KR20160146259A

KR20160146259A - Method for preparing hydro gel containing bio cellulose

Info

Publication number: KR20160146259A
Application number: KR1020150083277A
Authority: KR
Inventors: 오한선; 정영수; 박예경; 최수정
Original assignee: (주)뷰티화장품
Priority date: 2015-06-12
Filing date: 2015-06-12
Publication date: 2016-12-21

Abstract

The present invention relates to a production method of hydrogel including bio cellulose, which comprises the following steps: (a) inoculating a culture liquid including coconut juice with strains, and fermenting the same to obtain the bio cellulose; (b) crushing the bio cellulose obtained from the step (a); and (c) mixing the crushed bio cellulose with an aqueous solution of polyvinyl alcohol, carrageenan, and xanthan gum, and solidifying the mixture to obtain the hydrogel. The hydrogel including bio cellulose produced by the present invention includes bio cellulose which is obtained by fermenting coconut juice and has improved tensile strength compared to conventional hydrogel produced by only using water-soluble polymer components, and thereby can be used for cosmetic masks or dressing agents. The hydrogel including bio cellulose has improved adhering properties when being used on the skin. The hydrogel which is soaked in toners or medicines can improve a moisturizing effect and by allowing effective components to penetrate deep into the skin.

Description

BACKGROUND OF THE INVENTION 1. Field of the Invention [0001] The present invention relates to a method for preparing a hydrogel containing bio-

The present invention relates to a method for producing a hydrogel containing bio-cellulose.

Hydrogel means a hydrophilic polymer polymer which is prepared by using water as a dispersion medium and can maintain a three-dimensional shape without dissolving or dissociating in a sufficient amount of water. The hydrogel is an extracellular matrix, which is a natural tissue of the human body, It has a similar structure, excellent biocompatibility and viscoelastic properties, and excellent oxygen and nutrient permeability. In addition, the hydrogel can be prepared from various polymers, and has advantages of non-toxicity, excellent biocompatibility, high moisture content, excellent mechanical properties and easy processability, and thus is used for manufacturing products in biomedical or pharmaceutical fields.

Particularly, in recent years, hydrogels prepared using polyvinyl alcohol are generally used for producing artificial cartilage, molded implants, contact lenses, wound dressings or drug delivery media.

The polyvinyl alcohol may be crosslinked by a chemical or physical method to form a hydrogel. However, the hydrogel prepared by crosslinking as described above has relatively low mechanical properties such as tensile strength, Have problems.

Accordingly, in order to overcome the disadvantages described above, a hydrogel having improved tensile strength is prepared by using a natural polysaccharide such as agar, carrageenan, or logger beech gum in the production of a hydrogel.

For example, Patent Document 1 discloses a water-soluble hydrogel pack composition comprising agar, xanthan gum, carrageenan and rogurbin gum, and a technical content of a mask pack using the same.

However, since such a hydrogel sheet is generally made thick in order to secure a sufficient tensile strength, there is a limitation in sufficiently supplying nutrients useful for the skin due to the thick thickness, and the disadvantage that the hydrogel sheet can not sufficiently cover the bending portion of the skin have.

Therefore, there is a need for research on a method for producing a hydrogel having a sufficient tensile strength and a thin thickness.

Korean Registered Patent No. 10-1497040 (Registered on Feb. 23, 2015) Korean Patent Laid-Open No. 10-2014-0129509 (published on July 11, 2014). Korean Published Patent No. 10-2012-0043287 (published on May 4, 2012). Korean Patent Laid-Open No. 10-2010-0061402 (Published on June 7, 2010)

The inventors of the present invention have been studying a hydrogel, and it has been found that a hydrogel having improved tensile strength and moisturizing properties can be prepared by using a bio-cellulose to prepare a hydrogel.

Accordingly, it is an object of the present invention to provide a technical content of a hydrogel containing bio-cellulose which can be used as a cosmetic mask pack and a dressing agent.

In order to accomplish the above object, the present invention provides a method for producing bio-cellulose, comprising: (a) (b) pulverizing the bio-cellulose produced in step (a); And (c) mixing the pulverized bio-cellulose of step (b) with an aqueous solution containing polyvinyl alcohol, carrageenan and xanthan gum to prepare a hydrogel, and then hydrogel is produced. to provide.

In one embodiment, the culture of step (a) may comprise 50-90 wt% of coconut juice.

In one embodiment, the strain of step (a) may be at least one selected from the group consisting of genus Acetobacter, Rizobium genus and Agrobacterium genus.

In one embodiment, the bio-cellulose of step (c) may comprise from 0.1 to 20% by weight, based on the total weight of the hydrogel.

In one embodiment, the hydrogel of step (c) may comprise a crosslinking agent.

According to one aspect of the present invention, there is provided a hydrogel produced by the above-described method.

According to one aspect of the present invention, there is provided a cosmetic mask pack comprising the hydrogel as a support.

According to one aspect of the present invention, there is provided a dressing agent comprising the hydrogel as a support.

The hydrogel containing bio-cellulose prepared according to the present invention includes bio-cellulose prepared by fermenting coconut juice, and has a higher tensile strength than a hydrogel prepared using only a conventional water-soluble polymer component. Thus, a cosmetic mask pack and a dressing agent Can be usefully used.

In addition, the hydrogel containing bio-cellulose has good adhesion to skin when used, and the hydrogel immersed in cosmetic lotion and medicines has an effect of penetrating the active ingredient deep into the skin to improve the moisturizing property. Can be utilized.

FIG. 1 is a process diagram showing each step of a method for producing a hydrogel according to the present invention.
2 is a photograph of (a) the hydrogel according to Example 1 and (b) the hydrogel according to Comparative Example 1. Fig.

As shown in FIG. 1, the method for producing a bio-cellulose-containing hydrogel according to the present invention comprises the steps of: (a) preparing a bio-cellulose by adding a strain to a culture solution containing coconut juice and fermenting the same; (b) pulverizing the bio-cellulose produced in step (a); And (c) mixing the pulverized bio-cellulose of step (b) with an aqueous solution containing polyvinyl alcohol, carrageenan and xanthan gum to prepare a hydrogel.

Step (a) is a step of adding a strain to a culture solution containing coconut juice and fermenting to produce bio-cellulose.

The culture solution may contain 50 to 90% by weight of coconut juice.

When the coconut juice is less than 50% of the total weight of the culture liquid, the bio-cellulose production efficiency is inferior and it is difficult to obtain the bio-cellulose in which the effect of the active ingredient in the coconut is exhibited. When the content is more than 90% Since the mixing ratio is not appropriate and it may be difficult to produce bio-cellulose, it may be composed of 50 to 90% by weight.

Natural or synthetic components can be appropriately selected and mixed in the culture broth so that a hydrogel suitable for the intended use can be produced. For example, when the potato extract, cucumber juice, and aloe juice are added to the culture solution, bio-cellulose containing ascorbic acid can be produced and whitening effect can be obtained.

In this step, a sugar or a sugar-containing substance may be additionally added to the culture liquid to improve bio-cellulose productivity through fermentation with the microorganism.

The strains used for producing the bio-cellulose may be selected from the group consisting of acetobacterium, Rizobium genus or Agrobacterium genus, either alone or in combination. Preferably, the strains are selected from the group consisting of xanthium in the genus Acetobacter, And lactic acid bacteria producing bacteriocin may be mixed and cultured to produce bio-cellulose.

In addition, when the strain is cultured in the culture liquid, the pH of the culture liquid may be regulated so as to further improve the productivity of the bio-cellulose by the strain.

For example, it is preferable that the pH of the culture medium is adjusted to a range of 3 to 7 by appropriately mixing acetic acid in the culture of the strain so that the growth of the strain is maintained smoothly. More preferably, the pH of the culture medium is adjusted to pH 4.5 . &Lt; / RTI >

In addition, bio-cellulose can be manufactured by various known micro-organism culturing methods to increase the growth of the microorganisms, and examples thereof include stirring culture, shaking culture, and stationary culture, but the present invention is not limited thereto, And the environment is kept constant at 25 to 35 DEG C to improve the productivity of bio-cellulose by microorganisms.

When the coconut juice is fermented by fermentation with a microorganism under the above conditions, bio-cellulose is produced in the form of a translucent film on the culture liquid. The bio-cellulose produced as described above can be obtained through the extinction of the injected strain and the removal of the culture medium And may be configured to remove microorganisms remaining in the bio-cellulose by irradiating ultraviolet rays (UV) to the obtained bio-cellulose or washing with hot water.

The above-described ultraviolet irradiation is effective as a method of sterilizing the strains remaining in the bio-cellulose because it changes the intracellular nucleic acid such as bacteria and fungi to cause an obstacle to metabolism and loses its proliferative capacity and kills it.

Step (b) is a step of pulverizing the bio-cellulose produced in step (a).

The bio-cellulose may be pulverized using a wet pulverizer and may be pulverized to an average particle size of 4 to 5 탆 in order to ensure uniform dispersion in an aqueous solution containing a hydrophilic polymer to be described below.

Step (c) is a step of mixing and coagulating the pulverized bio-cellulose of step (b) with an aqueous solution containing polyvinyl alcohol, carrageenan and xanthan gum to prepare a hydrogel, which is configured to add polyvinyl alcohol, carrageenan and xanthan gum Thus, a hydrogel in which the tensile strength is remarkably improved due to an increase in viscosity can be produced.

Polyvinyl alcohol is effective as a binder, a film forming agent and a water-soluble thickener, and can be used for hydrogels.

Carrageenan, a hydrophilic natural polymer, is a polysaccharide that has antimicrobial and immunity-enhancing properties and is effective as a gelling agent, stabilizer for drugs and cosmetics, and can be used in hydrogels. There is almost no change in viscosity due to xanthan gum, alkali, salts and the like, and it has an effect of filming, gelation and moisturizing effect and can be used in hydrogels.

In addition, natural polysaccharides can be added to the hydrogel in this step so as to obtain the desired physical properties and effects. For example, black pepper can be used in hydrogels with the effect of imparting a black emulsion stabilizer, a water-soluble thickener, and a fragrance. It can be used for hydrogels because it has the effect of increasing the viscosity of black guar, improving emulsion stability and improving physical properties and feel. Agar is effective as a stabilizer to increase the viscosity and prevent pigment and additives from precipitating and can be used in hydrogels.

In order to prepare the hydrogel, the pulverized bio-cellulose is preferably contained in an amount of 0.1 to 20% by weight, more preferably 1 to 15% by weight, and most preferably 1 to 5% by weight based on the total weight of the hydrogel To prepare a hydrogel.

As described above, the reason why the added amount of bio-cellulose is limited is that when the bio-cellulose is used in an amount of less than 0.1% by weight, it is difficult to expect an effect of improved tensile strength and moisturizing property. It is not easy to handle, and bio-cellulose can be added in such a composition range.

The polyvinyl alcohol is preferably contained in an amount of 0.01 to 30% by weight, more preferably 0.01 to 20% by weight, and most preferably 0.06 to 20% by weight based on the total weight of the hydrogel.

If the concentration of the polyvinyl alcohol aqueous solution is less than 0.01 wt%, there is a problem that a hydrogel having too low physical properties is formed. When the concentration is more than 30 wt%, the viscosity of the prepared solution is too high, .

The aqueous hydrophilic natural polymer may be contained in an amount of preferably 0.1 to 10% by weight, more preferably 0.1 to 8% by weight, and most preferably 0.1 to 5% by weight based on the total weight of the hydrogel.

More specifically, an aqueous solution was prepared by adding 0.06% by weight of polyvinyl alcohol, 0.935% by weight of carrageenan, 0.7% by weight of xanthan gum, 0.814% by weight of carob bean gum, 0.07% by weight of guar gum and 0.07% by weight of agar based on the total weight of the hydrogel can do.

When the hydrophilic natural polymer is used in an amount of less than 1% by weight, the resulting hydrogel has poor mechanical properties and is easily broken down. When the hydrophilic natural polymer is used in an amount of more than 5% by weight, There is a problem that the hydrogels are not uniformly produced because the polymers are not uniformly mixed.

In addition, in this step, a hydrogel may be additionally prepared by adding natural cellulose having binding stability, emulsification stability and viscosity increasing effect to improve the mechanical properties of the hydrogel.

For example, hydrogels can be prepared by additionally including cellulose such as hemicellulose, lignin, and carboxymethylcellulose.

In addition, in this step, additives such as a hydrophilic natural or synthetic polymer and a viscosity increasing agent capable of obtaining the physical properties and effects required for the hydrogel may be additionally provided so that a hydrogel which can be used for various purposes can be manufactured.

For example, a hydrogel can be prepared by including a hydrophilic polymer such as hyaluronic acid, alginic acid, chitosan, collagen, gelatin, and polyvinylpyrrolidone.

The hydrophilic polymer has excellent solubility in water, and has effects such as viscosity and adsorption, and can be included to produce a hydrogel according to the application.

The viscosity increasing agent may be exemplified by potassium chloride. More specifically, potassium chloride may be contained in an amount of 0.035% by weight based on the total weight of the hydrogel.

As another example, the composition may further be configured to include additives such as a moisturizing agent, a surfactant, and an antiseptic to further improve the physical properties of the hydrogel.

As the moisturizing agent, squalene, glycerin, glucose and the like can be exemplified, and the hydrogel can supply the oil and nutrition to prevent the skin from being dried.

More specifically, the hydrogel may contain 0.035% by weight of glucose based on the total weight of the hydrogel.

In this step, in order to produce the hydrogel, a crosslinking agent may be added to an aqueous solution containing polyvinyl alcohol, carrageenan and xanthan gum to form a resilient and chemically stable hydrogel.

The cross-linking agent may be an acrylic cross-linking polymer, a styrene-based copolymer or a mixture thereof. The cross-linking agent is preferably 0.01 to 10% by weight, more preferably 0.03 to 10% by weight, based on the total weight of the hydrogel .

When the crosslinking agent is used in an amount of less than 0.01% by weight, a viscosity change occurs when the hydrogel is applied to the skin, causing the hydrogel to flow down from the skin. When the crosslinking agent is used in an amount of more than 10% by weight, Or the medicament is difficult to be filled in the hydrogel.

The present invention provides a hydrogel produced by the method described above.

Also provided is a cosmetic mask pack comprising a hydrogel prepared by the above-described method as a support.

The hydrogel thus prepared may be molded into a desired shape and immersed in a cosmetic lotion to prepare a cosmetic mask pack, which may be sealed to produce a final product.

A drying process can be performed to make the hydrogel in a certain water holding state before impregnating the lotion. The water content may be maintained at a weight of 1 to 50 times the dry weight of the hydrogel, then the lotion may be added, and most preferably, the moisture content within the weight range of 10 to 20 times the dry weight may be maintained.

When the moisture content of the hydrogel is less than the same weight as the dry weight of the hydrogel, swelling time of the mask is prolonged, swelling is insufficient and the lotion can not be sufficiently washed out and soft feeling is not obtained. If it carries moisture, it can not function as a cosmetic mask pack because it can not drain any further lotion.

The present invention also provides a dressing comprising a hydrogel prepared by the above-described method as a support.

The hydrogel thus prepared may be molded into a desired shape and immersed in a chemical to prepare a wet dressing agent, and the step of sealing to produce a final product.

For example, a hydrogel immersed in an aqueous solution containing betaglucan is effective for the treatment of skin regeneration because it absorbs body fluids, prevents infection from bacteria, is easy to adhere to wounds and skin, has transparency and ease of handling, It can be applied as wound dressing dressing.

Hereinafter, the present invention will be described in more detail with reference to preferred embodiments. The embodiments presented are only a concrete example of the present invention and are not provided for the purpose of limiting the scope of the present invention.

Example 1. Preparation of hydrogel

The hydrogel according to the present invention was prepared through the following steps.

Acetobacterium xylinum was inoculated on a medium containing 10 g / L of glucose, 10 g / L of yeast extract, 7 g / L of peptone, 0.2 g / L of succinic acid and 1.5 mL / L of acetic acid, . To make the culture solution, 500 g of coconut juice and 50 g of fructose were boiled at 100 ° C for 30 minutes, mixed well, and cooled to about 30 ° C at room temperature. 20 ml of the acetobacterium xylenium microorganism solution, which had been cultured in 300 ml of the prepared culture, was added and the mixture was allowed to stand for about 15 days while being maintained at 28 ° C. After 15 days, the bio-cellulose produced at 15 mm or more was obtained and washed and sterilized using hot water.

The washed and sterilized bio-cellulose was finely cut, finely ground with a grinder, and washed twice with distilled water.

1 g of bio-cellulose, 0.06 g of polyvinyl alcohol, 0.935 g of carrageenan, 0.7 g of xanthan gum, 0.814 g of carob bean gum, 0.07 g of guar gum, 0.07 g of agar, 0.035 g of potassium chloride, 0.035 g of glucose, 0.03 g of styrene / g, and 96.251 g of purified water were stirred at 60 占 폚. The homogenized solution was molded into a mold, cooled at room temperature, and aged at 50 캜 for 13 hours to prepare a hydrogel as shown in Fig. 2 (a).

Example 2.

A hydrogel was prepared in the same manner as in Example 1 except that 3 g of the bio-cellulose was used.

Example 3.

A hydrogel was prepared in the same manner as in Example 1, except that 5 g of the bio-cellulose was used.

Comparative Example 1

A hydrogel as shown in Fig. 2 (b) was prepared in the same manner as in Example 1, except that it did not contain bio-cellulose.

Test Example 1. Analysis of Physical Properties of Hydrogel

(1) Measurement of gelation rate

The gelation ratios were measured in order to analyze the tensile strengths of the hydrogels prepared according to Examples 1 to 3 and Comparative Example 1.

The hydrogel was cut to a size of about 1.3 x 1.3 cm and dried in a vacuum oven to a constant weight. Each sample was placed in a 100 ml bottle and filled with purified water. The bottles were placed in a shaking water bath and run at 37 DEG C and 60 rpm for 48 hours. The specimens were then removed from the bottle and placed in a vacuum oven, dried to constant weight, and the weight of the dried gel was measured. The gel content of the hydrogel was calculated using the following equation (1). The results are shown in Table 1.

[Formula 1]

(Where W _i is the weight of the originally dried specimen, and W _d is the weight of the extracted and dried specimen)

Example 1 Example 2 Example 3 Comparative Example 1 Gelation rate (%) 60.57 65.74 68.25 57.24

As shown in Table 1, it can be seen that the more the bio-cellulose is contained in the hydrogel, the higher the gelation rate and the higher the degree of crosslinking, thereby improving the tensile strength. As a result, hydrogels with improved tensile strength can be produced, and hydrogels suitable for use as cosmetic mask packs, dressings and external preparations for skin can be produced.

(2) Tensile strength

The hydrogels prepared in Examples 1 to 3 and Comparative Example 1 were tested for their mechanical properties.

The tensile strength of the hydrogel was measured using INSTRON series IX (Instron Co, Universal Testing System Model 5569, USA). The hydrogel was cut into 4 × 5 cm wide and 3.0 to 3.5 mm thick. Were measured. The results are shown in Table 2.

Example 1 Example 2 Example 3 Comparative Example 1 Tensile strength (Kgf / cm ² ) 0.59 0.72 0.95 0.30

As shown in Table 2, it can be seen that the more the bio-cellulose is contained in the hydrogel, the higher the intensity of the phosphorus is in proportion to the gelation rate. It can be confirmed that the hydrogel having the above-mentioned tensile strength can be used for attaching skin such as a cosmetic mask pack and a dressing agent.

(2) Measurement of water absorption rate

The water absorption rate was measured in order to analyze the performance of the hydrogel prepared according to Examples 1 to 3 and Comparative Example 1 as an external preparation for skin.

The prepared hydrogel was cut into a size of 1.3 x 1.3 cm, placed in a weighing dish, and poured into purified water. After immersing for 48 hours, the weight of the hydrogel was measured. The water absorption rate of the hydrogel was calculated using the following Equation 2, and the results are shown in Table 3.

[Formula 2]

(Where W _i is the weight of the initial sample, and W _s is the weight of the swollen sample)

Example 1 Example 2 Example 3 Comparative Example 1 Water Absorption Rate (%) 48.91 47.12 45.57 50.43

As shown in Table 3, as the hydrogel contains much bio-cellulose, the water absorption rate is decreased, and it can be confirmed that the gelation rate is inversely related to the gelation rate.

The higher the degree of crosslinking of the hydrogel, the smaller the internal structure of the gel, the smaller the space in which water can be contained, and the lower the water absorption rate.

However, the hydrogel according to Examples 1 to 3 has a water absorption rate that is not much different from that of Comparative Example 1, so that sufficient lotion and medicines can be dewatered, and sufficient ingredients can be supplied to the skin.

Test Example 2. Sensory Evaluation on the Usability of Hydrogel

Sensory tests were conducted to analyze the feeling of use of the hydrogels prepared according to Examples 1 to 3 and Comparative Example 1.

Thirty subjects were selected, and the hydrogels were used, and then the average value of the hydrogels was calculated by repeating two rounds of the 5-point scoring method for the feeling of adhesion, softness, moisturizing feeling after use, and overall satisfaction.

The results of the sensory evaluation of the hydrogel according to the present invention are shown in Table 4 below.

Example 1 Example 2 Example 3 Comparative Example 1 A sense of closeness 4 points 4 points 5 points 3 points Softness 5 points 4 points 4 points 5 points After use 3 points 4 points 5 points 2 points Overall satisfaction 4 points 5 points 5 points 3 points Total score 16 points 17 points 19 points 13 points

As shown in Table 4, as the hydrogel contains a large amount of bio-cellulose, the adhesiveness and moisturizing feeling after use are high, and the overall satisfaction is high, so that the hydrogel can be efficiently used for manufacturing a skin external preparation such as a cosmetic mask pack or a wet dressing It is possible to confirm that it is possible.

Claims

(a) adding a strain to a culture solution containing coconut juice and fermenting to produce bio-cellulose;
(b) pulverizing the bio-cellulose produced in step (a); And
(c) mixing and coagulating the bio-cellulose pulverized in step (b) with an aqueous solution containing polyvinyl alcohol, carrageenan and xanthan gum to prepare a hydrogel
Wherein the bio-cellulose is a biodegradable polymer.

The method of producing a hydrogel according to claim 1, wherein the culture liquid of step (a) comprises 50 to 90 wt% of coconut juice.

The method according to claim 1, wherein the strain of step (a) is at least one selected from the group consisting of genus Acetobacter, Rhizobium genus and Agrobacterium genus.

The method of manufacturing a hydrogel according to claim 1, wherein the bio-cellulose of step (c) is contained in an amount of 0.1 to 20% by weight based on the total weight of the hydrogel.

The method of claim 1, wherein the hydrogel of step (c) comprises a crosslinking agent.

A hydrogel prepared by the method according to any one of claims 1 to 5.

A cosmetic mask pack comprising the hydrogel of claim 6 as a support.

A dressing agent comprising the hydrogel of claim 6 as a support.