A bionic sebum film composite oil base special for color cosmetics and a preparation method thereof

Abstract

The present application provides a kind of bionic sebum film composite grease base special for makeup, which is composed of the following components by mass percentage, based on the total mass of the composition: 70-90wt% goose oil; 1-5wt% oil-soluble tea polyphenol; 0.1-1wt% tocopherol; and the balance is high-oleic goose oil fraction. The present application also provides a kind of makeup composition comprising the above-mentioned base, color powder and wax. The present application also provides a preparation method of the above-mentioned bionic sebum film composite grease base special for makeup. The present application is modified with tea polyphenol, which solves the problems of easy oxidation, heaviness and odor of goose oil, while retaining the advantages of goose oil bionics, giving antioxidant color protection function, and forming a special bionic base for makeup.

Description

Technical Field

[0001] This invention belongs to the field of cosmetics and relates to a type of makeup, specifically a biomimetic sebum film composite oil base material for makeup and its preparation method. Background Technology

[0002] Bionic technology serves as a bridge further connecting skincare products and the skin. By studying the skin's structure, function, and composition, it simulates the corresponding component and structural proportions of the skin, using biotechnology to extract and manufacture active ingredients and formulas that are similar to the human body's own structure and have high affinity, creating higher-performance products that better fit the skin. Bionic technology and systems will gradually become one of the new directions for concentrated investment in global skincare product research and development, and will also bring new possibilities for the innovative iteration and upgrading of functional skincare products.

[0003] Table 1 Comparison of Fatty Acid Composition of Human Skin Lipid Membrane and Goose Fat

[0004] .

[0005] Therefore, goose oil has positive value in the preparation of biomimetic cosmetics. However, goose oil also has many drawbacks, including easy oxidation and rancidity (PUFA self-oxidation), high melting point (mp~35-40°C), heavy spreading, and animal-like odor. Summary of the Invention

[0006] To address the aforementioned technical problems in the prior art, this invention provides a biomimetic sebum film composite oil base material for cosmetics and its preparation method. This biomimetic sebum film composite oil base material for cosmetics and its preparation method aim to solve the technical problems of goose oil being easily oxidized and rancid, having a high melting point, being viscous and heavy when spread, and having an animal-like fishy or muttony odor in the prior art.

[0007] This invention provides a biomimetic sebum film composite oil base material for cosmetics, which, based on the total mass of the composition, consists of the following components in the following mass percentages:

[0008] Goose fat 70-90 wt%

[0009] Oil-soluble tea polyphenols 1~5wt%;

[0010] Tocopherol 0.1~1wt%;

[0011] The remainder is high-oleic goose fat fraction;

[0012] Furthermore, the peroxide value of the composite oil base is ≤5 meq / kg, and the melting point is 30~38℃.

[0013] Specifically, the oil-soluble tea polyphenols mentioned are acetylated tea polyphenols or tea polyphenol palmitate.

[0014] Furthermore, the mixed tocopherols are composed of α-tocopherol, β-tocopherol, γ-tocopherol, and δ-tocopherol, with the following mass percentage content of each substance:

[0015] α-Tocopherol 10~15%;

[0016] β-Tocopherol 3~10%;

[0017] γ-Tocopherol 50-65%

[0018] δ-Tocopherol 15~25%.

[0019] Furthermore, the preparation method of the oil-soluble tea polyphenols is as follows:

[0020] 1) Dissolve soybean phospholipids in anhydrous ethanol at a concentration of 5-10 mg / mL, and stir at a constant temperature of 50-65℃ for 20-40 min to allow the phospholipids to fully swell and self-assemble into a lipid film dispersion.

[0021] 2) Dissolve tea polyphenols in anhydrous ethanol to obtain a tea polyphenol solution; the material ratio of soybean lecithin to tea polyphenols is (1~3):1;

[0022] 3) Inject the tea polyphenol solution into the lipid film dispersion and stir at 50-65℃ for 1-2 hours under nitrogen protection;

[0023] 4) Ultrasonic treatment for 20-30 minutes to form a micromicelle encapsulation system;

[0024] 5) Remove ethanol by rotary evaporation to obtain a micromicelle dispersion with a particle size of 50~200nm, which is the oil-soluble tea polyphenol. Freeze-dry to obtain a solid powder for later use.

[0025] Furthermore, the color difference ΔE of the makeup products made by adding pigments was ≤1.5 after 7 days of accelerated aging at 45℃.

[0026] Furthermore, in the goose oil, the mass percentage concentration of oleic acid is 52-60%, the mass percentage concentration of palmitoleic acid is 10-18%, and the acid value is <1.0 mgKOH / g.

[0027] Furthermore, the oil-soluble tea polyphenols contain ≥50% by mass of epigallocatechin gallate (EGCG).

[0028] Furthermore, the method for preparing the high-oleic goose oil fraction is as follows:

[0029] 1) Preheat the goose fat to 80~100℃ to remove moisture and impurities;

[0030] 2) Feed the sample into a short-path molecular distillation apparatus, and control the distillation temperature at 180~220℃, the vacuum degree at <10Pa, and the feed rate at 2~5mL / min;

[0031] 3) Collect the light fraction (mainly containing free fatty acids and low molecular weight volatiles) at 180~195℃ in the first stage and discard it;

[0032] 4) The second stage collects the heavy fraction at 195~220℃, which is the high oleic acid goose oil fraction rich in oleic acid; the high oleic acid goose oil fraction contains oleic acid C18:1≥70% and has a melting point of 20~25℃.

[0033] The core of molecular distillation is "discarding the light fraction and collecting the heavy fraction"—because oleic acid (C18:1) has a relatively large molecular weight (282), it will preferentially distill off under high vacuum at 180~220℃, while large molecules such as triglycerides remain in the residue. Collecting the fraction in the 195~220℃ range yields a high-purity oleic acid concentrate.

[0034] This invention also provides a method for preparing the above-mentioned biomimetic sebum film composite oil base for cosmetics, comprising the following steps:

[0035] 1) Weigh each material according to its mass percentage;

[0036] 2) Vacuum dehydrate the goose fat;

[0037] 3) Add tea polyphenols, tocopherols, and high oleic acid goose fat fraction at 60~80℃;

[0038] 4) Stir evenly under an inert atmosphere;

[0039] 5) Cooling and filtration yields a biomimetic sebum film composite oil base material specifically for cosmetics.

[0040] The present invention provides a cosmetic composition comprising any of the base materials, color powders, and waxes described above.

[0041] Table 2 shows the mechanism by which this invention overcomes the defects of goose fat:

[0042]

[0043] EGCG (extracellular glutamate) at 0.02%~0.1% can reduce the POV (Potential Oxidation Value) of animal fats by 60%~80%. Fat-soluble modified tea polyphenols (acetylated / phospholipid-encapsulated) are uniformly dispersed in the fat, inhibiting the lipid peroxidation chain reaction and reducing the POV to <5~10 meq / kg. This invention, by adding 1%~5% oil-soluble tea polyphenols (EGCG ≥50%), can reduce the POV of goose fat from an initial ~15 meq / kg to <5 meq / kg. This invention, by retaining the biomimetic advantages of goose fat (high oleic acid + ω-7 anti-inflammatory), endows it with antioxidant and color-protecting functions, forming a biomimetic base material specifically for cosmetics.

[0044] Compared with existing technologies, the technical effects of this invention are positive and obvious.

[0045] 1. Biomimetic basis: The fatty acid composition of goose fat (oleic acid 52-60%, palmitoleic acid 10-18%), the fatty acid distribution and S / U ratio of goose fat are highly similar to those of human sebum membrane (literature: Downing, Lipids 1983), which is a true "bionic sebum membrane", which can promote pigment spreading and reduce transdermal irritation.

[0046] 2. Overcoming defects: Modification with tea polyphenols solves the three major problems of goose fat being easily oxidized (POV<5), heavy, and having an off-flavor.

[0047] 3. Makeup performance: Pigment dispersion D50≤8um, accelerated darkening ΔE≤1.5 after 7 days at 45℃, which is superior to castor oil. Detailed Implementation

[0048] Example 1:

[0049] I. The preparation method of oil-soluble tea polyphenols is as follows:

[0050] 1) Dissolve 6.0g of soybean lecithin (PC content ≥60%) in 600mL of anhydrous ethanol at a concentration of 10mg / mL, and stir at a constant temperature of 60℃ for 30min to allow the lecithin to fully swell and self-assemble into a lipid film dispersion.

[0051] 2) Dissolve 3.0g of tea polyphenols (EGCG≥50%, acetylated tea polyphenols) in 100mL of anhydrous ethanol to obtain a tea polyphenol solution;

[0052] 3) Slowly inject the tea polyphenol solution into the phospholipid film dispersion and stir at 60°C for 1 hour under nitrogen protection;

[0053] 4) Ultrasonic treatment (power 400W) for 30 minutes to form a micromicelle encapsulation system;

[0054] 5) Ethanol was removed by rotary evaporation (60℃, -0.09MPa) to obtain a micromicelle dispersion with a particle size of 50~200nm.

[0055] 6) Freeze-dry (-40℃, 24h) to obtain a solid powder for later use, yielding approximately 8.5g of phospholipid-encapsulated tea polyphenols.

[0056] II. The preparation method of the high oleic acid goose fat fraction is as follows:

[0057] 500g of refined goose fat provided by Anhui Dezhengtang Pharmaceutical Group Co., Ltd. was used to prepare a high-oleic goose fat fraction using the following molecular distillation process:

[0058] 1) Pretreatment: Melt the goose fat at 80℃, then vacuum dehydrate it until the water content is <0.05%; at the same time, remove impurities;

[0059] 2) Feed into a short-path molecular distillation apparatus, molecular distillation conditions:

[0060] Distillation temperature: 200℃;

[0061] Vacuum degree: <5Pa;

[0062] Feed rate: 3 mL / min;

[0063] Scraping speed: 200 rpm;

[0064] Condensation temperature: 40℃.

[0065] 3) Fraction collection:

[0066] First stage (180~195℃): Light component fraction, mainly containing free fatty acids and low molecular weight volatiles, accounting for about 15% of the feed, is discarded;

[0067] The second section (195~220℃): the target fraction, rich in oleic acid, with a yield of about 35% (175g), which is the high oleic acid goose fat fraction;

[0068] Residue (not distilled at >220℃): mainly consists of macromolecules such as triglycerides, accounting for about 50%, which will be collected separately for other uses.

[0069] 4) The obtained high oleic acid goose oil fraction was analyzed by gas chromatography (GC): oleic acid C18:1 content was 72.5%, melting point was 22℃.

[0070] 5) Obtain 175g of high oleic acid goose oil fraction for later use.

[0071] III. Preparation method of biomimetic sebum film composite oil base for makeup

[0072] Take 78.0g of goose fat (from Anhui Dezhengtang Pharmaceutical Group Co., Ltd.).

[0073] 18.5g of high-oleic goose fat fraction.

[0074] Add 3.0g of oil-soluble tea polyphenols (EGCG≥50%, phospholipid encapsulation)

[0075] Mixed tocopherols 0.5g.

[0076] Specifically, the oleic acid in the goose oil has a mass percentage concentration of 52-60%, the palmitoleic acid has a mass percentage concentration of 10-18%, and the acid value is <1.0 mgKOH / g.

[0077] The mixed tocopherols consist of α-tocopherol, β-tocopherol, γ-tocopherol, and δ-tocopherol, with the following mass percentages of each substance:

[0078] α-Tocopherol 10%;

[0079] β-Tocopherol 5%;

[0080] γ-Tocopherol 60%

[0081] δ-Tocopherol 25%.

[0082] 1) Goose fat is vacuum dehydrated at 80℃.

[0083] 2) Then add high-oleic goose fat fraction, oil-soluble tea polyphenols, and mixed tocopherols;

[0084] 3) Purge with nitrogen and stir for 2 hours (to prevent oxidation), then stir at 500 rpm for 3 hours to achieve uniform dispersion / slight dissolution;

[0085] 4) Cool down to ≤40℃, filter through a 0.45um filter membrane to remove impurities, and obtain a light yellow transparent biomimetic sebum film composite oil base material.

[0086] Performance: Melting point 34℃ (DSC method), POV=3.2meq / kg, DPPH removal rate=84%, TiO2 dispersion D50=6.8um, viscosity at 25℃ 200~500nnPa·s, peroxide value ≤5meq / kg, DPPH removal rate.

[0087] The oil-soluble tea polyphenols used in this invention are encapsulated in soybean phospholipid micelles, which can form a uniform dispersion system in goose oil without obvious precipitation (observed visually and under an optical microscope). The system shows no stratification after 3 months of storage, indicating its stability.

[0088] The biomimetic sebum film composite oil base material was prepared according to the method described in the embodiments of the present invention. Its peroxide value was measured to be ≤5 meq / kg. When combined with pigments, the resulting cosmetic product showed a color difference ΔE ≤1.5 after accelerated aging at 45℃ for 7 days (the test method refers to GB / T5538 and ISO11664-4).

[0089] Example 2 (Lower Limit Verification):

[0090] Goose fat 83.0g

[0091] 15.5g of high oleic acid fraction

[0092] 1.0g of oil-soluble tea polyphenols

[0093] Mixed tocopherols 0.5g.

[0094] The mixed tocopherols consist of α-tocopherol, β-tocopherol, γ-tocopherol, and δ-tocopherol, with the following mass percentages of each substance:

[0095] α-Tocopherol 10%;

[0096] β-Tocopherol 5%;

[0097] γ-Tocopherol 60%

[0098] δ-Tocopherol 25%.

[0099] The preparation method is the same as in Example 1;

[0100] Peroxide value POV≤5meq / kg, melting point 36℃, DPPH removal rate≥80%, color difference ΔE≤1.5 after 7 days of accelerated aging at 45℃ for color powder cosmetics.

[0101] That is, all performance indicators within the same range as in Example 1 are deemed to meet the standards.

[0102] Example 3 (High Limit Verification):

[0103] Goose fat 76.0g

[0104] 18.0g of high oleic acid fraction

[0105] 5.0g of oil-soluble tea polyphenols

[0106] Mixed tocopherols 1.0g.

[0107] The mixed tocopherols consist of α-tocopherol, β-tocopherol, γ-tocopherol, and δ-tocopherol, with the following mass percentages of each substance:

[0108] α-Tocopherol 10%;

[0109] β-Tocopherol 5%;

[0110] γ-Tocopherol 60%

[0111] δ-Tocopherol 25%.

[0112] The preparation method is the same as in Example 1.

[0113] Peroxide value POV≤5meq / kg, melting point 31℃, DPPH removal rate≥80%, color difference ΔE≤1.5 after 7 days of accelerated aging at 45℃ for color powder cosmetics.

[0114] That is, all performance indicators within the same range as in Example 1 are deemed to meet the standards.

[0115] Comparative Example 1

[0116] 99.5g goose fat

[0117] Mixed tocopherols 0.5g

[0118] The mixed tocopherols consist of α-tocopherol, β-tocopherol, and γ-tocopherol, with the following mass percentages of each substance:

[0119] α-Tocopherol 10%;

[0120] β-Tocopherol 5%;

[0121] γ-Tocopherol 60%

[0122] δ-Tocopherol 25%.

[0123] (Equal amount of tocopherol as in Example 1, without the addition of tea polyphenols and high oleic acid fraction).

[0124] The preparation method is the same as in Example 1, POV=22, with severe darkening and an off-odor.

[0125] Comparative Example 2 (castor oil):

[0126] 97g of commercially available castor oil

[0127] 3.0g of oil-soluble tea polyphenols

[0128] (Equal amount of tea polyphenols as in Example 1).

[0129] The preparation method is the same as in Example 1, with poor dispersion (D50=12.5um) and dullness (ΔE=4.6).

[0130] The test methods of the present invention are shown in Table 3, and the test results are shown in Table 4.

[0131] Table 3

[0132]

[0133] Table 4

[0134]

[0135] The ΔE values ​​were all based on measured values: Example 1 ΔE=1.3, Comparative Example 1 ΔE=3.9, Comparative Example 2 ΔE=4.6.

[0136] Example 4: In vitro cell mildness

[0137] The base material of Example 1 was compared with that of Comparative Example 1 (unmodified goose fat) and Comparative Example 2 (castor oil) (see Table 5).

[0138] Test method:

[0139] EpiDerm: Cells were treated with OECD TG 439 at a 5% substrate concentration for 4 hours, and cell viability was determined by the MTT assay; a viability rate >50% was considered non-stimulating.

[0140] - Patch test: In accordance with ISO 10993-10:2021, 30 volunteers with sensitive skin (22 women and 8 men, aged 22-55 years) underwent 48 hours of closed patch application, and were evaluated by dermatologists at 30 minutes and 24 hours after removal.

[0141] Table 5

[0142]

[0143] Conclusion: Comparative Example 1 (unmodified goose fat) showed one case of mild erythema irritation (irritation rate 3.3%). This is because unmodified goose fat contains trace amounts of free fatty acids and aldehydes, which may cause mild irritation in highly sensitive individuals, but does not meet the criteria for "irritation" (irritation rate >10%). Example 1, after modification with tea polyphenols, showed further reduction in irritation, superior to Comparative Example 1.

[0144] Example 5: Preparation of Bionic Sebum Film Foundation Cream

[0145] The materials required to prepare the biomimetic sebum film foundation are shown in Table 6 below:

[0146] Table 6

[0147]

[0148] The mixed tocopherols consist of α-tocopherol, β-tocopherol, γ-tocopherol, and δ-tocopherol, with the following mass percentages of each substance:

[0149] α-Tocopherol 10%;

[0150] β-Tocopherol 5%;

[0151] γ-Tocopherol 60%

[0152] δ-Tocopherol 25%.

[0153] Process:

[0154] 1) Heat 40.0g of biomimetic sebum film composite oil base + 8.0g of beeswax + 3.0g of candelilla wax to 80℃ to melt, and homogenize at 1000rpm×5min;

[0155] 2) Cool down to 65℃, add pre-dispersed color powder slurry (TiO2 6.0g + Fe2O3 3.0g + mica powder 5.0g + a small amount of base material, and grind three times with a three-roll mill), and homogenize at 2500rpm×3min;

[0156] 3) Add 0.3g sodium hyaluronate, 0.5g mixed tocopherols, and 0.2g flavoring, and homogenize at 1500rpm for 2min;

[0157] 4) Vacuum degassing (-0.08MPa, 50℃, 30min), fill into aluminum cans, cool to room temperature and demold.

[0158] Technical effects:

[0159] Colorant D50 = 5.5μm (measured by laser particle size analyzer).

[0160] Spreading area = 9.2cm² / 0.1mL.

[0161] Accelerated aging at 45℃ for 7 days: ΔE = 1.1 (measured by colorimeter).

[0162] - Sensory evaluation: Adhesion 9 / 10, Smoothness 8.5 / 10, Makeup lasting power 8 / 10.

Claims

1. A biomimetic sebum film composite oil base material for cosmetics, characterized in that, The composition comprises the following components by mass percentage, based on the total mass of the composition: Goose fat 70-90 wt% Oil-soluble tea polyphenols 1~5wt%; Tocopherol 0.1~1wt%; The remainder is high-oleic goose fat fraction.

2. The biomimetic sebum film composite oil base material for cosmetics according to claim 1, characterized in that, The peroxide value of the composite oil base is ≤5 meq / kg, and the melting point is 30~38℃.

3. The biomimetic sebum film composite oil base material for cosmetics according to claim 1, characterized in that, The mixed tocopherols described herein consist of α-tocopherol, β-tocopherol, γ-tocopherol, and δ-tocopherol, with the following mass percentage content of each substance: α-Tocopherol 10~15%; β-Tocopherol 3~10%; γ-Tocopherol 50-65% δ-Tocopherol 15~25%.

4. The biomimetic sebum film composite oil base material for cosmetics according to claim 1, characterized in that... The preparation method of the oil-soluble tea polyphenols is as follows: 1) Dissolve soybean phospholipids in anhydrous ethanol at a concentration of 5-10 mg / mL, and stir at a constant temperature of 50-65℃ for 20-40 min to allow the phospholipids to fully swell and self-assemble into a lipid film dispersion. 2) Dissolve tea polyphenols in anhydrous ethanol to obtain a tea polyphenol solution; the material ratio of soybean lecithin to tea polyphenols is (1~3):1; 3) Inject the tea polyphenol solution into the lipid film dispersion and stir at 50-65℃ for 1-2 hours under nitrogen protection; 4) Ultrasonic treatment for 20-30 minutes to form a micromicelle encapsulation system; 5) Remove ethanol by rotary evaporation to obtain a micromicelle dispersion with a particle size of 50~200nm, which is the oil-soluble tea polyphenol. Freeze-dry to obtain a solid powder for later use.

5. The biomimetic sebum film composite oil base material for cosmetics according to claim 1, characterized in that... The color difference ΔE of makeup products made by adding pigments is ≤1.5 after 7 days of accelerated aging at 45℃.

6. The biomimetic sebum film composite oil base material for cosmetics according to claim 1, characterized in that... The goose oil contains 52-60% oleic acid and 10-18% palmitoleic acid, with an acid value of <1.0 mgKOH / g.

7. The biomimetic sebum film composite oil base material for cosmetics according to claim 1, characterized in that... The oil-soluble tea polyphenols contained ≥50% by mass of epigallocatechin gallate (EGCG).

8. The biomimetic sebum film composite oil base material for cosmetics according to claim 1, characterized in that... The method for preparing the high-oleic goose fat fraction is as follows: 1) Preheat the goose fat to 80~100℃ to remove moisture and impurities; 2) Feed the sample into a short-path molecular distillation apparatus, and control the distillation temperature at 180~220℃, the vacuum degree at <10Pa, and the feed rate at 2~5mL / min; 3) Collect the light fraction at 180~195℃ in the first stage and discard it; 4) The second stage collects the heavy fraction at 195~220℃, which is the high oleic acid goose oil fraction rich in oleic acid; the high oleic acid goose oil fraction contains oleic acid C18:1≥70% and has a melting point of 20~25℃.

9. The method for preparing a biomimetic sebum film composite oil base material for cosmetics as described in claim 1, characterized in that... Includes the following steps: 1) Weigh each material according to its mass percentage; 2) Vacuum dehydrate the goose fat; 3) Add oil-soluble tea polyphenols, tocopherols, and high-oleic goose fat fraction at 60~80℃; 4) Stir thoroughly under an inert atmosphere; 5) Cooling and filtration yields a biomimetic sebum film composite oil base material specifically for cosmetics.

10. A color cosmetic composition, characterized in that... It comprises the base material, colorant, and wax as described in any one of claims 1 to 7.

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