Whitening and freckle-removing skin care composition, preparation method and skin care product

Abstract

The present invention relates to a whitening and freckle-removing skin care composition, a preparation method and a skin care product, and belongs to the technical field of cosmetics. The formula of the whitening and freckle-removing skin care composition of the present invention includes ascorbic acid polypeptide, ascorbyl glucoside, 3-o-ethyl ascorbic acid, 4-butylresorcinol, and 4-hexylresorcinol. The present invention uses liposome technology to encapsulate effective ingredients such as 3-o-ethyl ascorbic acid, and optimizes the preparation process, thereby solving the problem of stickiness of high-concentration 3-O-ethyl ascorbic acid, and providing a series of skin care products with strong whitening and freckle-removing effects.

Description

Technical Field

[0001] The invention belongs to the technical field of cosmetics, and specifically relates to a whitening and freckle-removing skin care composition, a preparation method and a skin care product. Background Art

[0002] A Chinese patent with publication number CN109646320A discloses a skin-lightening freeze-dried powder containing oligopeptides and 3-O-ethyl ascorbic acid. The skin-lightening freeze-dried powder contains the following raw materials in parts by weight: 85-95 parts of deionized water, 3-8 parts of D-mannitol, 2-7 parts of vitamin C derivatives, 0.7-1.4 parts of a carbohydrate composition, and 0.0008-0.0018 parts of an oligopeptide; the oligopeptide is oligopeptide-5, the vitamin C derivative is 3-O-ethyl ascorbic acid, and the carbohydrate composition contains trehalose and pullulan; the obtained freeze-dried powder can quickly penetrate the skin, inhibit tyrosinase activity, inhibit the formation of melanin, and can effectively enhance skin brightness and effectively and continuously lighten the skin.

[0003] A Chinese patent with publication number CN111407680A discloses a whitening skin care product, which contains niacinamide, acetyl glucosamine, 3-O-ethyl ascorbic acid, hydroxydecyl ubiquinone, phenethyl resorcinol and resveratrol as main whitening ingredients, and can jointly exert whitening effects through multiple pathways.

[0004] According to numerous research results, 3-O-ethyl ascorbic acid is amphiphilic and lipophilic, suitable for different solvents. When added at more than 2%, it has significant effects on whitening, removing spots and anti-oxidation. However, high concentrations of 3-O-ethyl ascorbic acid also have defects such as poor skin feel and relatively sticky. Summary of the invention

[0005] The present invention overcomes the shortcomings of the prior art and utilizes liposome technology to encapsulate 3-o-ethyl ascorbic acid, thereby solving the stickiness problem of high-concentration 3-O-ethyl ascorbic acid and providing a whitening and freckle-removing skin care composition and skin care product with good skin feel and no stickiness.

[0006] Specifically, the scheme of the present invention is as follows:

[0007] The whitening and freckle-removing skin care composition of the present invention comprises ascorbic acid polypeptide, ascorbic acid glucoside, 3-o-ethyl ascorbic acid, 4-butylresorcinol and 4-hexylresorcinol in proportions of 5 to 15, 1 to 10, 20 to 30, 0.5 to 5 and 0.2 to 2 parts by weight.

[0008] The preparation method of the whitening and freckle-removing skin care composition comprises the following steps:

[0009] (1) dissolving ascorbic acid polypeptide and ascorbic acid glucoside in 40 to 80 parts by weight of a 0.5% to 5.5% aqueous solution of meglumine, adjusting the pH to 6.0 to 7.5 with a buffer solution, and refrigerating at 2° C. to 8° C. to obtain a hydrated solution for later use;

[0010] (2) Dissolve 3-o-ethyl ascorbic acid, 4-butylresorcinol and 15 to 30 parts by weight of lecithin in ethanol and perform rotary evaporation in a water bath at 25°C to 35°C. When the volume of the solution is half of the initial volume, add 4-hexylresorcinol and continue rotary evaporation until a thin film appears. Add a hydrating solution for hydration and continue rotary evaporation until no distillate is produced. Freeze-dry to obtain a whitening and anti-freckle skin care composition.

[0011] Furthermore, in order to adjust the pH value of the solution, the buffer solution is selected from one of a phosphate buffer solution, a carbonate buffer solution and a citrate buffer solution.

[0012] In the present invention, on the one hand, 0.5% to 5.5% meglumine aqueous solution has a certain promoting effect on the transdermal permeability of effective ingredients such as 3-o-ethyl ascorbic acid. On the other hand, it is found through experiments that the specific timing of adding 0.5% to 5.5% meglumine aqueous solution and the optimization of the overall preparation method can solve the defect of high-concentration 3-o-ethyl ascorbic acid having a strong sticky feeling, which helps to improve the texture and absorbency of skin care products. The concentration of the meglumine aqueous solution is screened through experiments, and both too high and too low concentrations will affect the skin feel of the whitening and anti-freckle skin care composition of the present invention and the stability of the effective ingredients.

[0013] The present invention also provides a skin care product composed of the above-mentioned whitening and freckle-removing skin care composition and acceptable auxiliary materials, wherein the auxiliary materials are selected from one or more of thickeners, pH regulators, moisturizers, emulsifiers, skin care ingredient enhancers, penetration enhancers, stabilizers, and fragrances. The amount and type of the auxiliary materials are all routine skills of those skilled in the art. The skin care products include but are not limited to toners, lotions, creams, eye creams, essences, and facial masks.

[0014] Compared with the prior art, the technical effects of the present invention are:

[0015] The present invention uses liposome technology to encapsulate effective ingredients such as 3-o-ethyl ascorbic acid, and optimizes the preparation process, especially selecting a suitable concentration of meglumine aqueous solution and improving some preparation parameters, thereby solving the problem of stickiness of high-concentration 3-O-ethyl ascorbic acid and improving the skin feel and experience of skin care products. In addition, the present invention also verifies the efficacy of skin care products obtained using the whitening and freckle-removing skin care composition in whitening, freckle removal, etc. BRIEF DESCRIPTION OF THE DRAWINGS

[0016] Figure 1: Example 4, Example 5, Example 6, and the change rate of skin melanin during use by the subjects in the control group.

[0017] Figure 2 : Typical images of standard photographs of subjects’ faces for visualization, (a) is on the 28th day; (b) is on the 0th day. DETAILED DESCRIPTION

[0018] In order to make the purpose and technical solution of the present invention clearer, the present invention is further described below in conjunction with embodiments, but the protection scope of the present invention is not limited to these embodiments, and the embodiments are only used to explain the present invention. It should be understood by those skilled in the art that any changes or equivalent substitutions that do not deviate from the concept of the present invention are included in the protection scope of the present invention.

[0019] Example 1 Whitening and anti-freckle skin care composition and preparation method

[0020] formula:

[0021] ;

[0022] Preparation method:

[0023] (1) Dissolve ascorbic acid polypeptide and ascorbic acid glucoside in 60 g of 2.5% by mass meglumine aqueous solution, adjust the pH to 7.0 with phosphate buffer solution, and refrigerate at 5° C. to obtain a hydrated solution for later use;

[0024] (2) Dissolve 3-o-ethyl ascorbic acid, 4-butylresorcinol and 25 g of lecithin in ethanol and perform rotary evaporation in a water bath at 25°C to 35°C. When the volume of the solution is half of the initial volume, add 4-hexylresorcinol and continue rotary evaporation until a thin film appears. Add hydration solution for hydration and continue rotary evaporation until no distillate is produced. Freeze-dry to obtain a whitening and anti-freckle skin care composition.

[0025] Example 2 Whitening and anti-freckle skin care composition and preparation method

[0026] formula:

[0027] ;

[0028] Preparation method:

[0029] (1) Dissolve ascorbic acid polypeptide and ascorbic acid glucoside in 40 g of 0.5% aqueous solution of meglumine, adjust the pH to 6.0 with carbonate buffer solution, and refrigerate at 2° C. to obtain a hydrated solution for later use;

[0030] (2) Dissolve 3-o-ethyl ascorbic acid, 4-butylresorcinol and 15 g of lecithin in ethanol and perform rotary evaporation in a water bath at 25°C to 35°C. When the volume of the solution is half of the initial volume, add 4-hexylresorcinol and continue rotary evaporation until a thin film appears. Add a hydrating solution for hydration and continue rotary evaporation until no distillate is produced. Freeze-dry to obtain a whitening and anti-freckle skin care composition.

[0031] Example 3 Whitening and freckle-removing skin care composition and preparation method

[0032] formula:

[0033] ;

[0034] Preparation method:

[0035] (1) Dissolve ascorbic acid polypeptide and ascorbic acid glucoside in 80 g of 5.5% by mass methylglucamine aqueous solution, adjust the pH to 7.5 with citrate buffer solution, and refrigerate at 8° C. to obtain a hydrated solution for later use;

[0036] (2) Dissolve 3-o-ethyl ascorbic acid, 4-butylresorcinol and 30 g of lecithin in ethanol and perform rotary evaporation in a water bath at 25°C to 35°C. When the volume of the solution is half of the initial volume, add 4-hexylresorcinol and continue rotary evaporation until a thin film appears. Add hydration solution for hydration and continue rotary evaporation until no distillate is produced. Freeze-dry to obtain a whitening and anti-freckle skin care composition.

[0037] Comparative Example 1 Whitening and freckle-removing skin care composition and preparation method

[0038] formula:

[0039] ;

[0040] Preparation method:

[0041] (1) dissolving ascorbic acid polypeptide and ascorbic acid glucoside in water, adjusting the pH to 7.0 with phosphate buffer solution, and refrigerating at 5° C. to obtain a hydrated solution for later use;

[0042] (2) Dissolve 3-o-ethyl ascorbic acid, 4-butylresorcinol and 25 g of lecithin in ethanol and perform rotary evaporation in a water bath at 25°C to 35°C. When the volume of the solution is half of the initial volume, add 4-hexylresorcinol and continue rotary evaporation until a thin film appears. Add hydration solution for hydration and continue rotary evaporation until no distillate is produced. Freeze-dry to obtain a whitening and anti-freckle skin care composition.

[0043] Comparative Example 2 Whitening and freckle-removing skin care composition and preparation method

[0044] formula:

[0045] ;

[0046] Preparation method:

[0047] (1) Dissolve ascorbic acid polypeptide and ascorbic acid glucoside in 60 g of 2.5% aqueous solution of meglumine, adjust the pH to 7.0 with phosphate buffer solution to obtain a hydrated solution, and prepare and use it immediately;

[0048] (2) Dissolve 3-o-ethyl ascorbic acid, 4-butylresorcinol and 25 g of lecithin in ethanol and perform rotary evaporation in a water bath at 25°C to 35°C. When the volume of the solution is half of the initial volume, add 4-hexylresorcinol and continue rotary evaporation until a thin film appears. Add hydration solution for hydration and continue rotary evaporation until no distillate is produced. Freeze-dry to obtain a whitening and anti-freckle skin care composition.

[0049] Comparative Example 3 Whitening and freckle-removing skin care composition and preparation method

[0050] formula:

[0051] ;

[0052] Preparation method:

[0053] Ascorbic acid polypeptide, ascorbic acid glucoside, 3-o-ethyl ascorbic acid, 4-butylresorcinol and 4-hexylresorcinol are crushed and sieved, mixed and freeze-dried to obtain a whitening and freckle-removing skin care composition.

[0054] Comparative Example 4 Whitening and freckle-removing skin care composition and preparation method

[0055] formula:

[0056] ;

[0057] Preparation method:

[0058] (1) Ascorbic acid polypeptide, ascorbic acid glucose, 3-o-ethyl ascorbic acid, 4-butylresorcinol, 4-hexylresorcinol, and 1.5 g of meglumine are crushed and sieved, mixed, and freeze-dried to obtain a whitening and freckle-removing skin care composition.

[0059] Example 4 Essence

[0060] formula:

[0061] Example 1 Whitening and freckle-removing skin care composition 6%, propylene glycol 5%, glycerin 3%, sodium hyaluronate 0.5%, mannitol 0.5%, and the balance is purified water.

[0062] Preparation method:

[0063] The whitening and freckle-removing skin care composition of Example 1, propylene glycol, glycerin, sodium hyaluronate and mannitol were dissolved in purified water and mixed evenly to obtain an essence.

[0064] Example 5 Essence

[0065] formula:

[0066] Example 2 Whitening and freckle-removing skin care composition 6%, propylene glycol 5%, glycerin 3%, sodium hyaluronate 0.5%, mannitol 0.5%, and the balance is purified water.

[0067] Preparation method:

[0068] The whitening and anti-freckle skin care composition of Example 2, propylene glycol, glycerin, sodium hyaluronate and mannitol were dissolved in purified water and mixed evenly to obtain an essence.

[0069] Example 6 Essence

[0070] formula:

[0071] Example 3 Whitening and freckle-removing skin care composition 6%, propylene glycol 5%, glycerin 3%, sodium hyaluronate 0.5%, mannitol 0.5%, and the balance is purified water.

[0072] Preparation method:

[0073] The whitening and anti-freckle skin care composition of Example 3, propylene glycol, glycerin, sodium hyaluronate and mannitol were dissolved in purified water and mixed evenly to obtain an essence.

[0074] Comparative Example 5 Essence

[0075] formula:

[0076] Comparative Example 1: 6% whitening and anti-freckle skin care composition, 5% propylene glycol, 3% glycerin, 0.5% sodium hyaluronate, 0.5% mannitol, and the balance is purified water.

[0077] Preparation method:

[0078] The whitening and anti-freckle skin care composition of Comparative Example 1, propylene glycol, glycerin, sodium hyaluronate and mannitol were dissolved in purified water and mixed evenly to obtain an essence.

[0079] Comparative Example 6 Essence

[0080] formula:

[0081] Comparative Example 2: 6% whitening and anti-freckle skin care composition, 5% propylene glycol, 3% glycerin, 0.5% sodium hyaluronate, 0.5% mannitol, and the balance is purified water.

[0082] Preparation method:

[0083] The whitening and anti-freckle skin care composition of Comparative Example 2, propylene glycol, glycerin, sodium hyaluronate and mannitol were dissolved in purified water and mixed evenly to obtain an essence.

[0084] Comparative Example 7 Essence

[0085] formula:

[0086] Comparative Example 3: 6% whitening and anti-freckle skin care composition, 5% propylene glycol, 3% glycerin, 0.5% sodium hyaluronate, 0.5% mannitol, and the balance is purified water.

[0087] Preparation method:

[0088] The whitening and freckle-removing skin care composition of Comparative Example 3, propylene glycol, glycerin, sodium hyaluronate and mannitol were dissolved in purified water and mixed evenly to obtain an essence.

[0089] Comparative Example 8 Essence

[0090] formula:

[0091] Comparative Example 4: 6% whitening and anti-freckle skin care composition, 5% propylene glycol, 3% glycerin, 0.5% sodium hyaluronate, 0.5% mannitol, and the balance is purified water.

[0092] Preparation method:

[0093] The whitening and anti-freckle skin care composition of Comparative Example 4, propylene glycol, glycerin, sodium hyaluronate and mannitol were dissolved in purified water and mixed evenly to obtain an essence.

[0094] Stickiness Evaluation

[0095] In order to explore the effect of the whitening and freckle-removing skin care composition of the present invention on improving the stickiness, the whitening and freckle-removing skin care compositions of Examples 1 to 3 and Comparative Examples 1 to 4 were prepared into essences. Under the same cosmetic dosage form and excipients, the stickiness of the essences of Examples 3 to 5 and Comparative Examples 5 to 8 was measured, and the stickiness was evaluated by skin feel observation, foam ball test, and absorption speed test, respectively.

[0096] Skin feel observation: Through real-person trial experience, you can directly feel the texture of the essence and the feeling after application to evaluate the stickiness of the essence. The stickiness can be scored from 1 to 5 from light to heavy (1 is refreshing and non-sticky, 5 is thick and sticky).

[0097] Table 1 Skin feel observation score

[0098] ;

[0099] The texture of the essence and the stickiness after application were scored by real people's trial experience, and the results showed that there were significant differences in the scores of Example 4-6 compared with Comparative Example 5, Example 4-6 compared with Comparative Example 6, Example 4-6 compared with Comparative Example 7, and Example 4-6 compared with Comparative Example 8, indicating that the whitening and freckle-removing skin care composition of the present invention overcomes the defect of poor skin feel of high-concentration 3-o-ethyl ascorbic acid.

[0100] Foam ball test: Apply the essence evenly on the back of your hand, let it sit for 10 seconds, then press the back of your hand on the foam ball and observe the number of foam balls left on the back of your hand. The more foam balls there are, the more sticky the skin care product is. The fewer foam balls there are, the more refreshing and non-sticky the skin care product is.

[0101] Table 2 Foam ball test ( , n=20)

[0102] ;

[0103] The foam ball test showed that the essence of the present invention was evenly applied to the back of the hand and then pressed on the foam ball for 10 seconds. The number of foam balls on the back of the hand was small, with an average of 5 to 6 foam balls, while the essence of the comparative example still had a sticky and heavy feeling, and the number of foam balls stuck was large. Compared with the comparative example 5 to 8 groups, P < 0.01, all of them had significant differences.

[0104] Absorption speed test: Evaluate the stickiness of the essence by measuring the time from applying the essence to being completely absorbed by the skin.

[0105] Table 3 Absorption rate test ( , n=20)

[0106] ;

[0107] Compared with the comparative examples 5 to 8, the differences in Examples 4 to 6 were significant (P<0.01). The essences in Examples 4 to 6 were absorbed quickly, felt more refreshing and comfortable, and the active ingredients were more easily absorbed by the skin.

[0108] In summary, the stickiness was evaluated by skin feel observation, foam ball test, and absorption speed test, and the effect of the whitening and anti-freckle skin care composition of the present invention on improving the stickiness was explored. The results showed that the essence prepared in Examples 1 to 3 of the present invention was refreshing and non-sticky, and could significantly improve the user experience and comfort, overcoming the defects of stickiness and poor skin feel of skin care products caused by high concentration of 3-o-ethyl ascorbic acid.

[0109] Transdermal permeability

[0110] Prepare several SD rats, SPF grade, 180-220g, experimental animal license number: SYXK (Lu) 2018 0008, and feed them for one week before the experiment. The rats were depilated with 8% sodium sulfide solution, raised for 24 hours, and the abdominal skin was taken after being killed by cervical dislocation, subcutaneous fat was removed, and the surface moisture was absorbed by filter paper. The treated rat abdominal skin was fixed between the supply pool and the receiving pool using a transdermal instrument, with the stratum corneum facing the supply pool. The supply pools were filled with equal amounts of the essences of Examples 3 to 5 and Comparative Examples 5 to 8; the receiving solution was 20% ethanol-pH 7.4 phosphate buffer, sampled at 1 hour, and supplemented with the corresponding volume of the receiving solution. The sample was filtered with a 0.22 μm microporous membrane, the content of the active ingredient 3-o-ethyl ascorbic acid in the receiving solution was determined, and the cumulative penetration of each embodiment was calculated according to the formula.

[0111] ) / A

[0112] Where V is the total volume of the receiving solution, Cn is the drug concentration measured at the nth sampling point (μg / mL), C is the drug concentration measured at the ith sampling point (μg / mL), V is the sampling volume, and A is the diffusion permeation area (cm 2 ).

[0113] Table 4 Cumulative permeation of 3-o-ethyl ascorbic acid ( , n=10)

[0114] ;

[0115] The transdermal permeability experiment in Table 4 shows that the essence prepared from the whitening and freckle-removing skin care composition of the present invention can be quickly absorbed by the skin, which on the one hand reflects the characteristics of light texture, and on the other hand, the absorption of effective ingredients can promote the manifestation of whitening and freckle-removing effects.

[0116] Evaluation of the effect of the whitening and anti-freckle skin care composition of the present invention

[0117] Subject information

[0118] The total number of subjects was 120, female, aged 35-59 years old, and they were divided into Example 4 group, Example 5 group, Example 6 group, and control group (Yuezhuang 20160040), with an average age of 50.1 years, 50.2 years, and 49.9 years old in each group. After cleansing and toning, apply an appropriate amount of the corresponding essence to the entire face and gently pat until absorbed. Twice a day for 4 consecutive weeks.

[0119] Melanin change rate

[0120] The melanin content in the skin was checked with a German CK skin melanin tester 1 day before use (day 0) and every week (day 7, day 14, day 21, day 28), and the skin melanin change rate was calculated.

[0121] Melanin change rate = skin melanin content measured after applying the sample / skin melanin content measured before applying the sample × 100%.

[0122] Transepidermal water loss TEWL value

[0123] The transepidermal water loss (TEWL) value of the test subjects' faces was tested using Tewameter TM300, and the measured value was significantly reduced, indicating that the transepidermal water loss rate of the skin was significantly reduced, and it is believed that this product has the effect of repairing the skin barrier.

[0124] Table 5 Transepidermal water loss TEWL value ( , n=30)

[0125] ;

[0126] Compared with the control group on day 28, *P<0.01.

[0127] After the subjects used the sample for 28 days, the transepidermal water loss TEWL value was significantly reduced compared with the control group, P<0.01.

[0128] Skin elasticity characterization R value

[0129] Cutometer was used to test the skin elasticity of the subjects' facial skin. The instrument is based on the principle of suction and stretching. It generates a negative pressure on the surface of the tested skin to suck the skin into a specific test probe. R2 refers to the ratio of the rebound displacement to the maximum stretch displacement after the skin is sucked up. The larger the R2 value, the better the skin elasticity.

[0130] Table 6 R value of skin elasticity characterization ( , n=30)

[0131] ;

[0132] Compared with the control group on day 28, *P<0.01.

[0133] After the subjects used the sample for 28 days, the R value, a measure of skin elasticity, was significantly increased compared with the control group (P<0.01).

[0134] Typical images

[0135] Figure 2The typical image of the standard facial visualization photo of subject screening number 17 is shown by comparison. It can be seen that after using the product of Example 5 for 28 days, the subject's facial skin color showed a white and shiny feeling, and the spots were significantly faded, which more intuitively proves that the composition and skin care products of the present invention have the effect of whitening, lightening and removing spots.

Claims

1. A whitening and freckle-removing skin care composition, characterized in that: The whitening and freckle-removing skin care composition comprises, by weight, 5 to 15 parts of ascorbic acid polypeptide, 1 to 10 parts of ascorbic acid glucoside, 20 to 30 parts of 3-o-ethyl ascorbic acid, 0.5 to 5 parts of 4-butylresorcinol, 0.2 to 2 parts of 4-hexylresorcinol, 15 to 30 parts of lecithin, and 40 to 80 parts by weight of a 0.5% to 5.5% aqueous solution of meglumine; The preparation method of the whitening and freckle-removing skin care composition comprises the following steps: (1) dissolving ascorbic acid polypeptide and ascorbic acid glucoside in a meglumine aqueous solution, adjusting the pH to 6.0-7.5 with a buffer solution, and refrigerating at 2°C-8°C to obtain a hydrated solution for later use; (2) Dissolve 3-o-ethyl ascorbic acid, 4-butylresorcinol and lecithin in an organic solvent, and perform rotary evaporation in a water bath at 25°C to 35°C. When the volume of the solution is half of the initial volume, add 4-hexylresorcinol, and continue rotary evaporation until a thin film appears. Add a hydrating solution for hydration, and continue rotary evaporation until no distillate is produced. The mixture is freeze-dried to obtain a whitening and anti-freckle skin care composition.

2. The whitening and freckle-removing skin care composition according to claim 1, characterized in that: The buffer solution is selected from one of a phosphate buffer solution, a carbonate buffer solution and a citrate buffer solution.

3. The whitening and freckle-removing skin care composition according to claim 1, characterized in that: The organic solvent is ethanol.

4. The whitening and freckle-removing skin care composition according to claim 1, characterized in that: The mass fraction of the meglumine aqueous solution is 2.5%.

5. A skin care product, characterized in that: The skin care product is composed of the whitening and freckle-removing skin care composition according to claim 1 and auxiliary materials.

6. The skin care product according to claim 5, characterized in that: The auxiliary material is selected from one or more of a thickener, a pH regulator, a humectant, an emulsifier, a penetration enhancer, a stabilizer, and a fragrance.

7. The skin care product according to claim 5, characterized in that: The skin care products are toner, lotion, face cream, eye cream, essence and facial mask.

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