound healing.

In the step (1), the aqueous solution of the silver precursor salt is an aqueous solution containing at least one salt selected from the group consisting of silver nitrate, silver acetate, silver chloride, silver carbonate, silver sulfate, silver bromide and phosphoric acid.

In the step (2), the heat treatment is performed at 250 to 400 ° C for 1 minute to 5 hours under an inert atmosphere.

In the step (3), 5 to 20 wt% of carboxymethyl cellulose and distilled water are mixed, and 0.5 to 3 wt% of the antibacterial carbon composite is added to the mixed solution.

In the step (4), the radiation is any one selected from the group consisting of a gamma ray, an electron beam, an ion beam, a neutron beam, UV, and plasma, and the total irradiation dose is 5 to 100 kGy.

The drying in the step (5) is any one selected from the group consisting of thermal drying, natural drying, and freeze drying.

The present invention also provides a highly functional cellulose wound dressing comprising an antimicrobial composition prepared by the method described above.

The wound dressing material which is non-toxic, easy to manufacture and effective in wound healing according to the present invention is prepared by blending carboxymethyl cellulose and antimicrobial carbon composite without using a crosslinking agent having a toxicity and a catalyst for crosslinking and then irradiating the wound dressing material It is harmless to the wound area, is easy to produce, exhibits high crosslinking degree, high absorbability and high wound healing power, and thus can be usefully used as a wound dressing material.

1 is a cross-sectional photograph of a wound dressing prepared according to the present invention.
2 is a graph showing the compressive strengths of the wound dressings prepared according to Examples 1 to 4 of the present invention.
3 is a graph showing the degree of swelling of the wound dressing prepared according to Examples 1 to 4 of the present invention.

Hereinafter, preferred embodiments of the present invention will be described in detail. The present invention is not limited to the scope of the present invention, but is merely an example, and various modifications can be made without departing from the technical spirit of the present invention.

(1) a step of immersing activated carbon in an aqueous solution of silver precursor salt to adsorb silver ions on activated carbon; (2) heat treating the activated carbon in the step (1) to produce an antimicrobial carbon composite; (3) adding the antibacterial carbon composite prepared in step (2) to a solution of carboxymethyl cellulose and distilled water; (4) irradiating and cross-linking the mixed solution of step (3) with radiation; (5) drying the carboxymethyl cellulose and the antibacterial carbon composite gel prepared in the step (4).

In the production method of the present invention, the step (1) is a step of immersing the activated carbon in an aqueous solution of the silver precursor salt to adsorb silver ions to the activated carbon.

Specifically, in the step (1), the aqueous solution of the precursor salt preferably contains at least one salt selected from the group consisting of silver nitrate, silver acetate, silver chloride, silver carbonate, silver sulfate, silver bromide, and silver phosphate. More specifically, it is more preferable to use an aqueous silver nitrate solution.

In the production method of the present invention, the step (2) is a step of producing the antimicrobial carbon composite by heat-treating the activated carbon of the step (1).

Specifically, in the step (2), the heat treatment is preferably performed at 250 to 400 ° C for 1 minute to 5 hours under an inert atmosphere. If the heat treatment is performed for less than 1 minute, the treatment time is too short to remove the anion salt, and if the heat treatment is performed for more than 5 hours, the antimicrobial carbon composite is oxidized too much to have a physical property difficult to be added to the mixed solution in the next step.

In the production method of the present invention, the step (3) is a step of adding an antimicrobial carbon composite to a solution obtained by mixing carboxymethylcellulose and distilled water.

Specifically, in the step (3), 5 to 20 wt% of the carboxymethyl cellulose and distilled water are preferably mixed, and 0.5 to 3 wt% of the antibacterial carbon composite is preferably added. Less than 5 wt% of carboxymethylcellulose or less than 0.5 wt% of the antimicrobial carbon composite is too small to be crosslinked, and more than 20 wt% of carboxymethylcellulose or more than 3 wt% of the antimicrobial carbon composite interferes with crosslinking, The absorbency of the manufactured wound dressing is lowered.

In the manufacturing method according to the present invention, the step (4) is a step of irradiating the cross-linking solution of the mixed solution of the step (3).

Specifically, in the step (4), the radiation is preferably selected from the group consisting of a gamma ray, an electron beam, an ion beam, a neutron beam, UV and plasma, and is preferably selected from the group consisting of gamma ray, electron ray and neutron ray desirable.

In the step (4), it is preferable that the total dose of radiation is 5 to 100 kGy. If the total irradiation amount of the radiation exceeds 100 kGy, the crosslinking between the carboxymethyl cellulose and the antibacterial carbon composite may be interrupted, or the physical properties and the absorbing power of the wound dressing after absorption may be lowered. The irradiation time of the radiation can be appropriately selected depending on the amount of the solution of the carboxymethyl cellulose / antibacterial carbon composite to be gelated and the strength of the desired gel.

In the manufacturing method according to the present invention, the step (5) is a step of drying the carboxymethylcellulose / antibacterial carbon composite gel prepared in the step (4).

Specifically, the drying in step (5) is preferably selected from the group consisting of heat drying, natural drying and freeze drying, but is not limited thereto.

The present invention also provides a wound dressing made by the above-described manufacturing method.

Hereinafter, the present invention will be described in more detail with reference to Examples and Experimental Examples. However, the embodiments are only examples of the present invention, and the scope of the present invention is not limited thereto.

[Example 1]

Powdered activated carbon was added to the silver nitrate aqueous solution at a weight ratio of 1: 1, and silver ions were adsorbed by stirring for 2 hours. Thereafter, powdery activated carbon adsorbed on the silver ion was heat - treated at 300 ° C for 1 hour in an inert argon atmosphere to remove nitrate ions to prepare an antimicrobial carbon composite. 15% by weight of carboxymethylcellulose was mixed with distilled water, and 1.0% by weight of an antibacterial carbon composite was added. Next, the carboxymethyl cellulose / carbon composite wound dressing was prepared by irradiating electron beams to the carboxymethyl cellulose / carbon composite mixture solution three times at a dose rate of 10 kGy, gelling and naturally drying.

[Example 2]

A wound dressing material was prepared in the same manner as in Example 1, except that the electron beam was irradiated five times.

[Example 3]

A wound dressing material was prepared in the same manner as in Example 1, except that the electron beam was irradiated seven times.

[Example 4]

A wound dressing material was prepared in the same manner as in Example 1, except that the electron beam was irradiated nine times.

[Comparative Example 1]

A wound dressing material was prepared in the same manner as in Example 1, except that powdered activated carbon in which silver ions were not adsorbed was added instead of the carbon composite material.

[Test Example 1]

A cross-sectional photograph was taken through an SEM to confirm whether or not the wound dressing prepared according to the above example was sufficiently gelated. FIG. 1 is a cross-sectional photograph of the wound dressing prepared in Example 2 by freeze-drying. It can be seen that the wound dressing prepared according to the present invention has a uniform pore structure.

[Test Example 2]

In order to examine the influence of the electron beam dose on the strength of the above Examples 1 to 4, the compressive strengths of the wound dressings prepared according to Examples 1 to 4 were measured using a micro material tester. Respectively. As the dose of electron beam increases, the compressive strength increases. It is considered that the crosslink density increases with increasing irradiation dose of electron beam, and the compressive strength increases with increasing crosslink density.

[Test Example 3]

The swelling degrees of the wound dressings prepared in Examples 1 to 4 were measured in order to examine the effect of the electron beam dose on the swelling degree of the wound dressing in the above Examples 1 to 4. The results are shown in FIG. It was confirmed that the degree of swelling decreased with increasing dose of electron beam. As the irradiation dose of electron beam increases, the degree of swelling decreases due to the increased crosslink density in the wound dressing.

[Test Example 4]

The antibacterial properties of Example 1 and Comparative Example 1 were tested. The method of ASTM E2149 was used, and Table 1 shows the results.

Example 1 (Carbon composite) Comparative Example 1 (Powder activated carbon) Antimicrobial activity
(%) Staphylococcus aureus Klebsiella pneumoniae Pseudomonal aeruginosa Staphylococcus aureus Klebsiella pneumoniae Pseudomonal aeruginosa 99.9 99.9 99.9 0 99.9 99.7

Carried out in the antibacterial test for Staphylococcus aureus (Staphylococcus aureus) Example 1 Comparative Example 1, while showing a high antimicrobial activity did not show antimicrobial activity.

Claims (6)

(1) a step of immersing activated carbon in an aqueous solution of silver precursor salt to adsorb silver ions on activated carbon;
(2) heat treating the activated carbon in the step (1) to produce an antimicrobial carbon composite;
(3) adding the antimicrobial carbon composite prepared in step (2) to a mixture of carboxymethylcellulose (CMC) and distilled water;
(4) irradiating and cross-linking the mixed solution of step (3) with radiation;
(5) drying the carboxymethyl cellulose and the antibacterial carbon composite gel prepared in the step (4); and (5) drying the antibacterial carbon composite gel.
The method according to claim 1,
In the step (1), the aqueous solution of the silver precursor salt is an aqueous solution containing at least one salt selected from the group consisting of silver nitrate, silver acetate, silver chloride, silver carbonate, silver sulfate, silver bromide, Wherein the heat treatment is carried out at 250 to 400 DEG C for 1 minute to 5 hours under an inert atmosphere.
The method according to claim 1,
Characterized in that in step (3), 5 to 20 wt% of carboxymethyl cellulose is mixed with distilled water, and 0.5 to 3 wt% of an antimicrobial carbon composite is added to the mixed solution. The method for producing a highly functional cellulose wound dressing .
The method according to claim 1,
In the step (4), the radiation is any one selected from the group consisting of a gamma ray, an electron beam, an ion beam, a neutron beam, UV, and plasma, and the total irradiation amount of the radiation is 5 to 100 kGy. ≪ / RTI > by weight of the cellulose.
The method according to claim 1,
Wherein the drying in step (5) is any one selected from the group consisting of thermal drying, natural drying, and freeze drying.
A highly functional cellulose wound dressing comprising an antimicrobial composition produced by the method of any one of claims 1 to 5.

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