KR20220049697A - Sodium Hyaluronate Mesh Film and Preparation Method Thereof - Google Patents

Abstract

The present invention relates to a hyaluronate mesh film and a method for manufacturing the same. Particularly, the hyaluronate mesh film retains its shape as it is even in a hydrated state, and thus can be used for a cosmetic mask pack, patch for a medical instrument, wound covering material, or the like. The hyaluronate mesh film according to the present invention is characterized in that hyaluronate is infiltrated into the openings of a mesh sheet. Unlike the conventional product, the hyaluronate mesh film according to the present invention is not torn when being detached from a base film, and can be detached while maintaining its shape before drying. In addition, since the thickness of the film can be controlled freely, the hyaluronate mesh film can be manufactured with ease. In addition, the hyaluronate mesh film retains its shape as it is even in a hydrated state, and thus can be applied to various uses, such as cosmetics, medicines, packs for medical instruments, patches, artificial skin, or the like.

Description

Hyaluronate mesh film and its manufacturing method {Sodium Hyaluronate Mesh Film and Preparation Method Thereof}

The present invention relates to a mesh film of hyaluronate and a method for manufacturing the same, and more particularly, to a mesh film of hyaluronate that maintains its shape even in a hydrated state and can be used as a cosmetic mask pack, a patch for medical devices, a wound dressing, etc. It relates to a manufacturing method.

Hyaluronate (Sodium Hyaluronate, Hyaluronic Acid, HA) is the highest hydrophilic substance known in nature. It is one of the components that make up skin cells along with collagen and elastin. It is called a natural moisturizer and provides excellent moisturizing power.

Hyaluronate, a jelly-like substance contained between collagen and elastin fibers, is a component naturally present in all living organisms. Hyaluronate, which is present in various parts of the human body, is particularly abundant in the skin and plays a role in giving elasticity and volume to the skin. is going on

There are patents registered for manufacturing methods of films containing high concentration hyaluronate by using the advantages of hyaluronate, but harmful preservatives such as phenoxyethanol are added to these hyaluronate films.

Japanese Patent No. 6084833 is a dried product of a hyaluronic acid solution having a viscosity of 24.5 Pa·s or more and 210 Pa·s or less, and the initial contact angle to water is 25° or more and 90° or less. Disclosed is a hyaluronic acid film characterized in that the concentration of ronic acid is 5% or more.

When using the hyaluronate film for transdermal use, it must be quickly absorbed into the skin in a hydrated state, so it is preferable to prepare it in a thin thickness using a low-viscosity hyaluronate solution. However, in the case of the existing hyaluronate film, a high-viscosity hyaluronate solution was used, and the film had to be made thicker than a certain level in order to be able to manufacture the film. When the thickness of the film is 10 μm or more, it is difficult to attach to the skin if sufficient moisture is not provided during use.

In addition, even when a thin hyaluronate film is prepared, there is a problem in that the film is torn due to the thin thickness when detached from the base film.

Therefore, as a result of the present inventors' efforts to solve the above problems, when the base film is placed on the automatic applicator and the hyaluronate solution is injected, and then the mesh sheet is placed on the hyaluronate solution and dried, the thickness is thin and hydrated It was confirmed that it was possible to manufacture a hyaluronate mesh film that maintains its shape even during the process, and the present invention was completed.

An object of the present invention is to provide a method for preparing a hyaluronate film without the use of an excipient for film formation.

Another object of the present invention is to provide a hyaluronate film and a method of manufacturing the same, which are thin in thickness and capable of maintaining shape without curling of the edge portion during hydration.

Another object of the present invention is to provide a cosmetic mask pack and patch, a medical device patch, and a wound dressing containing a hyaluronate film that is easily absorbed through the skin only with purified water.

In order to achieve the above object, the present invention provides a hyaluronate mesh film, characterized in that the hyaluronate is permeated into the hole of the mesh sheet.

The present invention also comprises the steps of (a) dissolving a hyaluronate in a solvent to prepare a hyaluronate solution of 0.1 to 30.0% by weight; (b) injecting the prepared hyaluronate solution after positioning the base film in the automatic applicator; and (c) placing the mesh sheet on the injected hyaluronate solution and drying the mesh sheet.

In the present invention, the hyaluronate solution is characterized in that the casting to a thickness of 0.05 ~ 5.0 mm.

In the present invention, the thickness of the mesh sheet is 0.1 ~ 0.3mm, it is characterized in that 400 ~ 800mesh.

In the present invention, the mesh sheet is polyurethane, TPE (thermoplastic elastomer), nylon, polyester, viscose rayon, Lanseal, polypropylene, polyethylene, polyethylene terephthalate (PET), polylactic acid (PLA), latex , characterized in that it is selected from the group consisting of non-woven fabric and silicone.

In the present invention, the elongation of the mesh sheet is characterized in that 10 to 30%.

In the present invention, the thickness of the hyaluronate mesh film is characterized in that 0.1 ~ 0.3mm.

The present invention also provides a cosmetic mask pack, a medical device patch, and a wound dressing comprising a hyaluronate mesh film.

Unlike conventional products, the hyaluronate mesh film of the present invention does not tear the film when it is detached from the base film, and has the effect of being able to detach while maintaining the shape before drying. In addition, the thickness of the film can be freely controlled, so it is easy to manufacture, and the shape is maintained even in a hydrated state, so that it can be applied to various uses such as cosmetics, pharmaceuticals, medical device packs, patches, and artificial skin.

1 is an external photograph of the hyaluronate mesh film of the present invention and the conventional hyaluronate film detached from the base film (left: Example 1, right: Comparative Example 1).
2 is a photograph showing the appearance of the hyaluronate mesh film of the present invention detached from the base film and the conventional hyaluronate film when hydrated (left: Example 1, right: Comparative Example 1).

In the present invention, when a mesh sheet is used, it is possible to manufacture a hyaluronate mesh film that is thin and has excellent skin absorption, but is not detached from the base film or damaged during hydration and maintains its shape.

In the present invention, a hyaluronate solution of various concentrations is cast to various thicknesses, a mesh sheet is placed on the hyaluronate solution and dried to prepare a hyaluronate mesh film, and then the thickness of the prepared hyaluronate mesh film; It was checked whether the base film was damaged during detachment or hydration.

As a result, when 0.1 to 30.0 wt% of a hyaluronate solution was dried at a temperature of 30 to 70 ° C. It can be prepared to a thickness of 0.5 mm, and the prepared hyaluronate mesh film maintained its shape without damage to the film even when it was detached from the base film or hydrated for skin application.

Accordingly, the present invention in one aspect, (a) dissolving the hyaluronate in a solvent to prepare a 0.1 to 30.0% by weight hyaluronate solution; (b) injecting the prepared hyaluronate solution after positioning the base film in the automatic applicator; And (c) it relates to a method for producing a hyaluronate mesh film comprising the step of placing the mesh sheet on the injected hyaluronate solution, and drying.

In the present invention, the hyaluronate salt is bound to hyaluronic acid, and may include sodium hyaluronate, calcium hyaluronate, potassium hyaluronate, and the like, but is not limited thereto.

In the present invention, the molecular weight of the hyaluronate may be used without any particular limitation, but it is preferably 3 kDa to 2.5 MDa. In addition, the content of the hyaluronate in the hyaluronate solution is characterized in that 0.1 to 30.0% by weight. That is, when the concentration of the hyaluronate solution is less than 0.1% by weight, there is a difficulty in film forming, and when it exceeds 30% by weight, the coated surface of the film may be irregular due to high viscosity. For reference, the viscosity of the hyaluronate solution in the above range corresponds to 300 ~ 100,000 cPs. In the case of low molecular weight hyaluronic acid, it must be dissolved at a high concentration to meet the reference viscosity, and in the case of high molecular weight hyaluronic acid, it must be dissolved at a low concentration to match the reference viscosity to produce a uniform film.

The solvent is for dissolving the hyaluronate, 100% water or an aqueous ethanol solution may be used, and the ethanol aqueous solution preferably has an ethanol content of 0.01 to 30% by volume. When dissolving hyaluronate using water alone, much attention is required to prevent microbial contamination. However, when dissolving hyaluronate with an aqueous ethanol solution, the effect of preventing microbial contamination is excellent as the ethanol content increases. However, there is an effect of shortening the film formation time. However, when the ethanol content exceeds 30% by volume, there is a problem in that the film becomes opaque or the film is not formed as the molecular weight of the hyaluronate increases.

In the present invention, the automatic applicator is a device widely used in manufacturing a general film, and includes an applicator and a thickness control dial for controlling the thickness of the main body and the film.

In the present invention, after positioning the base film in the automatic applicator, the step of injecting the prepared hyaluronate solution is performed. The base film can be used without particular limitation as long as it protects the hyaluronate film and can be easily peeled off later, and may be exemplified by polyethylene (PE), polypropylene, polyester, and the like.

The hyaluronate solution is preferably cast to a thickness of 0.05 to 5.0 mm using an applicator and a thickness control dial.

In the present invention, it is characterized in that the hyaluronate film is made thin so that it can be quickly absorbed by the skin, and the mesh sheet is placed on the injected hyaluronate solution to maintain its shape even during hydration, and then dried.

The mesh sheet has a thickness of 0.1 to 0.3 mm, preferably 400 to 800 mesh. When the thickness of the mesh sheet exceeds 0.3 mm, the mesh is thick and there is a problem that skin adhesion or feeling is reduced. When the thickness is less than 400 mesh, the solution is not evenly applied to the mesh sheet and exceeds 800 mesh When the mesh film is detached from the skin attachment site, there is a problem in that it cannot be completely detached and remains in a hydrated state on the mesh sheet.

The material of the mesh sheet is polyurethane, TPE (thermoplastic elastomer), nylon, polyester, viscose rayon, Lanseal, polypropylene, polyethylene, polyethylene terephthalate (PET), polylactic acid (PLA), latex, nonwoven fabric, It is preferable to use silicone or the like, and the elongation of the mesh sheet is preferably 10 to 30%. When the elongation rate of the mesh sheet exceeds 30%, the shape is not maintained in the cast state during the drying process, and it is difficult to fix the mesh sheet. There is a problem that the acid solution does not penetrate evenly.

In the present invention, the drying of the hyaluronate mesh film is preferably performed for 6 to 10 hours at 30 to 70 ℃ conditions. As long as the drying is performed at 30 to 70° C., various drying methods may be used without particular limitation. If the drying is less than 30 ℃, there is a problem that is not completely dried, when it exceeds 70 ℃, there is a problem that the film is separated from the mesh sheet due to excessive drying.

In the present invention, the hyaluronate mesh film can be prepared by placing a mesh sheet on the base film and then drying the hyaluronate solution after injecting it, but the hyaluronate solution must be cast to a thickness greater than the mesh sheet thickness.

The present invention also relates to a hyaluronate mesh film characterized in that the hyaluronate is permeated into the pores of the mesh sheet.

The hyaluronate contained in the hyaluronate mesh film preferably has a molecular weight of 3 kDa to 2.5 MDa, and a hyaluronate solution having a hyaluronate content of 0.1 to 30.0 wt % is dried.

The mesh sheet included in the hyaluronate mesh film may be of the same material, thickness, and mesh as described above.

The thickness of the finally prepared hyaluronate mesh film is preferably 0.1 to 0.5 mm.

The hyaluronate mesh film according to the present invention can be easily molded into a desired shape with ordinary scissors or a knife, has excellent mechanical properties through the mesh sheet serving as a support, and can maintain its shape even when hydrated. It can be used as a cosmetic mask pack containing a mesh film, a patch for medical devices, and a wound dressing.

[Example]

Hereinafter, the present invention will be described in more detail through examples. These examples are only for illustrating the present invention, and it will be apparent to those of ordinary skill in the art that the scope of the present invention is not to be construed as being limited by these examples.

Example 1: Confirmation of the ability to form a hyaluronate mesh film according to molecular weight

Hyaluronate (molecular weight 3kDa, 0.1MDa, 0.8MDa, 1.2MDa and 2.5MDa) was dissolved in each 20% by volume aqueous ethanol solution at a concentration of 0.3 to 30% by weight.

After positioning the polyethylene base film in an automatic applicator (COAD 411, Uiwang Machinery, Korea), the thickness of the film applicator of the automatic applicator was set to 1.0 mm, and the dissolved hyaluronate solution was injected.

A mesh sheet (PE, thickness: 0.17 mm, 500 mesh, elongation 12%) was placed on the hyaluronate solution injected into the automatic applicator, and then dried at 40° C. for 6 to 10 hours to prepare a hyaluronate mesh film.

As a result, when 3 kDa hyaluronate is used, the concentration of hyaluronate is increased to 15% by weight, and when 2.5MDa is used, when the concentration of hyaluronate is lowered to 0.1% by weight, a mesh film of hyaluronate can be prepared. was found to be That is, when the concentration of the hyaluronate solution was appropriately adjusted according to the molecular weight of the hyaluronate, a hyaluronate mesh film could be manufactured.

However, when using a 3kDa hyaluronate 0.1% by weight solution, there are some empty spaces that are not filled with the hyaluronate solution between the meshes of the dried film, so it is preferable to prepare at least 15% by weight.

Example 2: Confirmation of the formation ability of the hyaluronate mesh film according to the thickness of the film applicator

Hyaluronic acid salt (molecular weight 0.8MDa) was dissolved in 20 vol% ethanol aqueous solution, respectively. It was dissolved at a concentration of 1.0% by weight.

After positioning the polyethylene base film in an automatic applicator (COAD 411, Uiwang Machinery, Korea), the thickness of the film applicator of the automatic applicator was set to 0.01 to 6.0 mm, and the dissolved hyaluronate solution was injected.

A mesh sheet (PE, thickness: 0.17 mm, 500 mesh, elongation 12%) was placed on the hyaluronate solution injected into the automatic applicator, and then dried at 40° C. for 6 to 10 hours to prepare a hyaluronate mesh film.

As a result, when the thickness of the applicator was less than 0.1 mm, there was a problem that the hyaluronate solution could not be filled between the meshes after the film was dried. When it exceeds 5.0 mm, there was a problem in that the surface was cast unevenly, but in the case of 0.1 to 5.0 mm, it was found that a mesh film was well formed.

Example 3: Confirmation of the ability to form a hyaluronate mesh film according to the mesh sheet

Hyaluronate (molecular weight 0.8MDa) was dissolved in 20% by volume ethanol aqueous solution at a concentration of 1.0% by weight.

After positioning the polyethylene base film in an automatic applicator (COAD 411, Uiwang Machinery, Korea), the thickness of the film applicator of the automatic applicator was set to 1.0 mm, and the dissolved hyaluronate solution was injected.

Put a mesh sheet (PE, thickness: 0.05-0.5 mm, 300-900 mesh, elongation: 5-40%) on the hyaluronate solution injected into the automatic applicator, and then dry the hyaluronate mesh film at 40°C for 6-10 hours. prepared.

As a result, it was found that the film formation was best when the thickness of the mesh sheet was 0.1 to 0.3 mm, 400 to 800 mesh, and the elongation was 10 to 30%, depending on the thickness of the mesh sheet, the mesh and the elongation of the mesh sheet. On the other hand, when the mesh sheet is less than 400mesh, an empty space without a hyaluronate solution was confirmed between the meshes of the dried film as the size of the mesh increased. The film remained on the mesh sheet instead of the attachment site, making it impossible to use.

In addition, when the elongation of the mesh sheet is less than 10%, there is no problem in manufacturing the film, but the feeling of use is reduced due to the stiff and rough feeling generated when attached to the skin. Due to this, while the film was applied, the mesh could not be attached to the hyaluronate solution and showed mobility, resulting in wrinkles in the drying process.

Example 4: Confirmation of the ability to form a hyaluronate mesh film according to the drying temperature

Hyaluronate (molecular weight 0.8MDa) was dissolved in 20% by volume ethanol aqueous solution at a concentration of 1.0% by weight.

After positioning the polyethylene base film in an automatic applicator (COAD 411, Uiwang Machinery, Korea), the thickness of the film applicator of the automatic applicator was set to 1.0 mm, and the dissolved hyaluronate solution was injected.

A mesh sheet (PE, thickness: 0.17 mm, 500 mesh, elongation 12%) was placed on the hyaluronate solution injected into the automatic applicator, and then dried at 20 to 80° C. for 6 to 10 hours to prepare a hyaluronate mesh film.

As a result, depending on the drying temperature, when the drying temperature was less than 30 ℃, an undried part occurred during drying, and when it exceeded 70 ℃, the mesh sheet and the film part were peeled off due to excessive drying.

Comparative Example 1: Preparation of a conventional hyaluronate film

A hyaluronate film was prepared in the same manner as in Example 1, except that a mesh sheet was not used and a hyaluronate of 0.8 MDa was used.

Experimental Example 1: Base film detachment of hyaluronate mesh film

The base film of the hyaluronate mesh film prepared in Examples 1 to 4 and the hyaluronate film prepared in Comparative Example 1 was detached.

As a result, as shown in FIG. 1 , the hyaluronate film prepared in Comparative Example 1 was torn when detached from the base film, whereas in the case of the hyaluronate mesh films prepared in Examples 1 to 4 of the same thickness. It was confirmed that detachment from the base film was easy.

Experimental Example 2: Appearance comparison of hydrated hyaluronate mesh film

In order to attach the hyaluronate film to the skin, it is necessary to hydrate the hyaluronate film. Therefore, after detaching the base film of the hyaluronate mesh film prepared in Examples 1 to 4 and the hyaluronate film prepared in Comparative Example 1, it was attached to the skin and hydrated by spraying purified water.

As a result, as shown in FIG. 2 , the hyaluronate mesh film in Examples 1 to 4 maintained the appearance even after being hydrated, whereas the hyaluronate film prepared in Comparative Example 1 had only the edge portion due to the curling phenomenon. It was confirmed that it was thickly aggregated. The agglomerated parts are not absorbed into the skin and remain, giving a feeling of foreign body.

As the specific parts of the present invention have been described in detail above, for those of ordinary skill in the art, it is clear that these specific descriptions are only preferred embodiments, and the scope of the present invention is not limited thereby. will be. Accordingly, it is intended that the substantial scope of the present invention be defined by the appended claims and their equivalents.

Claims (13)

A hyaluronate mesh film, characterized in that the hyaluronate is permeated into the holes of the mesh sheet.
The hyaluronate mesh film according to claim 1, wherein the mesh sheet has a thickness of 0.1 to 0.3 mm, and 400 to 800 mesh.
According to claim 1, wherein the mesh sheet is polyurethane, TPE (thermoplastic elastomer), nylon, polyester, viscose rayon, Lanseal, polypropylene, polyethylene, polyethylene terephthalate (PET), polylactic acid (PLA), A mesh film of hyaluronate, characterized in that it is selected from the group consisting of latex, non-woven fabric and silicone.
According to claim 1, wherein the elongation of the mesh sheet is hyaluronate mesh film, characterized in that 10 to 30%.
The hyaluronate mesh film according to claim 1, wherein the hyaluronate mesh film has a thickness of 0.1 to 0.5 mm.
(a) dissolving the hyaluronate in a solvent to prepare a hyaluronate solution of 0.1 to 30.0% by weight;
(b) injecting the prepared hyaluronate solution after positioning the base film in the automatic applicator; and
(c) placing the mesh sheet on the injected hyaluronate solution, and drying the method for producing a hyaluronate mesh film.
The method of claim 6, wherein the hyaluronate solution is cast to a thickness of 0.05 to 5.0 mm.
The method of claim 6, wherein the mesh sheet has a thickness of 0.1 to 0.3 mm and 400 to 800 mesh.
According to claim 6, wherein the mesh sheet is polyurethane, TPE (thermoplastic elastomer), nylon, polyester, viscose rayon, Lanseal, polypropylene, polyethylene, polyethylene terephthalate (PET), polylactic acid (PLA), A method for producing a hyaluronate mesh film, characterized in that it is selected from the group consisting of latex, non-woven fabric and silicone.
The method of claim 6, wherein the elongation of the mesh sheet is 10 to 30%.
A cosmetic mask pack comprising the hyaluronate mesh film of any one of claims 1 to 5.
A medical device patch comprising the hyaluronate mesh film of any one of claims 1 to 5.
A wound dressing comprising the hyaluronate mesh film of any one of claims 1 to 5.

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