Cosmetic Material Composition Comprising Solid Phase Polymer Having Improved Solubility

Abstract

The present invention relates to a solid phase cosmetic composition comprising a freeze-dried component of a composition comprising a functional component and a basic amino acid. A solid phase component according to the present invention has excellent re-dissolvability, and exhibits insignificant changes in the hardness and pH of the composition for dissolving the solid component even after re-dissolution, and thus a cosmetic having excellent stability can be provided.

Claims

1. A solid-phase cosmetic composition comprising a freeze-dried ingredient, wherein the freeze-dried ingredient comprises a functional ingredient and a basic amino acid.

2. The solid-phase cosmetic composition of claim 1, wherein the functional ingredient is one or more of a water-dispersible polymer or a keratin care ingredient.

3. The solid-phase cosmetic composition of claim 2, wherein the water-dispersible polymer is one or more selected from the group consisting of collagen, hyaluronic acid, hydrolyzed hyaluronic acid, β-glucan, xanthan gum, carboxymethyl cellulose, a biosaccharide, cellulose, cellulose gum, arabic gum, gelatin, agar, carrageenan, algin, chitosan, starch, galactomannan, glucomannan, guar gum, locust bean gum, alginate, and gellan.

4. The solid-phase cosmetic composition of claim 1, wherein the basic amino acid is one or more selected from the group consisting of arginine, lysine, asparagine, citrulline, ornithine, tromethamine, and cysteamine.

5. The solid-phase cosmetic composition of claim 1, wherein the composition further comprises a hydrophilic amino acid and/or an acidic amino acid.

6-10. (canceled)

11. A cosmetic comprising: a first composition in a solid phase, and the first composition comprises a freeze-dried ingredient comprising a functional ingredient and a basic amino acid; and a second composition in the form of an emulsion, and the second composition has a hardness of 5 dyne/cm.sup.2 or more.

12-15. (canceled)

16. A method for improving the re-dissolvability of a functional ingredient, comprising: a step of preparing an aqueous solution comprising a functional ingredient and a basic amino acid; and a step of freeze drying the aqueous solution into a solid-phase cosmetic composition comprising the freeze-dried ingredient.

17. The method of claim 16, further comprising a step of mixing the solid-phase cosmetic composition and an emulsion composition having a hardness of 5 dyne/cm.sup.2 or more.

Description

DESCRIPTION OF DRAWINGS

[0041] FIG. 1 is a diagram illustrating the mechanism in which a solid-phase composition of the present invention is dissolved in a liquid-phase formulation.

[0042] FIG. 2 is a diagram illustrating the change over time when a solid-phase composition according to an embodiment of the present invention is mixed with a liquid-phase formulation.

MODES OF THE INVENTION

[0043] Hereinafter, examples will be provided to facilitate understanding of the present invention. However, the following examples are not intended to limit the present invention.

Experimental Example 1. Preparation of Solid-Phase Composition and Cream Formulation

[0044] Solid-phase cosmetic compositions comprising arginine as an amino acid, and hydrolyzed hyaluronic acid (0.5 to 10 kDa, SK Bioland Co., Ltd, Korea) or hyaluronic acid (10 kDa or more, SK Bioland Co., Ltd, Korea) as a functional polymer were prepared according to Table 1.

TABLE-US-00001 TABLE 1 Content (w/w %) Comparative Comparative Ingredient Example 1 Example 2 Example 1 Example 3 Example 4 Example 2 Hydrolyzed 25% 25% 25% hyaluronic acid Hyaluronic acid 25% 25% 25% Serine 65% 65% 75% 65% 65% 75% Arginine 10% — — 10% — — Lysine — 10% — — 10% —

[0045] Specifically, ingredients shown in Table 1 were dissolved in an excessive amount of water to prepare an aqueous solution, and the prepared aqueous solution was solidified by rapid cooling at −150° C. to form a solid phase, followed by a freeze-drying process. The freeze-dried solid was pulverized for convenient use to prepare a solid-phase composition in a powder form of the present invention. When the solid phase composition is decompressed at a temperature below the triple point, water molecules comprised in the composition sublimes, meaning that they become a gaseous phase without going through a liquid phase. In this case, the remaining ingredients shown in Table 1 maintain the water-dissolved structure and form a porous structure. The porous structure is a microstructure and may maintain its porosity without being destroyed during the pulverization process, which is a macroscopic change in properties. A second composition for dissolving the solid-phase cosmetic composition was prepared according to Table 2.

TABLE-US-00002 TABLE 2 Ingredient Content (w/w) Stearyl alcohol 4 Hydrogenated polydecene 8.5 PEG-40 stearate 2.5 Dimethicone 6.5 Water 60.9 Glycerin 17 Acrylate/C10-30 0.2 alkylacrylate crosspolymer Carbomer 0.1 Tromethamine 0.3 Total 100

[0046] As a composition to dissolve the above prepared solid phase composition, a cosmetic composition as a cream having low flowability was prepared according to Table 2. The pH and hardness of this cream composition was 7.15 and 30 dyne/cm.sup.2, where the hardness was measured using a hardness meter immediately after preparation. The hardness was measured using an indentation hardness test method which is generally widely used. The indentation hardness test method is a test method in which the cosmetic material is pressed using a presser with a constant test load for a certain period of time to obtain the degree of indentation in numerical terms, and a Fudoh rheometer (Rheo Tech Co., Ltd., Japan) was used as the hardness meter.

Test Example 1. Confirmation of Change in Physical Properties of Composition

[0047] Each of the solid-phase cosmetic compositions prepared in Examples 1 and 2 and Comparative Example 1 was mixed with the cream composition having a hardness of 30 dyne/cm.sup.2, which was prepared in Experimental Example 1, and the re-dissolvability and re-dissolution time of the solid-phase composition, and the changes in pH and hardness of the cream composition were examined. A portion of each solid-phase composition (Examples 1 and 2 and Comparative Example 1) were taken by a spatula or by hand and mixed with the cream composition by hand to confirm the re-dissolution. (FIG. 2).

TABLE-US-00003 TABLE 3 Hardness (dyne/cm.sup.2) Re- Re-dissolution (variation relative dissolvability time (s) to initial cream) PH Example 1 ⊚  15 s 25 (83%) 7.12 Example 2 ⊚  17 s 27 (90%) 7.13 Comparative ◯  35 s 29 (97%) 7.15 Example 1 Example 3 Δ 112 s 30 (100%) 7.14 Example 4 Δ 125 s 31 (103%) 7.13 Comparative X not 31 (103%) 7.16 Example 2 re-dissolved (⊚ very good, the powder did not agglomerate, and the surface of the composition after re-dissolution was very uniform, ◯: good, trace amounts of powder agglomeration were seen, and the surface of the composition after re-dissolution was uniform, : slightly poor, the surface of the composition after re-dissolution was slightly non- uniform and agglomeration was visible, X: very poor, re-dissolution was not reached, and agglomeration was severe)

[0048] As shown in Table 3, in the case of the solid-phase compositions of Examples 1 and 2 which are compositions comprising ultra-low-molecular-weight hydrolyzed hyaluronic acid and a basic amino acid, it can be confirmed that the solid ingredient was re-dissolved in the cream having low flowability at a high rate via the mechanism shown in FIG. 1. However, it was confirmed that in the case of the solid ingredient of Comparative Example 1 which was formed only of a functional polymer without the use of a basic amino acid, the re-dissolution time was at least twice as long compared to Examples 1 and 2, wherein the re-dissolution time was determined based on measuring how long it took for the solid ingredient to be invisible and unfelt, thus being a uniformly mixed state. In the case of the compositions comprising high-molecular-weight hyaluronic acid, the solid-phase ingredient agglomerated severely and did not re-dissolve as in Comparative Example 2. It can be confirmed that when a basic amino acid was used as in Examples 3 and 4, the improvement in re-dissolvability of the present invention could be reached, but hydrolyzed hyaluronic acid is more preferred to have the excellent quality of a cosmetic.

Experimental Example 2. Preparation of Solid-Phase Composition Comprising Various Functional Polymer Ingredients

[0049] In order to confirm the improve in re-dissolvability of the present invention based on the use of various functional polymer ingredients other than hydrolyzed hyaluronic acid as provided in Examples 1 and 2, solid-phase cosmetic compositions were prepared according to Table 4.

TABLE-US-00004 TABLE 4 Content (w/w %) Comparative Comparative Comparative Ingredient Example 5 Example 6 Example 7 Example 3 Example 4 Example 5 β-glucan 30% — — 30% — — Xanthan gum — 30% — — 30% — Carboxymethyl — — 30% — — 30% cellulose Serine 60% 60% 60% 70% 70% 70% Arginine 10% 10% 10% — — —

Test Example 2. Confirmation of Re-Dissolvability of Solid-Phase Composition Comprising Various Functional Polymer Ingredients

[0050] In order to confirm the re-dissolvability of the solid-phase compositions of Examples 5 to 7 and Comparative Examples 3 to 5 which were prepared in Experimental Example 2, they were mixed with the cream composition having a hardness of 30 dyne/cm.sup.2, which was prepared according to Table 2 in Experimental Example 1, and the re-dissolvability, the re-dissolution rate improvement (%), and the changes in pH and hardness were observed. Specifically, the rate of improvement in the re-dissolution rate was confirmed by comparing the re-dissolution rate (1/re-dissolution time) of the experimental groups that comprise basic amino acid (Examples 5 to 7) with the experimental groups which do not comprise basic amino acid (Comparative Example 3 or 5), where all experimental groups included the same polymer. In addition, the variation in hardness was confirmed by measuring the hardness immediately after mixing the solid-phase composition and the cream composition and comparing it to the initial hardness (30 dyne/cm.sup.2) of the cream composition.

TABLE-US-00005 TABLE 5 Hardness (dyne/cm.sup.2) (variation relative Re-dissolution to initial cream Re-dissolvability time (s) hardness) PH Example 5 ⊚ 18 s 24 (80%) 7.11 Example 6 ⊚ 38 s 27 (90%) 7.14 Example 7 ⊚ 32 s 26 (87%) 7.15 Comparative Δ 58 s 30 (100%) 7.15 Example 3 Comparative Δ 64 s 30 (100%) 7.14 Example 4 Comparative Δ 58 s 30 (100%) 7.15 Example 5 (⊚ very good, the powder did not agglomerate, and the surface of the composition after re-dissolution was very uniform, ◯: good, trace amounts of powder agglomeration were seen, and the surface of the composition after re-dissolution was uniform, : slightly poor, the surface of the composition after re-dissolution was slightly non-uniform and agglomeration was visible, X: very poor, re-dissolution was not reached, and agglomeration was severe)

TABLE-US-00006 TABLE 6 Rate of improvement in re-dissolution rate (%) (relative to re-dissolution rate of Comparative Examples 1, 3, 4, and 5 which do Type of polymer not comprise basic amino acid) Hydrolyzed hyaluronic acid 233.3% β-glucan 322.2% Xanthan gum 168.4% Carboxymethyl cellulose 181.3%

Test Example 3. Confirmation of Re-Dissolvability in Various Preparations

[0051] In order to confirm that the re-dissolvability of the solid-phase composition of the present invention is improved in various preparations other than the cream composition according to Table 2 (hardness: 30 dyne/cm.sup.2), the re-dissolvability of the solid-phase composition of Example 1 was compared with Comparative Example 1 (which does not include basic amino acid) when mixed with an essence (8100 cps) or a solubilized toner (3800 cps). The essence and toner were prepared according to the compositions shown in Table 7 and Table 8, respectively, and evaluated. The viscosity of the essence was measured at 30 rpm for 60 seconds using a Brookfield viscometer (Brookfield LV, Brookfield Engineering Laboratories, Inc., MA, USA). To reduce the effect of air bubbles, the viscosity was measured after defoaming.

TABLE-US-00007 TABLE 7 Ingredient Content (w/w) PEG/PPG/polybutylene glycol-8/5/3glycerin 2 Sodium polyacrylate 0.2 Carbomer 0.18 Acrylate/C10-30alkylacrylate crosspolymer 0.05 PEG-150 1.2 Glycerin 11 Cyclopentasiloxane 1 Dimethicone 6.26 PEG-60 hydrogenated castor oil 0.4 Tromethamine 0.21 1,2-Hexanediol 1.5 Dipropylene glycol 8 Water 68 Total 100

TABLE-US-00008 TABLE 8 Ingredient Content (w/w) Water 78 Alcohol 1 Glycerin 9.5 PEG-40 hydrogenated castor oil 0.6 Carbomer 0.08 Dipropylene glycol 6.64 1,2-Hexanediol 2 Dimethicone 2 Ammonium acryloyldimethyltaurate/ 0.1 VP copolymer Tromethamine 0.08 Total 100

TABLE-US-00009 TABLE 9 Improvement of Re-dissolvability re-dissolution rate (%) Cream ⊚ 234.5% Essence ⊚ 122.7% Toner (solubilized) ⊚ 105.8%

[0052] As shown in Table 9, in the case of the solid-phase composition in which both a functional polymer and a basic amino acid were freeze-dried, it can be confirmed that the re-dissolution rates were improved in all of the cream, essence, and toner formulations as compared to when the solid-phase composition of Comparative Example 1 was mixed with each formulation, and particularly, the degree of improvement of the re-dissolution rate in the cream formulation was higher than that in the solubilized toner where the re-dissolution of the freeze-dried polymer was not problematic due to the low viscosity/hardness of the formulation itself.

Test Example 4. Confirmation of Re-Dissolution Improvement Effect According to Type of Amino Acid

[0053] In order to confirm whether the re-dissolution improvement effect of the freeze-dried solid composition is obtained even with the use of neutral and acidic amino acids other than the basic amino acid of the present invention, glutamic acid as an acidic amino acid, serine as a neutral amino acid, and arginine as a basic amino acid were freeze-dried with a functional polymer as shown in Table 10, and the change in re-dissolvability and hardness in the cream preparation according to Table 2 was confirmed.

TABLE-US-00010 TABLE 10 Content (w/w%) Ingredient Example 6 Example 7 Example 8 Hydrolyzed hyaluronic acid 70% 70% 70% Glutamic acid 30% — — Serine — 30% — Arginine — — 30%

TABLE-US-00011 TABLE 11 Re-dissolution Hardness Re-dissolvability time (s) (dyne/cm.sup.2) PH Example 6 ◯ 20 s 27 6.89 Example 7 Δ 25 s 30 7.15 Example 8 ⊚ 12 s 26 7.45 (⊚ very good, the powder did not agglomerate, and the surface of the composition after re-dissolution was very uniform, ◯: good, trace amounts of powder agglomeration were seen, and the surface of the composition after re-dissolution was uniform, : slightly poor, the surface of the composition after re-dissolution was slightly non-uniform and agglomeration was visible, X: very poor, re-dissolution was not reached, and agglomeration was severe)

[0054] As shown in Table 10, it was confirmed that the neutral amino acid did not exhibit any improvement in re-dissolvability, and that the acidic amino acid and the basic amino acid improved re-dissolvability and re-dissolution time. However, in the case of the acidic amino acid, it was confirmed that the improvement in re-dissolvability of the polymer (carbomer) ingredient was caused by the presence of acidic amino acid reducing the hardness of the composition, and it can be seen that the acidic amino acid is less effective than basic amino acid in terms of weakening the binding force between the polymer (in the solid phase) and water.