KR20160126793A - Cosmetic materials and process for producing the same - Google Patents
Cosmetic materials and process for producing the same Download PDFInfo
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- KR20160126793A KR20160126793A KR1020150058322A KR20150058322A KR20160126793A KR 20160126793 A KR20160126793 A KR 20160126793A KR 1020150058322 A KR1020150058322 A KR 1020150058322A KR 20150058322 A KR20150058322 A KR 20150058322A KR 20160126793 A KR20160126793 A KR 20160126793A
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/64—Proteins; Peptides; Derivatives or degradation products thereof
- A61K8/65—Collagen; Gelatin; Keratin; Derivatives or degradation products thereof
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
- A61K8/73—Polysaccharides
- A61K8/735—Mucopolysaccharides, e.g. hyaluronic acid; Derivatives thereof
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
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Abstract
A cosmetic material containing water-soluble collagen and a hyaluronic acid compound and having a non-crosslinked structure between the water-soluble collagen and the hyaluronic acid compound and being water-soluble and having an apparent density of 0.002 to 0.015 g / cm 3 , and a method for producing the same.
Description
The present invention relates to a cosmetic material and a method for producing the same, and more specifically, to a cosmetic material having excellent shape stability in a dry state and dissolving at a high rate in an aqueous solution, and a method for producing the same.
The skin protects the body from the outside, is responsible for maintaining the homeostasis such as body temperature control and sebum secretion. If the functions of the skin are unbalanced due to external chemical and physical stimulation, stress and nutritional status, and aging, the activity of the cells existing in the skin is lowered, and the constituents of the skin can not maintain the original stable structure, .
Components constituting the skin dermis include cells such as fibroblasts and endothelial cells, and substances constituting an extracellular matrix such as collagen, elastin and fibronectin. These extracellular matrix components form and stabilize the structure of the dermis. When they are abnormally produced or degraded, they affect the structure of the entire skin, resulting in wrinkles and skin elasticity.
Collagen, which is the most noticeable component of wrinkle formation, is also known as light protein or collagen, widely distributed in multicellular animals such as invertebrates and vertebrates, and is the most frequently found light protein. In mammals, it accounts for approximately one-quarter of the total protein, and is a fiber-like, light-weight, light protein that constitutes the connective tissue of animals and transmits power without loss in tendons or ligaments. The basic structural unit of collagen is tropo-collagen with a molecular weight of about 300,000. This molecule has a triple helix structure with three right-handed polypeptide chains. Tropo-collagen molecules are assembled to form collagen fibers (collagen fibers). Each molecule is arranged to be shifted by 1/4 in the axial direction to form a unique stripe of 64 nm intervals. Becomes insoluble. However, if the collagen is boiled for a long time in hot water, dilute acid or dilute alkali, it turns into water-soluble induction protein gelatin. Collagen peptide is a kind of fibrous protein composed of glycine, proline, hydroxyproline, glutamic acid and so on, which is small in amino acid containing sulfur in amino acid. It is a light protein with a shape of long and narrow band of 1,000 amino acids gathered. It is mainly found in the membranes surrounding the body organs, joint cartilage, eye cornea, bones and skin, and plays a very important role as a constituent of the dermis layer in the skin. The main functions of collagen are known as firmness of skin, resistance and binding force of tissue, and support of cell adhesion. Such collagen is known to be closely related to the formation of wrinkles in the skin due to the thinning of the skin due to aging and photoaging due to ultraviolet irradiation.
As income levels rise and aging society, extensive research on skin aging advances, and the function of collagen skin is becoming clear. As collagen metabolism becomes active by promoting collagen synthesis, it is expected that the effect of collagen synthesis stimulating material retinoic acid (retinoic acid ), TGF (transforming growth factor), animal-derived placenta, betulinic acid, and chlorella extract as skin-reinforcing cosmetic compositions.
In addition, many products containing collagen, which is a cosmetic composition for protecting skin, have been sold. However, there is still a problem that it is difficult to expect the moisturizing action of the skin because of the difficulty of transdermal absorption of collagen as a polymer.
There is still a demand for the development of cosmetic materials using collagen, which have improved morphological stability, are easily absorbed by the skin of the body, and have improved moisture and moisturizing properties.
A problem to be solved by the present invention is to provide a cosmetic material excellent in shape stability in a dry state, dissolved in an aqueous solution at a high speed, and improved in moisture retention.
Another object to be solved by the present invention is to provide a method for manufacturing the cosmetic material.
To solve these problems, according to one aspect of the present invention,
A cosmetic material comprising water-soluble collagen and a hyaluronic acid compound and having a non-crosslinked structure between the water-soluble collagen and the hyaluronic acid compound and being water-soluble and having an apparent density of 0.002 to 0.015 g / cm 3 is provided.
The weight ratio of the water soluble collagen and the hyaluronic acid compound may be 70:30 to 90:10.
The water-soluble collagen may be fish-derived collagen.
Wherein the hyaluronic acid compound is selected from the group consisting of hyaluronic acid, sodium hyaluronate, potassium hyaluronate, ammonium hyaluronate, calcium hyaluronate, magnesium hyaluronate, zinc hyaluronate, and cobalt hyaluronate Or more.
The cosmetic material can be dissolved in distilled water at 37 ° C within 10 seconds and the cosmetic material can be dissolved in distilled water at 37 ° C within 5 seconds.
The outer shape of the cosmetic material may be spherical.
Wherein the ratio of the major axis length to the minor axis length of the pores is 2.0 to 10.5, and the ratio of the major axis length to the minor axis length of the pores is in the range of 2.0 to 10.5. Lt; / RTI >
The cosmetic material may be in the form of a porous foam having a surface in the form of a fine fiber.
According to another aspect of the present invention,
Dissolving a water-soluble collagen and a hyaluronic acid compound in water to prepare a solution for a cosmetic material; And
Freezing the solution for the cosmetic material and then drying the solution,
There is provided a method for producing a cosmetic material having a non-crosslinked structure between the water soluble collagen and a hyaluronic acid compound and having a water-solubility and an apparent density of 0.002 to 0.015 g / cm < 3 >.
The weight ratio of the water soluble collagen and the hyaluronic acid compound may be 70:30 to 90:10.
The water-soluble collagen may have a weight average molecular weight of 2,200 Da or more, and the hyaluronic acid compound may have a weight average molecular weight of 100,000 to 2,000,000 Da.
The concentration of the solution for the production of the cosmetic material may be 0.2 to 1.0 w / v%.
The freezing step may be carried out at a temperature of from -5 to -25 < 0 > C.
The freezing step may include a first freezing step at a temperature of -5 to -10 DEG C and a second freezing step at -15 DEG C or less.
The drying step may further include a gamma ray irradiation step.
The gamma ray irradiation dose may be 5 to 30 kGy.
Since the cosmetic material according to one embodiment of the present invention does not require the use of an acidic solution for preparing a solution by including water-soluble collagen, a separate neutralization step or solvent removal step is not necessary and no cross- Water-soluble, has a very fast dissolution rate, and can have an appropriate viscosity which is easy to apply to the skin upon dissolution in cosmetics and the like.
In addition, the cosmetic material of the present invention is excellent in shape stability in a dry state and can be improved in moisture sensitivity and moisturizing property by containing a hyaluronic acid compound. The cosmetic material can be prepared by freeze drying method, It is easy to dissolve and use. It can be free from spoilage and infections caused by microorganisms, and has the advantage of applying fresh cosmetic material directly to skin.
BRIEF DESCRIPTION OF THE DRAWINGS The accompanying drawings, which are incorporated in and constitute a part of the specification, illustrate preferred embodiments of the invention and, together with the description of the invention given below, serve to further the understanding of the technical idea of the invention, And should not be construed as limiting.
1 to 6 are photographs of the cosmetic materials prepared in Examples 1 to 6, respectively.
7 is a graph showing the apparent density of the cosmetic materials produced in Examples 1 to 6. FIG.
8A and 8B are SEM photographs showing the results of observing the cross section of the cosmetic material of Example 1 at 50 magnifications and 100 magnifications, respectively.
12A and 12B (Example 5), Figs. 13A and 13B (Figs. 13A and 13B), Figs. 12A and 12B Example 6) is an SEM photograph of a cross section of a cosmetic material of Examples 2 to 6 at 50 magnifications and 100 magnifications.
14 is a graph showing the short axis length and the major axis length of the pores contained in the cosmetic material prepared in Examples 1 to 6. FIG.
15 is a graph showing the dissolution rate of the cosmetic material prepared in Examples 1 to 6 in distilled water at 37 ° C.
16A is a photograph showing the cosmetic material produced in Examples 1 to 6 after irradiation with a gamma ray.
16B is a comparative graph of dissolution rates in distilled water at 37 DEG C after irradiation of gamma rays of the cosmetic materials prepared in Examples 1 to 6. Fig.
17A to 17C are photographs of the cosmetic materials prepared in Examples 10, 11 and 8.
Figs. 18A to 18C are SEM photographs of the cosmetic material prepared at the freezing temperature of -5 DEG C (Example 10), -10 DEG C (Example 11), and -15 DEG C (Example 8).
19 is a photograph of the cosmetic material produced in Example 12. Fig.
Hereinafter, the present invention will be described in detail. Prior to this, terms and words used in the present specification and claims should not be construed as limited to ordinary or dictionary terms, and the inventor should appropriately interpret the concepts of the terms appropriately It should be construed in accordance with the meaning and concept consistent with the technical idea of the present invention based on the principle that it can be defined.
Therefore, the embodiments shown in the drawings and the drawings described in the present specification are merely the most preferred embodiments of the present invention and do not represent all the technical ideas of the present invention. Therefore, It is to be understood that equivalents and modifications are possible.
According to an aspect of the present invention, there is provided a cosmetic material containing water-soluble collagen and a hyaluronic acid compound, having a non-crosslinked structure between the water-soluble collagen and the hyaluronic acid compound and being water-soluble and having an apparent density of 0.002 to 0.015 g / cm 3 do
Collagen has a characteristic of improving the moisturizing and wrinkle-reducing effect in a specific part of the body including the face, and thus its application as a cosmetic material has been attempted. Conventional collagen is hydrolyzed with strong acid and neutralized with a strong base and then desalted by dialysis or ion exchange. However, since it is difficult to completely remove salts, its use has been restricted not only to cosmetics but also to foods and medicines.
On the other hand, the water-soluble collagen used in the cosmetic material of the present invention does not require the use of an acidic solution in order to prepare a solution, and since a solution can be prepared using water, a separate neutralization step is not necessary, And there is no need to remove the solvent.
Such water-soluble collagen can be obtained, for example, by pulverizing a vegetable, animal or marine origin-derived collagen raw material to a small size (for example, 100 탆 or less) and then subjecting it to pretreatment such as hydrolysis or hot water treatment, Can be.
The marine-origin collagen can be obtained from fish, fish scales, skin, mollusk, crustaceans, marine mammals and the like. In addition, the plant-derived collagen can be obtained by extracting from carrot, red ginseng, pine needle, sesame, top mushroom, oyster mushroom and the like, and animal-derived collagen can be obtained by extracting from pork, wheat, bone and bark.
As the water-soluble collagen, the above-mentioned marine-derived collagen is preferable, and fish-derived collagen is more preferable. Since animal-derived collagen is mainly obtained from a pig skin or bark, there may be safety problems such as mad cow disease, This is because animal problems are sometimes avoided because of problems. In addition, the collagen extracted from fish skins and scales has a small molecular weight, is layered, thin and small, easy to process, and low in molecular weight, so that collagen absorption rate is higher.
The hyaluronic acid compound means hyaluronic acid or an inorganic salt thereof, and is a water-soluble polysaccharide biopolymer having characteristics of high viscosity, moisturizing property, biocompatibility, etc., and is one of the three major components of skin together with collagen and elastin. Hyaluronic acid is a linear, long-chain polymer composed of β-D-glucuronic acid and β-D-N-acetylglucosamine in mutual beta bonds.
Specifically, the hyaluronic acid compound is hyaluronic acid; And one or more of hyaluronic acid inorganic salts such as sodium hyaluronate, potassium hyaluronate, ammonium hyaluronate, calcium hyaluronate, magnesium hyaluronate, zinc hyaluronate, and cobalt hyaluronate, And mixtures of two or more.
The cosmetic material of the present invention contains a water-soluble collagen and a hyaluronic acid compound, and has a non-crosslinked structure without any physical and chemical cross-linking therebetween, thereby exhibiting water solubility. As a result, It can show fast dissolution rate.
The cosmetic material of the present invention may be used in an amount of 0.002 to 0.015 g / cm 3 , preferably 0.003 to 0.014 g / cm 3 , more preferably 0.004 to 0.010 g / cm 3 , still more preferably 0.005 to 0.007 g / cm 3 3 Has an apparent density.
In the present specification, the term "apparent density" refers to a density of the porous body having solid phase portions and pore portions in an object such as powder, particle, fiber form, foam, etc., The volume of the total sum including all of them.
When the apparent density satisfies the above range, the dissolution rate with respect to water is greatly improved, and when dissolved in cosmetics such as essence, it has an appropriate viscosity for application to the skin, and the shape stability can be excellent. 0.002g / cm is less than 3 drops a lot of form stability, if the bulk density is 0.015g / cm 3 greater than the dissolution rate may be decreased.
In the cosmetic material according to an embodiment of the present invention, the weight ratio of the water soluble collagen and the hyaluronic acid compound may be 70:30 to 90:10, more preferably 80:20 to 90:10. When the weight ratio satisfies the above range, excellent morphological stability can be maintained while increasing the collagen content, and it is possible to improve the moisture and moisturizing property upon dissolving in the cosmetic lotion, and it can be quickly dissolved in lotion such as essence.
According to one embodiment of the present invention, the dissolution rate of the cosmetic material may be 10 seconds or less, more preferably 5 seconds or less, in distilled water at 37 占 폚. As a result, the cosmetic material dissolves in distilled water at 37 ° C, which corresponds to the body temperature, within 10 seconds, so that it is possible to prepare the cosmetic material of the present invention in an optimum state for applying the cosmetic material to the body in the shortest time , And can be very conveniently applied as a cosmetic material.
In addition, the cosmetic material according to one embodiment of the present invention may be the result of lyophilization of a solution for a cosmetic material containing water-soluble collagen and a hyaluronic acid compound. When the cosmetic material is the result of lyophilization produced by the freeze-drying method, the cosmetic material is easily stored without denaturing the ingredients of the cosmetic material and can be easily dissolved in an aqueous solution and used, so that it is free from corruption or infection caused by microorganisms And has the advantage of applying fresh cosmetic material directly to the skin.
As a result, the cosmetic material of the present invention can be obtained in various shapes such as a spherical shape, a hexahedron shape, and a tetrahedron shape, depending on the shape of the mold used for freezing the solution.
The cosmetic material may be in a porous form with pores. At this time, the average long axis shortening ratio of the pores may be 1.05 to 10.5, preferably 2.0 to 10.5, more preferably 2.0 to 6.0.
When the pores included in the cosmetic material have such an average short axis ratio, the feel of the natural material can be expressed in various textures, and a fast dissolution rate can be obtained.
The term "long axis" and "short axis" of pores in the present specification mean a line segment having the longest length and a line segment having the shortest length, respectively, among vertical bisectors dividing each pore formed in the cosmetic material into two halves. In this case, the term "average length and shortening ratio of pores" means the ratio of the average major axis length to the average minor axis length of pores, that is, "(average major axis length) / (average minor axis length)".
In addition, the cosmetic material according to one embodiment of the present invention may further include any component such as a skin-beauty-active ingredient and its skin-absorption-promoting ingredient within a qualitative and quantitative range that does not exert an action effect.
Examples of the skin care active ingredient include retinol, arbutin, mulberry extract, licorice extract, raspberry seed extract, chrysanthemum extract, ethyl ascorbyl ether, ascorbyl glucoside, magnesium ascorbyl phosphate, ascorbic acid, kojic acid, glutathione, tyrosinase (AHA), adenosine, stem cells, and botulinum toxin, as well as liposomes, such as, for example, diosmithine, mace lignan, vitamins, asiaticoside, ubidecarenone, peanut extract, polyethoxylated retinamide, hydroxyproline, retinoic acid, And may be any one or more selected from the group consisting of the components.
Examples of the skin absorption promoting component of the skin care active ingredient include phospholipids, phosphatidyls, glycosyl ceramide, fatty acids, nonionic surfactants, sugar fatty acid esters, gels, glycerides, amino sugars, amino acids, glucagon , Glycerin, glutamic acid, polyethylene glycol (PEG), acrylic carnitine, citric acid, menthol, ethyl alcohol, propylene glycol, butylene glycol, ethylene glycol, glycerin and triacetin. Any ingredient effective to promote absorption into the skin is not limited.
According to another aspect of the present invention, there is provided a method for preparing a cosmetic composition, comprising: preparing a solution for a cosmetic material by dissolving a water soluble collagen and a hyaluronic acid compound in water; And a step of freezing and drying the solution for cosmetic material, wherein the cosmetic material has a non-crosslinked structure between the water-soluble collagen and the hyaluronic acid compound and is water-soluble and has an apparent density of 0.002 to 0.015 g / cm 3 / RTI > Hereinafter, a method of manufacturing a cosmetic material will be described in detail.
First, a solution for cosmetic materials is prepared by dissolving a water-soluble collagen and a hyaluronic acid compound in water.
The types of the water soluble collagen and the hyaluronic acid compound are as described above.
Specifically, the water-soluble collagen has a weight average molecular weight of 2,200 Da or more, preferably 2,400 to 9,000 Da, more preferably 2,500 to 5,000, and the weight average molecular weight of the hyaluronic acid compound is 100,000 to 2,000,000 Da, To 1,500,000 Da.
When the weight average molecular weight of the water-soluble collagen satisfies the above range, it is excellent in morphological stability, has water solubility, and can have a fast dissolution rate. In addition, when the weight average molecular weight of the hyaluronic acid compound satisfies this range, it is possible to solve the problem that it is difficult to dissolve or to maintain the morphological stability.
The weight average molecular weight of such water soluble collagen and hyaluronic acid compounds can be measured using gel permeation chromatography (GPC).
The concentration of the cosmetic material solution may be 0.2 to 1.0 w / v%, preferably 0.25 to 0.9 w / v%, more preferably 0.3 to 0.8 w / v%.
In this case, "w / v%" is a unit of the concentration expressed by the weight of the solute contained in the unit volume of the solution. For example, 1.0 w / v% dissolves 1 g of the solute in a solvent to make the total amount to 100 mL Solution.
When the concentration of the solution satisfies the above range, the apparent density of the obtained cosmetic material can be controlled to 0.002 to 0.015 g / cm 3 , the structure of various surfaces can be controlled while maintaining the shape stability, The dissolution rate is greatly improved to such an extent that it dissolves in a short time, and it is suitable for use since it has an appropriate viscosity for application to the skin.
Next, the previously prepared solution for the cosmetic material is frozen and then dried.
At this time, the freezing step may be performed at a temperature of -5 to -25 ° C. When the freezing temperature satisfies the above range, the obtained cosmetic material can be quickly dissolved while maintaining the shape stability, and the shape, size and distribution of the pores can be controlled, and the feel and texture of the natural material can be expressed in various ways have. On the other hand, the rapid freezing method of less than -40 ° C may cause irregular cracking due to the volume expansion upon freezing, and it is difficult to make a cosmetic material having a small pore size and fast melting property.
When the freezing temperature is controlled within the range of from -5 to -25 DEG C, it is possible to realize a form having a relatively small pore size of a smooth surface at a relatively lower temperature, that is, closer to -25 DEG C, That is, the closer the temperature is to -5 ° C, the greater the pore size on the surface of the microfibers. As the average long axis short axis ratio (average major axis length / average short axis length) of the pores becomes larger, for example, when the pore size is 2.0 to 10.5, long pores having a long major axis length are formed to have a fine fiber surface structure, You can visualize the texture.
Further, the freezing step may be carried out by two or more steps having different temperature ranges. For example, the freezing step may comprise a primary freezing step at -5 to -10 ° C and a secondary freezing step at -15 ° C or less. When the temperature of the freezing step is divided into two or more steps, the cosmetic material can be given a natural texture, for example, a microfibre surface in the first freezing step of -5 to -10 ° C, It is possible to increase the morphological stability in the subsequent vacuum drying step by subjecting to a second freezing step at a temperature of, for example, -15 ° C or lower, preferably -15 to -80 ° C, more preferably -15 to -40 ° C .
On the other hand, when vacuum drying is performed immediately after freezing at -5 to -10 ° C, there is a problem that the shape stability of the sample is remarkably lowered because the sample is partially melted and the shape of the surface of the sample is damaged. According to one embodiment of the present invention, after this freezing step, the drying step can be carried out under vacuum at a temperature of 45 ° C or less, and the reason for raising the drying temperature is to dry quickly.
Accordingly, the cosmetic material according to an embodiment of the present invention can be variously manufactured from a sponge or foam form having a smooth surface to a bulky form having a bundle of fine fibers depending on a freezing temperature.
According to an embodiment of the present invention, the drying step may further include a gamma ray irradiation step.
This gamma irradiation step has the effect of sterilizing the cosmetic material directly applied to the skin without using heat or chemicals. In particular, the treatment with gamma irradiation can be carried out even when the cosmetic material is sealed as a final product.
The gamma irradiation may be carried out at an irradiation dose of, for example, 5 to 30 kGy. In addition to the sterilization effect mentioned above, irradiation with the gamma rays may also have the advantage of significantly reducing the molecular weight of the water-soluble collagen or hyaluronic acid compound contained in the cosmetic material, thereby further improving the dissolution rate for cosmetic lotion and the like. In addition, according to one embodiment of the present invention, even if the gamma ray irradiation treatment is performed, the shape stability of the cosmetic material is not affected.
BEST MODE FOR CARRYING OUT THE INVENTION Hereinafter, the present invention will be described in detail with reference to the following examples. However, the embodiments according to the present invention can be modified into various other forms, and the scope of the present invention should not be construed as being limited to the following embodiments. Embodiments of the invention are provided to more fully describe the present invention to those skilled in the art.
Example 1
Soluble collagen (weight average molecular weight: 3,000 Da) and sodium hyaluronate (weight average molecular weight: 1.15 x 10 6 Da) were dissolved in distilled water at a weight ratio of 7: 3 to prepare a cosmetic product having a concentration of 0.2 w / v% Solution was prepared. The weight average molecular weight of the water soluble collagen and sodium hyaluronate was measured using gel permeation chromatography (GPC). The prepared solution was then poured into a uniform spherical mold and frozen at -15 ° C for 24 hours And vacuum-dried at 45 ° C. to prepare a ball-shaped collagen-hyaluronic acid cosmetic material having an average diameter of 13.5 mm. FIG. 1 shows a photograph of the collagen-hyaluronic acid cosmetic material manufactured.
Example 2
A ball-shaped collagen-hyaluronic acid cosmetic material was prepared in the same manner as in Example 1, except that water-soluble collagen and sodium hyaluronate were dissolved in distilled water to prepare a solution for cosmetic material at a concentration of 0.3 w / v% . At this time, a photograph of the manufactured collagen-hyaluronic acid cosmetic material is shown in Fig.
Example 3
A ball-shaped collagen-hyaluronic acid cosmetic material was prepared in the same manner as in Example 1, except that water-soluble collagen and sodium hyaluronate were dissolved in distilled water to prepare a solution for cosmetic materials at a concentration of 0.4 w / v% . At this time, a photograph of the manufactured collagen-hyaluronic acid cosmetic material is shown in Fig.
Example 4
A ball-shaped collagen-hyaluronic acid cosmetic material was prepared in the same manner as in Example 1, except that water-soluble collagen and sodium hyaluronate were dissolved in distilled water to prepare a solution for cosmetic material at a concentration of 0.5 w / v% . At this time, a photograph of the manufactured collagen-hyaluronic acid cosmetic material is shown in FIG.
Example 5
A ball-shaped collagen-hyaluronic acid cosmetic material was prepared in the same manner as in Example 1, except that water-soluble collagen and sodium hyaluronate were dissolved in distilled water to prepare a solution for cosmetic materials at a concentration of 0.8 w / v% . At this time, a photograph of the manufactured collagen-hyaluronic acid cosmetic material is shown in Fig.
Example 6
A ball-shaped collagen-hyaluronic acid cosmetic material was prepared in the same manner as in Example 1, except that water-soluble collagen and sodium hyaluronate were dissolved in distilled water to prepare a solution for cosmetic materials at a concentration of 1.0 w / v% . A photograph of the manufactured collagen-hyaluronic acid cosmetic material is shown in Fig.
Apparent density measurement of cosmetic materials
The weight of the cosmetic material of the collagen-hyaluronic acid compound prepared in Examples 1 to 6 was measured, and the bulk density was determined by calculating the volume. The results are shown in Table 1 and FIG.
That is, the apparent density of the cosmetic material according to the concentration of collagen and hyaluronic acid solution, which is a solution for cosmetic materials used in the freeze-drying, is shown. The concentrations of the solutions used in Examples 1 to 6 were 0.2 w / v%, 0.3 w / v%, 0.4 w / v%, 0.5 w / v%, 0.8 w / v%, and 1.0 w / v%.
(g / cm 3)
Referring to Table 1 and Fig. 7, the apparent density of these cosmetic materials was measured in the range of 0.003 to 0.014 g / cm < 3 >. All of Examples 2 to 6 were well freeze-dried, including Example 1 having the lowest apparent density at 0.00316 g / cm < 3 >
Analysis of microstructure and pore size distribution of cosmetic materials
In order to observe the microstructure and pore size distribution of the cosmetic materials prepared in Examples 1 to 6, each cosmetic material was frozen in liquid nitrogen to cut the cross section, and then the surface was cut into 150 seconds using an ion coater (E-1045) Lt; / RTI > Coated samples were observed at 50 magnifications and 100 magnifications using field emission scanning electron microscopy (FE-SEM, SU 8010). The results of observation of the cross section of the cosmetic material of Example 1 at 50 magnifications and 100 magnifications are shown in Figs. 8A and 8B, respectively. 10A and 10B (Example 3), Figs. 11A and 11B and Figs. 11A and 11B show the results of observing cross sections of the cosmetic materials of Examples 2 to 6 at 50 magnification and 100 magnification, 11a and 11b (Example 4), Figs. 12A and 12B (Example 5) and Figs. 13A and 13B (Example 6).
The shortening of the pores and the length of the major axis of the cosmetic material prepared in Examples 1 to 6 were measured using an image analysis program (Image J), and the short axis length average value, long axis length average value, long axis length And the short axis length (long axis length / short axis length).
Length (㎛)
Length (㎛)
Shortening ratio ratio
14 shows the average value and standard deviation of the short axis length and long axis length of the pores of the cosmetic material according to the concentration of the collagen and hyaluronic acid solution used as a solution for the cosmetic material used in the lyophilization. Were respectively 0.2 w / v%, 0.3 w / v%, 0.4 w / v%, 0.5 w / v%, 0.8 w / v%, and 1.0 w / v%.
Referring to Table 2 and FIG. 14, it was confirmed that the larger the concentration of collagen and hyaluronic acid compound in the preparation, the smaller the pore size and the denser the structure. When the concentration was less than 0.3 w / v% As the ratio increased, the pore shape was also found to be longer in the longitudinal direction. That is, when the cosmetic material is manufactured at a low concentration of 0.3% or less, the pore size is increased, the dissolution rate is increased through the absorption of water, and it is confirmed that the texture of the natural material of collagen and hyaluronic acid compound is better represented Respectively.
Evaluation of dissolution rate of cosmetic material according to concentration of cosmetic material solution
The dissolution rates of the cosmetic materials prepared in Examples 1 to 6 were measured in distilled water at 37 占 폚 and are shown in Fig.
That is, the dissolution rate of the cosmetic material according to the concentration of the collagen and hyaluronic acid solution, which is the solution for the cosmetic material used in the freeze-drying, is shown. The concentrations of the solutions used in Examples 1 to 6 were 0.2 w / v%, 0.3 w / v%, 0.4 w / v%, 0.5 w / v%, 0.8 w / v%, and 1.0 w / v%.
The measurement was performed by stirring 40 mL of distilled water in a 100 mL beaker and measuring the time until the cosmetic material having diameters of about 13.5 mm prepared in Examples 1 to 6 was put in and then completely dissolved. It was confirmed that as the concentration of the solution for cosmetic material decreases, the dissolution time becomes shorter.
Specifically, Examples 1 to 5, which were cosmetic materials made of a solution having a concentration of 0.8% or less, all dissolved within 10 seconds at 37 ° C, and in particular, Examples 1 to 3 Of the solution was dissolved within 5 seconds. From these results, it was found that the dissolution rate of the cosmetic material prepared according to the concentration of the solution for cosmetic material and the temperature upon dissolution can be controlled.
Effect of Dissolution Rate on Gamma Irradiation
Sterilization by gamma irradiation can sterilize the product without using heat or chemicals. The product can be sterilized in a sealed state without a rise in temperature by a gamma ray having strong permeability. In order to confirm whether changes in cosmetic material or change in dissolution rate occurred after irradiation with gamma rays, the cosmetic material prepared in Examples 1 to 6 was irradiated with a dose of 25 kGy, and then the appearance and dissolution rate were measured. 16A, there was no change in appearance of the cosmetic material after the irradiation with the gamma rays, such as the shape and color. Referring to FIG. 16B, when the dissolution rate was measured at 37 ° C, it was confirmed that the dissolution rate was significantly accelerated within 5 seconds compared with that before the irradiation with the gamma ray. This suggests that gamma irradiation may have affected the molecular weight reduction of collagen and hyaluronic acid.
Example 7
Soluble collagen (weight average molecular weight: 3,000 Da) and sodium hyaluronate (weight average molecular weight: 1.15 x 10 6 Da) were dissolved in distilled water at a weight ratio of 9: 1 to prepare 0.75 w / v% Solution was prepared. Then, the prepared solution was poured into a mold having a uniform spherical shape, frozen at -15 DEG C for 24 hours, and vacuum dried at 45 DEG C to prepare a ball-shaped collagen-hyaluronic acid cosmetic material having an average diameter of 13.5 mm. The apparent density of the obtained cosmetic material was 0.0117 g / cm < 3 & gt ;.
Example 8
A ball-shaped collagen-hyaluronic acid cosmetic material was prepared in the same manner as in Example 7, except that the weight ratio of water-soluble collagen to sodium hyaluronate was 8: 2. The apparent density of the obtained cosmetic material was 0.0121 g / cm < 3 & gt ;.
Example 9
A ball-shaped collagen-hyaluronic acid cosmetic material was prepared in the same manner as in Example 7, except that the weight ratio of water-soluble collagen to sodium hyaluronate was 7: 3. The apparent density of the obtained cosmetic material was 0.0129 g / cm < 3 & gt ;.
Comparative Example 1
A ball-shaped collagen-hyaluronic acid cosmetic material was prepared in the same manner as in Example 7, except that the weight ratio of water-soluble collagen to sodium hyaluronate was changed to 10: 0. The apparent density of the obtained cosmetic material was 0.0212 g / cm < 3 & gt ;.
Comparative Example 2
A ball-shaped collagen-hyaluronic acid cosmetic material was prepared in the same manner as in Example 7, except that the weight-average molecular weight of the water-soluble collagen was 2,000 Da and the weight ratio of the water-soluble collagen to the sodium hyaluronate was 9: 1 . The apparent density of the obtained cosmetic material was 0.0312 g / cm < 3 & gt ;.
Comparative Example 3
A ball-shaped collagen-hyaluronic acid cosmetic material was prepared in the same manner as in Example 7, except that the weight-average molecular weight of the water-soluble collagen was 2,000 Da and the weight ratio of the water-soluble collagen to the sodium hyaluronate was 10: 0 . The apparent density of the obtained cosmetic material was 0.0681 g / cm < 3 & gt ;.
Appearance evaluation of cosmetic materials according to content ratio of collagen and hyaluronic acid compounds
In the case of Comparative Example 1, which was made solely of water-soluble collagen having a weight average molecular weight of 3,000 Da, it was made into a foam form, but its shape stability was poor. On the other hand, in Examples 7 to 9, the shape stability of the cosmetic material was excellent, and it was confirmed that as the content of the hyaluronic acid compound to be mixed increased, the cosmetic material became more excellent. In the case of Comparative Example 3, when the collagen had a weight average molecular weight of 2,000 Da alone, it was prepared in powder form without lyophilization, and when it was prepared by mixing hyaluronic acid as in Comparative Example 2, Although it was possible, the morphological stability was significantly reduced.
Example 10
A ball-shaped collagen-hyaluronic acid cosmetic material was prepared in the same manner as in Example 8, except that it was frozen at -5 ° C. The apparent density of the obtained cosmetic material was 0.0109 g / cm < 3 & gt ;.
Example 11
A ball-shaped collagen-hyaluronic acid cosmetic material was prepared in the same manner as in Example 8, except that it was frozen at -10 ° C. The apparent density of the obtained cosmetic material was 0.0113 g / cm < 3 & gt ;.
Appearance evaluation of cosmetic material according to freezing temperature condition
17A to 17C, in Example 10 in which the freezing temperature is -5 DEG C, a fiber-shaped texture is obtained. As the freezing temperature is lowered to -10 DEG C and -15 DEG C, .
Figs. 18A to 18C are SEM photographs of samples that were frozen and dried at a freezing temperature of -5 DEG C (Example 10), -10 DEG C (Example 11), and -15 DEG C (Example 8). 18A to 18C, it can be seen that the larger the freezing temperature, the larger the pore size, and the cosmetic material of desired texture can be manufactured by changing the freezing temperature condition.
Example 12
The water-soluble collagen (weight average molecular weight: 3,000 Da) and sodium hyaluronate (weight average molecular weight: 1.15 x 10 6 Da) were mixed in a weight ratio of 8: 2 and dissolved in distilled water to give a concentration of 0.4 w / v% To prepare a solution for cosmetic materials. The resulting solution was poured into a mold having a uniform spherical shape, frozen at -10 DEG C for 4 hours, then cooled to -20 DEG C for further 24 hours, vacuum-dried at 45 DEG C to obtain a ball having an average diameter of 13.5 mm Shaped collagen-hyaluronic acid cosmetic material. A photograph of the obtained cosmetic material is shown in Fig. The apparent density of the obtained cosmetic material was 0.00621 g / cm < 3 & gt ;.
Referring to FIG. 19, it can be confirmed that the fiber has a fibrous surface texture such as a large pore and a bundle of fibers. This surface texture is a natural material and the characteristic of collagen having a fine fiber structure appears on the surface, so that a more natural and natural feeling of a cosmetic material can be utilized.
Claims (18)
Wherein the weight ratio of the water soluble collagen and the hyaluronic acid compound is 70:30 to 90:10.
Wherein the water soluble collagen is fish-derived collagen.
Wherein the hyaluronic acid compound is at least one selected from the group consisting of hyaluronic acid, sodium hyaluronate, potassium hyaluronate, ammonium hyaluronate, calcium hyaluronate, magnesium hyaluronate, zinc hyaluronate, and cobalt hyaluronate Cosmetic material containing more than.
Wherein the cosmetic material is dissolved in distilled water at 37 ° C within 10 seconds.
Wherein the cosmetic material is dissolved in distilled water at 37 DEG C within 5 seconds.
Wherein the cosmetic material has a spherical outer shape.
Wherein the cosmetic material is a porous form having pores and the average long axis short axis ratio (average long axis length / average short axis length) of the pores is 1.05 to 10.5.
Wherein the cosmetic material is a porous form having pores and the average long axis short axis ratio (average long axis length / average short axis length) of the pores is 2.0 to 10.5.
Wherein the cosmetic material is in the form of a porous foam having a surface in the form of fine fibers.
Freezing the solution for the cosmetic material and then drying the solution,
Wherein the water soluble collagen and the hyaluronic acid compound have a non-crosslinked structure and are water-soluble, and have an apparent density of 0.002 to 0.015 g / cm < 3 >.
Wherein the weight ratio of the water soluble collagen and the hyaluronic acid compound is 70:30 to 90:10.
Wherein the water soluble collagen has a weight average molecular weight of 2,200 Da or more and the hyaluronic acid compound has a weight average molecular weight of 100,000 to 2,000,000 Da.
Wherein the concentration of the solution for the cosmetic material is 0.2 to 1.0 w / v%.
Wherein the freezing step is carried out at a temperature of from -5 to -25 占 폚.
Wherein the freezing step comprises a first freezing step at a temperature of -5 to -10 占 폚 and a second freezing step at a temperature of -15 占 폚 or less.
Further comprising the step of irradiating gamma rays after the drying step.
Wherein the gamma ray irradiation amount is 5 to 30 kGy.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20180060537A (en) * | 2016-11-29 | 2018-06-07 | (주)웰빙해피팜 | Whitening functional cosmetic composition having skin-regeneration and moistureizing |
| CN109106610A (en) * | 2018-08-13 | 2019-01-01 | 浙江珂瑞康生物医疗科技有限公司 | A kind of sterilization process of no antiseptic activity collagen mask |
| CN109288745A (en) * | 2018-10-10 | 2019-02-01 | 广州锦同生物科技有限公司 | A kind of tender skin maintenance cosmetic composition and preparation method thereof |
| CN110075006A (en) * | 2019-04-19 | 2019-08-02 | 华熙生物科技股份有限公司 | Promote the method for the solution compatibility of hyaluronic acid substance and typeⅡ Collagen and the composition containing both substances |
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2015
- 2015-04-24 KR KR1020150058322A patent/KR20160126793A/en active Search and Examination
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20180060537A (en) * | 2016-11-29 | 2018-06-07 | (주)웰빙해피팜 | Whitening functional cosmetic composition having skin-regeneration and moistureizing |
| CN109106610A (en) * | 2018-08-13 | 2019-01-01 | 浙江珂瑞康生物医疗科技有限公司 | A kind of sterilization process of no antiseptic activity collagen mask |
| CN109288745A (en) * | 2018-10-10 | 2019-02-01 | 广州锦同生物科技有限公司 | A kind of tender skin maintenance cosmetic composition and preparation method thereof |
| CN110075006A (en) * | 2019-04-19 | 2019-08-02 | 华熙生物科技股份有限公司 | Promote the method for the solution compatibility of hyaluronic acid substance and typeⅡ Collagen and the composition containing both substances |
| CN110075006B (en) * | 2019-04-19 | 2022-02-25 | 华熙生物科技股份有限公司 | Method for promoting solution compatibility of hyaluronic acid type substance and type II collagen and composition containing the same |
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