KR20180115070A - Manufacturing method of freeze-drying collagen solution for cosmetic compositions - Google Patents

Abstract

The present invention relates to a method for manufacturing a freeze-drying collagen solution, and more specifically, comprises: a step (a) of dissolving collagen in purified water to manufacture a collagen dissolving liquid; a step (b) of dissolving a thickener in the purified water to manufacture a thickener dissolving liquid; a step (c) of dissolving a functional composition for improving skin condition in the purified water to manufacture a functional dissolving liquid; a step (d) of mixing the collagen dissolving liquid in the step (a) with the thickener dissolving liquid in the step (b); a step (e) of mixing the mixed solution of the step (d) with the functional dissolving liquid in the step (c); a step (f) of injecting the mixed solution of the step (e) in a container to be freeze-dried; and a step (g) of packing the freeze-dried material of the step (f). The present invention prevents collagen from being gelatinized such that natural physical properties are maintained, accommodation and distribution are easy, and any preservative treatment is not necessary. In addition, the present invention is conveniently used as a cosmetic composition.

Description

Technical Field [0001] The present invention relates to a freeze-dried collagen solution for cosmetic composition,

The present invention relates to a method for producing a freeze-dried collagen solution for a cosmetic composition, and more particularly, to a method for producing a freeze-dried collagen solution for a cosmetic composition, which comprises preparing a collagen solution for a cosmetic composition in a lyophilized state to prevent gelatinization of the collagen, And to a method for producing a freeze-dried collagen solution for a cosmetic composition.

Collagen is a light protein that is widely distributed in multicellular animals such as invertebrates and vertebrates, and is found most quantitatively. It is a type of fibrous protein composed of proline, oxyproline, glycine, and glutamic acid. It is a protein with the shape of a slender band.

In mammals, it accounts for approximately one-quarter of the total protein, and is a protein consisting of amino acids that make up the bones and skin. Especially, it is mainly found in membranes wrapping organs in human body, articular cartilage, eye cornea, bones and skin. It plays a very important role as a constituent of the dermis layer in the skin.

Collagen is presently known to be about 20 kinds, collagen type 1 being the most, morphologically being present as fibrous solid, three-stranded polypeptide having a twisted structure by hydrogen bonding, molecular weight of about 300 kDa to be.

Collagen is dissolved in dilute acid or dilute alkali and can be prepared in liquid form. The higher the concentration, the higher the viscosity. Collagen is suitable for living tissue and is a biodegradable material and is widely used as a medical material such as a tissue restorative material, a skin graft material, a bone graft material, a cell culture, an additive for a cosmetic composition, and a raw material for a health food.

On the other hand, since collagen extracted from various raw materials is prepared in a liquid phase, the collagen produced in the liquid phase should be filtered to remove foreign substances and microorganisms. Therefore, in order to filter collagen, which is a polymer protein, it should be prepared in a low concentration liquid phase. Especially, in case of microfiltration to remove microorganisms, a concentration of less than about 5 mg / mL for permeating a filtration membrane having a small pore size of 0.2 to 0.45 micrometer .

Therefore, collagen for cosmetic compositions in the past has been stored and distributed in a low concentration, or has been stored and distributed at a high concentration of collagen at a low concentration.

However, when stored and distributed in the liquid state as described above, the storage and distribution costs are increased, and the gelatinization proceeds rapidly, and the collagen can not be used for its original purpose. However, There is a disadvantage in that a separate preservative must be mixed for reasons such as the above.

In addition, the low-concentration collagen solution has been circulated in powder form by vacuum drying or lyophilization, and powdered collagen is also mixed with another preservative because of bacterial infection or the like. In addition, such powdery collagen has been used as a cosmetic composition, mixed with a solvent such as purified water, and then mixed with a functional composition for improving skin condition after being made into a liquid form. In addition, the functional composition for improving the skin condition was also mixed with preservatives because of bacterial infection, and stored and distributed. As a result, there was a bad effect on the skin due to the preservative.

KR 10-1105603 B1

An object of the present invention is to solve the problems of conventional collagen processed in a liquid or powder form and to prevent gelatinization of collagen by freeze-drying a collagen solution mixed with a functional composition for improving skin condition, To keep the composition as it is, to improve the functionality and utility as a cosmetic composition, and to extend the storage period without using preservatives to facilitate storage and distribution.

In order to accomplish the above object, the present invention provides a method for preparing a lyophilized collagen solution, comprising the steps of: (a) dissolving collagen in purified water to prepare a collagen solution; (b) dissolving the thickener in purified water (C) dissolving a functional composition for improving skin condition in purified water to prepare a functional dissolving liquid; and (d) dissolving the collagen solution of step (a) and the step (E) mixing the functional liquid of step (c) with the liquid mixture of step (d), and (f) injecting the mixed liquid of step (e) And (g) packing the lyophilized product of step (f), wherein the functional composition for skin condition improvement is selected from the group consisting of vitamin, hyaluronic acid, peptide, arbutin, horse bone extract, horse placenta extract, One or more of the powders And it characterized in that.

The collagen is at least one kind selected from the group consisting of bovine, porcine and marine collagen, and the enhancer is at least one of alginic acid, glycerin, cellulose, xanthan gum and agar gum.

The collagen, the thickening agent and the functional composition are used in a weight ratio of 1: 0.001 to 0.1: 0.1 to 0.5.

The functional composition for improving skin condition comprises vitamin, hyaluronic acid, peptide, arbutin, horse bone extract, horse placenta extract, and floss powder.

In the step (e), the bamboo shoot extract and the daughter-in-law's belly extract are further mixed.

According to the present invention, gelatinization of collagen is prevented, original physical properties are maintained, storage and distribution are easy, and separate preservative treatment is unnecessary.

Further, it has an advantage that it can be easily used as a cosmetic composition.

BRIEF DESCRIPTION OF THE DRAWINGS Fig. 1 is a view showing a manufacturing procedure of a lyophilized collagen solution according to the present invention. Fig.

Hereinafter, the present invention will be described in detail with reference to the accompanying drawings.

A method for producing a lyophilized collagen solution for a cosmetic composition according to the present invention comprises the steps of (a) dissolving collagen in purified water to prepare a collagen solution, (b) dissolving the thickener in purified water, (C) dissolving the functional composition for improving skin condition in purified water to prepare a functional dissolving liquid; and (d) dissolving the collagen dissolving solution in step (a) and the gradually dissolving solution in step (E) mixing the functional liquid of step (c) into the mixed liquid of step (d), and (f) injecting the mixed liquid of step (e) And (g) packing the lyophilisate of the step (f).

That is, the present invention relates to a method for improving skin condition by freeze-drying a collagen solution containing the functional composition for improving skin condition, thereby preventing collagen gelatinization and deterioration, preventing bacterial infection, prolonging the storage period, will be.

Hereinafter, the manufacturing method of the present invention will be described step by step with reference to FIG.

(a) In purified water  Collagen Dissolve  A step of preparing a collagen solution.

First, collagen is added to purified water and dissolved in a high-speed mixer at 5,000 to 10,000 rpm for 10 to 60 minutes to prepare a collagen solution. At this time, the concentration of the collagen solution is preferably about 0.1 to 10%. If the concentration is too high, dissolution and mixing with other ingredients are not easy because of excessive amount.

The collagen may be at least one selected from the group consisting of bovine, porcine, and marine-derived collagen. The collagen may be in the form of a liquid or a low concentration concentrated by extraction or filtration, Or may be a lyophilized powdery phase, without limitation. However, the collagen used in the present invention should be one in which no preservatives are mixed.

(b) In purified water Increasing agent Dissolve Incrementer  A step of preparing a dissolution liquid.

Separately from the step (a), an increasing agent is added to purified water and dissolved in a high-speed mixer at 5,000 to 10,000 rpm for 30 to 90 minutes to prepare a gradual solution. At this time, the concentration of the gradual solution is preferably about 0.1 to 10%.

At least one of alginic acid, glycerin, cellulose, xanthan gum and agar gum is used as the above-mentioned incrementing agent because the above-mentioned thickening agent is a substance having excellent skin safety.

The reason for using the thickening agent in the present invention is to increase the viscosity of the dissolving solution of the collagen solution and the functional composition to be described later through the thickening agent to facilitate lyophilization and to improve usability as a cosmetic composition.

(c) In purified water  A functional composition for improving skin condition Dissolve  A step of producing a functional dissolution liquid.

Next, the functional composition for improving skin condition is added to purified water and dissolved in a high-speed mixer at 5,000 to 10,000 rpm for 10 to 60 minutes to prepare a functional dissolution solution. At this time, the concentration of the functional dissolution liquid is preferably about 0.1 to 10%.

In the present invention, the functional composition for improving skin condition means a composition having an effect of improving the skin condition, and preferably at least one of vitamin, hyaluronic acid, peptide, arbutin, horse bone extract, horse placenta extract, And more preferably vitamin, hyaluronic acid, peptide, arbutin, horse bone extract, horse placenta extract, and floss powder.

In the present invention, by lyophilizing the functional composition for improving skin condition together with the collagen, it is convenient to use as a cosmetic composition and also it is possible to distribute the functional composition without using a preservative. In addition, the skin condition is remarkably improved through interaction between the collagen and the functional composition, and the collagen can be stably stored due to the functional composition having anti-inflammatory and antibacterial functions.

It is preferable to use vitamin C and vitamin E as one of the above-mentioned functional compositions. This is because the vitamin C is an antioxidant that protects the body from active oxygen and prevents collagen deterioration, and vitamin E prevents skin aging. Also, since vitamin E helps the skin to absorb vitamin C, it is preferable to use vitamin C and vitamin E together at a ratio of 1: 0.5 ~ 1 weight ratio.

And the hyaluronic acid keeps moisture on the skin and softens the skin. When used with collagen, it nourishes and replenishes the collagen, which significantly improves skin elasticity.

The peptide enhances elasticity and imparts vitality and vitality to the skin. Specifically, it is possible to use SIE-polypeptide-11 or the like.

Arbutin is a functional whitening ingredient and inhibits the activity of tyrosinase in the step of producing melanin pigment to inhibit the production of excessive melanin pigment.

The horse bone extract has an effect of nourishing the skin and alleviating skin texture, and the horse placenta extract has an effect on spots and the like and can be extracted by the steam distillation method. Illustratively, the horse bone or horse placenta is cut to a size of 5 to 10 cm, and the cut horse or horse placenta is immersed in purified water at 10 to 20 ° C for 2 to 3 hours to remove the blood, and then washed with purified water. Then, the washed horse bone or horse placenta is poured into the extractor together with purified water (2 to 20 times the total weight of the injected horse bone or horse placenta), and the extractor is hermetically sealed and heated at a temperature of 120 to 150 ° C. and 2 to 3 kgf / Cm < 2 > for 48 to 55 hours, and the extractor is further heated for 5 to 8 hours at a pressure of 3 to 4 kgf / cm2 to open the steam outlet connected to the extractor in units of 20 to 40 minutes, The steam is discharged. And liquefying and collecting the discharged steam. The liquefied and collected extract is lyophilized to produce powder.

The floss powder improves skin wrinkles and elasticity, and the floss powder means freeze-dried and pulverized.

In the present invention, as the functional composition, 10 to 15% by weight of the vitamin, 10 to 15% by weight of hyaluronic acid, 10 to 15% by weight of peptide, 10 to 15% by weight of arbutin, 10 to 15% by weight of horse bone extract, By weight and 10-15% by weight of the floss powder are preferably used because these compositions have the best effect for improving the skin condition.

In addition, the particle size of the above-mentioned powder materials is not limited, but it may be sufficient to be used in purified water. And may be, for example, about 100 to 300 mesh.

(d) dissolving the collagen solution of step (a) and the collagen solution of step Incrementer  Mixing the dissolution liquid.

Next, the increasing solution of step (b) is added to the collagen solution of step (a), and the solution is sufficiently mixed at 5,000 to 10,000 rpm for 10 to 60 minutes using a high-speed mixer.

(e) mixing the functional solution of step (c) into the mixed solution of step (d).

Then, the functional solution of step (c) is added to the mixture of step (d) and mixed thoroughly at 5,000 to 10,000 rpm for 10 to 60 minutes using a high-speed mixer.

(f) injecting the mixed liquid of step (e) into a container and freeze-drying the mixture.

Next, the mixed solution of step (e) is injected into a container using an injector, frozen at -80 to -50 ° C for 10 to 24 hours, and then dried in a freeze dryer for 72 to 90 hours. Here, the vacuum state does not mean a complete vacuum, but it is sufficient if it is dried under the pressure of freeze-drying.

At this time, the size and shape of the container are irrelevant, and the kind of the container is not limited as long as it is a container capable of being packed after being injected with the mixed solution of the step (e) and freeze-dried.

(g) packing the lyophilisate of step (f).

Next, the lyophilizate in step (f) is quickly packed to block moisture in the air, thereby completing the preparation of the lyophilized collagen solution.

In the present invention, the collagen, the thickeners and the functional compositions are preferably used in a weight ratio of 1: 0.001 to 0.1: 0.1 to 0.5, and as long as they are used as such a compounding ratio, they can exhibit excellent effects as a cosmetic composition, .

The collagen solution prepared by the above method is water-soluble and easily dissolved in water, so that it can be easily used as a cosmetic composition, and is safe from microorganisms, so that there is no need for a separate preservative treatment. In addition, there is no deterioration of collagen and the original purpose and effect are not deteriorated, and there is an advantage that various functionalities can be utilized as cosmetics because of the lyophilized functional ingredients.

In other words, in the simplest case, the collagen solution can be used by dissolving the collagen solution in a skin, an emulsion or an essence which is conventionally used by a consumer. For example, the cosmetic cotton is sufficiently wetted with the skin, and then a collagen solution is slightly sprayed or applied Can be used.

In addition, it can be used as a raw material for various other cosmetics, and can be included in various kinds of known cosmetic compositions as well as mask packs, skins, essences, emulsions and creams. Here, the use amount of the collagen solution of the present invention can be used in the range of 1 to 99% by weight based on 100% by weight of the cosmetic composition, and its use is not limited.

Meanwhile, in the step (e) of the present invention, the bamboo shoot extract and the daughter-in-law's extract may be further mixed. At this time, it is preferable that the functional composition, the bamboo shoot extract and the daughter-in-law's extract are 0.1 to 0.5: 0.01 to 0.05: 0.01 to 0.05 weight ratio.

In the present invention, the bamboo shoot extract imparts an antioxidative effect to improve the shelf life of the collagen solution, as well as to improve the skin wrinkles. Also, the above-mentioned daughter-in-law's belly extract has an excellent antimicrobial effect, which improves the storage stability of the collagen solution and protects the skin by reducing the incidence of skin diseases caused by skin bacteria and other bacteria.

The bamboo shoot extract or daughter-in-law's extract may be obtained by extracting the extract from a liquid phase obtained by cold-pressing or warm-extracting with water or ethanol as a solvent, and evaporating or lyophilizing the solvent.

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

(Example 1)

Small collagen was dissolved in purified water to prepare a 10% collagen solution. Then, glycerin was dissolved in purified water to prepare a gradual solution of 5% concentration. Next, 15% by weight of vitamin C, 5% by weight of vitamin E, 15% by weight of hyaluronic acid, 15% by weight of S-PE polypeptide-11, 15% by weight of arbutin, 15% by weight of horse bone extract, And 15% by weight of a red flour powder was dissolved to prepare a functional dissolution liquid having a concentration of 10%. The collagen solution and the gradual solution were mixed, and then the functional solution was mixed again. Then, it was poured into a stainless steel container at a height of 3 cm, frozen at -50 ° C for 24 hours, dried in a freeze dryer for 72 hours, and immediately packed.

At this time, horse bone extract and horse placenta extract were prepared as follows. The horse bone or horse placenta was cut to a size of 5 cm and the cut horse bone or horse placenta was immersed in purified water at 15 ° C for 2 hours to remove the blood and then washed with purified water. Then, the washed horse bone or horse placenta was poured into the extractor together with 10 times by weight of purified water, and the extractor was closed. Then, the extractor was heated at a temperature of 130 ° C and a pressure of 2 kgf / cm 2 for 50 hours. The steam outlet connected to the extractor was opened in units of 30 minutes while being further heated at the pressure for 5 hours to discharge the steam to the outside. Then, the discharged steam was liquefied and collected, and was freeze-dried to prepare a 200-mesh powder.

And, the red pepper powder was prepared by lyophilization and crushing at 200 mesh.

The bovine collagen, thickening agent and functional composition were used in a weight ratio of 1: 0.1: 0.5.

(Example 2)

The same procedure as in Example 1 was carried out except that the bamboo shoot extract and the daughter-in-law's womb extract were further mixed when the functional solution was mixed. At this time, the functional composition, the bamboo shoot extract, and the womb-worm extract were 0.5: 0.05: 0.05 weight ratio.

The dried bamboo shoot or daughter-in-law's belly of the bamboo shoot extract or daughter-in-law's belly extract is crushed to a size of about 10 to 50 mesh, and 10 times by weight of water is added thereto and extracted at 50 to 70 ° C for 10 hours , Followed by filtration, lyophilization and pulverization at 200 mesh.

(Test Example 1)

Safety test

The above Examples 1 and 2 were applied once a day to the skin of 40 male rabbits (20 rats per group) with hair on the dorsal skin removed, 5 times a week to 2 mg / cm 2 or more. The application was performed by mixing the purified water with the above-mentioned each example at a weight ratio of 1: 2, and the experiment was performed for 2 weeks, and the removal of the hair was performed on the final application foil every week. The test was performed at 24, 48, and 72 hours after application with the primary irritation test using erythema and edema as an index.

As a result, no erythema and edema were observed in all the experimental groups and it was judged as negative.

(Test Example 2)

After applying the above Examples 1 and 2 to the left side of the face for 12 weeks, moisturizing, anti-inflammatory (acne relief), and anti- (4.5 points) on the right side to evaluate the moisturizing, anti-inflammatory (acne relieving), elasticity, whitening, wrinkle improvement, overall satisfaction as compared with the right side. Here, the left face was mixed with 1: 0.5 weight ratio of Example 1 or 2 provided on the skin that was usually used, and the skin on the right side was used. .

The results are shown in Table 1 below. The test results shown in Table 1 are average values of the respective groups.

Results of Test Example 2. division Moisturizing Anti-inflammatory elasticity Whitening wrinkle improvement Overall satisfaction Example 1 7.2 7.0 7.3 7.6 7.5 7.4 Example 2 7.9 7.5 7.8 8.0 7.6 7.8

As can be seen in the above Table 1, it was confirmed that in all of the examples, moisturizing, anti-inflammation (acne relief), elasticity, whitening, wrinkle improvement and overall satisfaction were significantly higher than the right face (reference 4.5)

While the present invention has been particularly shown and described with reference to exemplary embodiments thereof, it is to be understood that the scope of the present invention is not limited to the disclosed exemplary embodiments. It will also be appreciated that many modifications and variations will be apparent to those skilled in the art without departing from the scope of the present invention.

Claims (5)

(a) dissolving collagen in purified water to prepare a collagen solution,
(b) dissolving the thickener in purified water to prepare an increasing solution,
(c) dissolving the functional composition for improving skin condition in purified water to prepare a functional dissolving liquid,
(d) mixing the collagen lysate of step (a) and the lysing solution of step (b)
(e) mixing the functional solution of step (c) into the mixed solution of step (d)
(f) injecting the mixed liquid of step (e) into a container and freeze-drying the mixture,
(g) packing the lyophilisate of step (f)
Wherein the functional composition for skin condition improving comprises at least one of vitamin, hyaluronic acid, peptide, arbutin, horse bone extract, horse placenta extract, and floss powder.
The method according to claim 1,
The collagen is at least one of bovine, porcine and marine collagen,
Wherein the thickening agent is at least one of alginic acid, glycerin, cellulose, xanthan gum, and agar gum.
3. The method of claim 2,
Wherein the collagen, the thickening agent and the functional composition are used in a weight ratio of 1: 0.001 to 0.1: 0.1 to 0.5.
3. The method of claim 2,
Wherein the functional composition for improving skin condition comprises vitamin, hyaluronic acid, peptide, arbutin, horse bone extract, horse placenta extract, and floss powder.
3. The method of claim 2,
In the step (e)
Wherein the bamboo shoot extract and the daughter-in-law's belly extract are further mixed together to form a freeze-dried collagen solution.

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