Tea fermentation energy composition with anti-wrinkle and repairing functions and application of tea fermentation energy composition
Through the synergistic combination of black tea fermentation liquid, Artemia extract and hydrolyzed sodium hyaluronate, the problems of low transdermal absorption efficiency of black tea fermentation liquid, poor stability of Artemia extract and functional limitations of hydrolyzed sodium hyaluronate are solved, achieving multi-pathway synergistic anti-wrinkle and barrier repair, and improving the anti-wrinkle repair effect of cosmetics.
Patent Information
- Application Number
- CN202510916942.2
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-07-03
- Publication Date
- 2025-10-17
AI Technical Summary
In the existing technology, the transdermal absorption efficiency of black tea fermentation liquid is low, the stability of Artemia extract is poor and its function is single, and the function of hydrolyzed sodium hyaluronate is limited, resulting in its skin care value in the cosmetics field not being maximized.
Provided is a tea fermentation energy composition, which is a synergistic combination of black tea fermentation liquor, Artemia extract and hydrolyzed sodium hyaluronate. Through multi-pathway synergistic anti-wrinkle, barrier repair and 3D repair anti-wrinkle pathways, it achieves microecological regulation of black tea fermentation liquor, repair of Artemia extract and penetration enhancement of hydrolyzed sodium hyaluronate.
It achieves multi-pathway synergistic anti-wrinkle, strengthens barrier repair, opens up 3D repair anti-wrinkle pathways, has strong anti-wrinkle and repair effects, and improves the skin care effect of cosmetics.
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Figure CN120788967A_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The present application relates to the field of cosmetics, in particular to a tea fermentation energy composition with anti-wrinkle repair and application thereof. BACKGROUND
[0002] The black tea fermentation liquor contains tea polyphenols, theaflavins, flavonoids and other components. Tea polyphenols have antioxidant properties and can strongly scavenge free radicals, reducing the oxidative damage of free radicals to skin cells, thereby delaying skin aging and reducing the formation of wrinkles and fine lines. It also contains a variety of anti-inflammatory active ingredients such as tannic acid and polysaccharides. Tannic acid has astringent properties and can reduce edema and exudation at the inflammation site. It can also inhibit the release of inflammatory mediators such as prostaglandins and leukotrienes, thereby reducing inflammation. The polyphenols enriched in black tea fermentation liquor are exogenous antioxidants that mainly scavenge free radicals in the epidermis and are difficult to directly act on the cell repair pathway in the dermis, achieving a deep anti-aging effect. When used alone, it has weak effects on improving deep wrinkles and skin laxity.
[0003] Brine shrimp (ARTEMIA) extract is rich in various nutritional components and bioactive substances, with protein, amino acids, unsaturated fatty acids, vitamins and minerals as the core components. The components in brine shrimp extract such as GP4G and stress proteins (such as HSP70) can target mitochondria to enhance cell energy metabolism and have certain antioxidant effects, which can scavenge free radicals in the skin, slow down the aging process of the skin and prevent the formation of wrinkles and laxity. Amino acids are the basic units of proteins and can participate in skin metabolism, promote cell repair and regeneration, and help improve skin texture and elasticity. Unsaturated fatty acids can form a protective film on the skin surface, reduce water loss, enhance the skin's moisture retention capacity, and keep the skin in a moist state. However, the stability of brine shrimp extract is poor because its core components are stress proteins, astaxanthin and GP4G (tetraphosphodi guanosine). Stress proteins have the natural vulnerability of proteins and are prone to denaturation under high temperature or acidic and alkaline conditions. Astaxanthin has a molecular structure with many long conjugated unsaturated double bonds, which is sensitive to light and high temperature. GP4G has four phosphate groups and is prone to hydrolysis. Therefore, when used alone, it has low compatibility with acidic or strongly basic ingredients and can only reduce damage but cannot promote the synthesis of new collagen.
[0004] Hydrolyzed sodium hyaluronate is a small molecule product obtained by treating sodium hyaluronate through a hydrolysis process, which can penetrate the stratum corneum, combine with water molecules to increase the water content of the skin, and prevent damage to the barrier caused by water deficiency. Low molecular weight sodium hyaluronate can also promote collagen signaling, reduce collagen degradation, and induce the synthesis of type III collagen. In addition, it also has the synergistic effect of a carrier, reduces the density of the stratum corneum through a water-rich environment, and improves the penetration efficiency of other ingredients. When used alone, hydrolyzed sodium hyaluronate does not have antioxidant and anti-aging activities, and is mainly used as a moisturizing agent. Its mechanism is to exogenously supplement water, which is difficult to improve the skin's self-repairing ability. Moreover, it does not involve the positive regulation of collagen synthesis or the inhibition of inflammatory factors, and the anti-aging pathway is missing.
[0005] In summary, the above three alone cannot maximize their skin care value in the field of cosmetics. SUMMARY
[0006] The purpose of the present application is to overcome the shortcomings of the prior art and provide a tea fermentation energy composition with anti-wrinkle repair and its application.
[0007] To achieve the above-mentioned purpose, the technical scheme adopted by the present application is:
[0008] In a first aspect, the present application provides a tea fermentation energy composition with anti-wrinkle repair, which is composed of the following ingredients by weight: 2-10 parts of black tea fermentation liquor, 0.1-3 parts of halocyprid extract, and 0.05-1 part of hydrolyzed sodium hyaluronate.
[0009] In view of the problems of low transdermal absorption efficiency of black tea fermentation liquor, poor stability of halocyprid extract, and single anti-aging pathway of hydrolyzed sodium hyaluronate in the prior art, a synergistic composition is provided by combining red tea fermentation liquor (microecological regulation combined with antioxidant), halocyprid extract (repair combined with collagen promotion), and hydrolyzed sodium hyaluronate (penetration synergism combined with moisturizing), which achieves the following technical effects:
[0010] 1. Multi-pathway synergistic anti-wrinkle:
[0011] ① Tea polyphenols in black tea fermentation liquor scavenge free radicals, inhibit MMP-1 enzyme, and prevent newly formed collagen from being degraded; ② Anti-stress proteins in halocyprid extract repair DNA damage and promote cell synthesis of type I collagen through the TGF-β pathway; ③ Hydrolyzed sodium hyaluronate induces collagen synthesis, and combines with water to keep collagen fibers elastic, delay relaxation, and form an anti-wrinkle network.
[0012] 2. Barrier repair and strengthening:
[0013] Black tea fermentation liquid adjusts skin microflora and pH; anti-stress protein (HSP70) in Artemia extract acts as a "molecular radar" to reduce inflammatory factors (such as IL-6) and reduce the risk of barrier damage, and amino acids provide raw materials for barrier structure repair; hydrolyzed sodium hyaluronate maintains a moist environment and constructs an anti-wrinkle repair closed loop.
[0014] 3. Open up the 3D repair anti-wrinkle pathway:
[0015] The polyphenols in black tea fermentation liquid scavenge epidermal free radicals, and the small molecules of sodium hyaluronate penetrate and soften the keratin, thereby improving the transdermal rate of black tea fermentation liquid / Artemia extract. The anti-stress protein (HSP70) in Artemia extract inhibits the activity of MMP-1 enzyme and reduces collagen degradation; GP4G (tetraphosphodi guanosine) enters the dermis and decomposes energy substances ATP, thereby promoting collagen synthesis. That is, the pathway is: epidermal free radical scavenging→shallow layer collagen degradation reduction→deep layer collagen fiber formation promotion.
[0016] All of them have antioxidant properties, and after scientific proportioning, they have strong anti-wrinkle and repair efficacy, which can bring new possibilities for the application of cosmetics.
[0017] Meanwhile, the combination of the black tea fermentation liquid, Artemia extract and hydrolyzed sodium hyaluronate has a synergistic effect. If the Artemia extract is replaced by Chlorella extract or the hydrolyzed sodium hyaluronate is replaced by acetylated sodium hyaluronate in the tea fermentation energy composition of the present application, the effect of the corresponding composition will be reduced. The "tea fermentation energy" of the present application refers to a composition containing black tea fermentation liquid (i.e. tea fermentation) and Artemia extract which can provide cell energy.
[0018] As a preferred embodiment of the tea fermentation energy composition of the present application, the tea fermentation energy composition is composed of the following ingredients in parts by weight: 6-10 parts of black tea fermentation liquid, 2-3 parts of Artemia extract and 0.05-0.5 parts of hydrolyzed sodium hyaluronate. The effect of the composition in this range is better.
[0019] As a preferred embodiment of the tea fermentation energy composition of the present application, the tea fermentation energy composition is composed of the following ingredients in parts by weight: 10 parts of black tea fermentation liquid, 2 parts of Artemia extract and 0.5 parts of hydrolyzed sodium hyaluronate.
[0020] As a preferred embodiment of the tea fermentation energy composition of the present application, the black tea fermentation liquid includes golden flower black tea fermentation liquid, yeast and acetic acid bacillus black tea fermentation liquid or Eurotium cristatum K8824 and yeast black tea fermentation liquid.
[0021] The golden flower black tea fermentation liquid, i.e. the fermentation liquid obtained by fermenting black tea with Eurotium cristatum complex bacterial species, such as the golden flower black tea fermentation liquid of Bozhou Mingqi Biological Technology Co., Ltd.
[0022] The yeast and the wood vinegar bacillus black tea fermentation liquor, i.e., the fermentation liquor obtained by fermenting black tea with yeast and wood vinegar bacillus, such as the black tea fermentation liquor of Dongguan Juxin New Material Technology Co., Ltd.
[0023] The Eurotium cristatum K8824 and the yeast black tea fermentation liquor, i.e., the fermentation liquor obtained by fermenting black tea and sea buckthorn leaves with Eurotium cristatum K8824 and yeast, such as the black tea fermentation liquor obtained by fermenting black tea and sea buckthorn leaves with Eurotium cristatum K8824 and yeast according to the method disclosed in CN119818402A.
[0024] In a second aspect, the present application provides a use of the tea fermentation energy composition in the preparation of a cosmetic product.
[0025] In a third aspect, the present application provides a cosmetic product comprising the tea fermentation energy composition and an auxiliary material.
[0026] As a preferred embodiment of the cosmetic product of the present application, the cosmetic product comprises a cleansing product, a cosmetic water, a cream or a mask. The cream comprises a lotion or a cream.
[0027] In a fourth aspect, the present application provides a lotion comprising the tea fermentation energy composition 2.15% to 14%, an auxiliary material 23.02% to 30.45% and water in remainder by weight percentage.
[0028] As a preferred embodiment of the lotion of the present application, the lotion comprises black tea fermentation liquor 2% to 10%, artemia extract 0.1% to 3%, hydrolyzed sodium hyaluronate 0.05% to 1%, an auxiliary material 23.02% to 30.45% and water in remainder by weight percentage.
[0029] As a preferred embodiment of the lotion of the present application, the auxiliary material comprises one or more of a skin conditioning agent, a humectant, an emulsifier, a chelating agent, a preservative or a thickening agent.
[0030] As a preferred embodiment of the lotion of the present application, the skin conditioning agent comprises one or more of caprylic / capric triglyceride, hydrogenated polyisobutene, cyclopentasiloxane, dimethicone or cetearyl alcohol; the chelating agent is disodium EDTA; the humectant comprises one or more of glycerin, butylene glycol, 1,2-hexanediol or dipropylene glycol; the preservative comprises one or both of phenoxyethanol or ethylhexylglycerin; the emulsifier comprises one or both of PEG-100 stearate or glyceryl stearate; and the thickening agent comprises one or both of xanthan gum or carbomer.
[0031] As a preferred embodiment of the emulsion of the present application, the emulsion comprises the tea ferment energy composition 2.15% to 14%, humectant 9% to 10%, thickening agent 0.3% to 0.45%, chelating agent 0.02% to 0.1%, emulsifier 1% to 3%, skin conditioning agent 12% to 16%, preservative 0.7% to 0.9% and water in balance, by weight percentage.
[0032] As a preferred embodiment of the emulsion of the present application, the emulsion comprises the tea ferment energy composition 2.15% to 14%, glycerin 3% to 5%, butylene glycol 2% to 3%, dipropylene glycol 1% to 3%, 1,2-hexanediol 0.5% to 1%, xanthan gum 0.2% to 0.4%, carbomer 0.05% to 0.2%, disodium EDTA 0.02% to 0.1%, PEG-100 stearate 1% to 2%, glyceryl stearate 1% to 1.5%, caprylic / capric triglyceride 3% to 5%, hydrogenated polyisobutene 2% to 3%, cyclopentasiloxane 2% to 4%, dimethicone 2% to 4%, cetearyl alcohol 1% to 2%, phenoxyethanol 0.2% to 0.8%, ethylhexylglycerin 0.1% to 0.5% and water in balance, by weight percentage.
[0033] As a preferred embodiment of the emulsion of the present application, the emulsion comprises the tea ferment energy composition 2.15% to 14%, glycerin 3% to 5%, butylene glycol 2% to 3%, dipropylene glycol 1% to 3%, 1,2-hexanediol 0.5% to 1%, xanthan gum 0.2% to 0.4%, carbomer 0.05% to 0.2%, disodium EDTA 0.02% to 0.1%, PEG-100 stearate 1% to 2%, glyceryl stearate 1% to 1.5%, caprylic / capric triglyceride 3% to 5%, hydrogenated polyisobutene 2% to 3%, cyclopentasiloxane 2% to 4%, dimethicone 2% to 4%, cetearyl alcohol 1% to 2%, phenoxyethanol 0.2% to 0.8%, ethylhexylglycerin 0.1% to 0.5% and water in balance, by weight percentage.
[0034] In a fifth aspect, the present application provides a preparation method of the above-mentioned emulsion, comprising the following steps:
[0035] S1, mix the skin conditioning agent and the emulsifier, heat to 75°C to 80°C, dissolve until completely transparent, to obtain an oil phase mixture.
[0036] S2, after heating the water to 75°C to 80°C, add the humectant, chelating agent and thickening agent, mix until no particles, to obtain an aqueous phase mixture.
[0037] S3, mix the oil phase mixture and the aqueous phase mixture, homogenize, mix well under stirring, cool to 42 to 48°C, adjust the pH value to 5.8 to 6.2, to obtain a water-oil mixture auxiliary material.
[0038] S4, the water-oil mixed adjuvant is mixed with the hydrolyzed sodium hyaluronate, and after being uniformly dissolved, the temperature is reduced to 35-40 DEG C, a preservative is added, and then mixed uniformly; then, the black tea fermentation liquor and the Artemia extract are added and mixed uniformly. The temperature is reduced to 30-35 DEG C, and then filtered to obtain the emulsion.
[0039] As a preferred embodiment of the preparation method of the emulsion of the present application, in step S2, if the thickening agent is xanthan gum, the xanthan gum is first dispersed into a xanthan gum moisturizing agent (glycerol) solution with part of the moisturizing agent (glycerol). The weight ratio of the xanthan gum to the moisturizing agent (glycerol) is 0.2:1.
[0040] As a preferred embodiment of the preparation method of the emulsion of the present application, in step S2, the mixing is performed at 800-1200 rpm (high speed) for 20 min.
[0041] In step S3, the homogenization is performed at 2200-2800 rpm for 5 min, and the stirring is performed at 75-80 DEG C for 10 min and then at 600-1000 rpm for 10 min.
[0042] In step S4, the uniform dissolution is performed by stirring at 800-1000 rpm for 10 min, and after the addition of the preservative, the stirring is performed at 600-1000 rpm for 10 min to mix uniformly; the black tea fermentation liquor and the Artemia extract are added, and the stirring is performed at 300 rpm for 15 min to mix uniformly. The room temperature is below 35 DEG C, and the filtering is performed with a mesh size of 100.
[0043] As a preferred embodiment of the preparation method of the emulsion of the present application, in step S3, the pH adjustment is performed with 10% triethanolamine aqueous solution; the hydrolyzed sodium hyaluronate is first dispersed with the moisturizing agent butanediol before being added; and the Artemia extract is first dispersed with the moisturizing agent 1,2-hexanediol before being added.
[0044] By reducing the obtained emulsion crude product to about 45 DEG C (42-48 DEG C), and adjusting the pH to the interval of 5.5-6.5 with 10% triethanolamine aqueous solution, and then adding the hydrolyzed sodium hyaluronate pre-dispersed with appropriate butanediol, and then adding the Artemia extract pre-dispersed with 1,2-hexanediol and the black tea fermentation liquor, the stability of the obtained emulsion can be better improved, and the efficacy of the composition can be maximally reserved.
[0045] As a preferred embodiment of the preparation method of the emulsion of the present application, the hydrolyzed sodium hyaluronate is pre-dispersed uniformly with 3 times its weight of butanediol; and the Artemia extract is pre-dispersed uniformly with 3 times its weight of 1,2-hexanediol.
[0046] Compared with the prior art, the present application has the following beneficial effects:
[0047] The tea fermentation energy composition of the present application utilizes the synergistic effect of black tea fermentation liquor, Artemia extract and hydrolyzed sodium hyaluronate to achieve multi-pathway synergistic anti-wrinkle, strengthen barrier repair, and open up the 3D repair anti-wrinkle pathway. Compared with other substances with similar functions, the combination of black tea fermentation liquor, Artemia extract and hydrolyzed sodium hyaluronate has better anti-wrinkle and repair functions. It can bring new choices for the application of cosmetics. BRIEF DESCRIPTION OF DRAWINGS
[0048] Figure 1 The fluorescence pictures corresponding to the tests of the tea fermentation energy compositions of examples 1, 5 and 9 in test example 5 of the present application;
[0049] Figure 2 The EDU relative fluorescence intensity column chart corresponding to the tests of the tea fermentation energy compositions of examples 1, 5 and 9 in test example 5 of the present application. DETAILED DESCRIPTION
[0050] In order to better illustrate the purpose, technical scheme and advantages of the present application, the present application will be further described below in combination with specific examples.
[0051] Unless otherwise specified, other materials, reagents, etc. used in the examples can be obtained from commercial channels.
[0052] The black tea fermentation liquor is a liquid, which is purchased from Bozhou Mingqi Biological Technology Co., Ltd. and Dongguan Juxi New Material Technology Co., Ltd.
[0053] The Artemia extract is a powder, which is purchased from Shaanxi Haichen Health Biological Technology Co., Ltd.
[0054] The hydrolyzed sodium hyaluronate is a powder, which is purchased from Guangzhou SnuoKe Biological Technology Co., Ltd.
[0055] Examples 1-14 and comparative examples 1-6
[0056] The composition components of the tea fermentation energy compositions of examples 1-14 are shown in Table 1-1 below, examples 13 and 14 are the same as example 12; the composition components of the compositions of comparative examples 1-6 are shown in Table 1-2 below,
[0057] Table 1-1
[0058]
[0059]
[0060] Table 1-2
[0061]
[0062] The black tea fermentation liquor in the tea fermentation energy compositions of Examples 1-12, Comparative Examples 1, 4-6 was Jinhua black tea fermentation liquor (Bozhou Mingqi Biotechnology Co., Ltd.); the black tea fermentation liquor in the tea fermentation energy composition of Example 13 was the black tea fermentation liquor obtained by fermenting black tea and sea buckthorn leaves with Eurotium cristatum K8824 and yeast according to the method described in CN119818402A (co-researched by Guangzhou Zhongzhuangmei Industry and All-China Federation of Supply and Marketing Cooperatives Hangzhou Tea Research Institute); the black tea fermentation liquor in the tea fermentation energy composition of Example 14 was the black tea fermentation liquor obtained by fermenting black tea with yeast and acetic acid bacteria (Dongguan Juxin New Material Technology Co., Ltd.).
[0063] Test Example 1
[0064] The pH values and colors of the tea fermentation energy compositions of Examples 1-14 were determined.
[0065] The pH values were tested by a pH tester, and the colors of the compositions were observed by pouring the samples into transparent sample bottles, and the test results are shown in Table 2 below,
[0066] Table 2
[0067] Sample pH Color Sample pH Color Example 1 6.20 Light yellow Example 8 6.26 Light yellow Example 2 6.26 Light yellow Example 9 6.31 Yellow Example 3 6.30 Yellow Example 10 6.19 Light yellow Example 4 6.22 Light yellow Example 11 6.27 Light yellow Example 5 6.27 Light yellow Example 12 6.29 Yellow Example 6 6.28 Yellow Example 13 6.28 Yellow Example 7 6.21 Light yellow Example 14 6.30 Yellow
[0068] The results in Table 2 show that the pH values of the prepared tea fermentation energy compositions 1-14 meet the provisions in the “Cosmetic Safety Technology Specifications” (2015 Edition). The colors of the tea fermentation energy compositions are yellow.
[0069] Test Example 2
[0070] The safety was tested by patch test. Test samples: tea fermentation energy compositions of Examples 1-14 (mixing the components according to the proportions).
[0071] Subjects: A total of 42 people, 16 men and 26 women, aged 22-45 years, with an average age of 28.3±3.2 years, meeting the subject volunteer selection criteria. Divided into A and B groups, 21 people in group A tested Examples 1-7 and the blank control group, and 21 people in group B tested Examples 8-14 and the blank control group.
[0072] The patch test method is as follows:
[0073] Select qualified patch test materials, and use the closed patch test method to test the patching products containing the test samples (cut into the size of the patch test device, about 50 mm 2) were placed in the patch tester, and the outer low-sensitization adhesive tape was attached to the back of the subject. After 24 hours, the test sample was removed, and the skin reaction was observed at 0.5, 24, and 48 hours after removal, respectively. A blank control (blank, without treatment) was set. The results were recorded according to the skin reaction grading standard in Chapter 7 of the Cosmetic Safety Technical Specifications (2015 Edition). The tea ferment energy compositions of Examples 1-14 were safe, and the safety patch test results are shown in Table 3 below,
[0074] Table 3
[0075]
[0076]
[0077] Test Example 3
[0078] Elastase test
[0079] 1. Principle of experiment: Collagen forms collagen fibers and reticular fibers, and elastin forms elastic fibers. These three fibers together constitute the connective tissue of the skin, forming a structure that is full and elastic. Elastase has the ability to decompose collagen, elastin, and other proteins. Changes in the structure of elastin are closely related to skin aging. The enzyme label instrument is used to detect the inhibitory effect of the test sample on the catalysis of the substrate by elastase, to determine whether the test sample has the ability to inhibit elastase.
[0080] 2. Reagents and materials: 30 U / mg elastase (porcine trypsin), N-succinyl-alanine-alanine-alanine-p-nitroaniline, Tris, concentrated hydrochloric acid, and epigallocatechin gallate (EGCG).
[0081] 3. Determination steps:
[0082] (1) Preparation of solutions:
[0083] ① 0.2 mol / L Tris-HCl buffer solution (buffer) with pH 8.0: accurately weigh 4.8456 g of Tris particles, add 100 mL of deionized water, stir to dissolve, and obtain a 0.4 mol / L Tris solution (solution A); take 3.34 mL of concentrated hydrochloric acid, dilute with 96.66 mL of deionized water, and obtain a 0.4 mol / L HCl solution (solution B); mix 100 mL of solution A and 44.76 mL of solution B, adjust the pH to 8.0, and add deionized water to make up to 200 mL, to obtain the buffer solution.
[0084] ② Elastase solution (enzyme solution): prepared with the above buffer solution, 0.033 g of elastase was added to 10 mL of the buffer solution to prepare 100 U / mL of elastase solution, which was prepared immediately before use.
[0085] ③ Substrate solution: 1.8057 mg of N-succinyl-alanine-alanine-alanine-p-nitroaniline was weighed and dissolved in 10 mL of the above buffer solution to obtain 0.18057 mg / mL of N-succinyl-alanine-alanine-alanine-p-nitroaniline solution.
[0086] ④ Positive control: EGCG solution: 0.001 g of EGCG powder was weighed and dissolved in 1 mL of the above buffer solution to prepare 1.0 mg / mL of EGCG solution, which was diluted with the buffer solution to obtain 0.5, 0.1, 0.01, 0.005, 0.003, 0.002, and 0.001 mg / mL of EGCG solution, respectively.
[0087] (2) Preparation of sample solution:
[0088] The tea ferment energy compositions of Examples 1-14 and the compositions of Comparative Examples 1-6 were each prepared into a sample solution according to Table 4:
[0089] Table 4
[0090] Composition / (μL) Sample solution Enzyme solution Substrate solution Buffer A-sample group 50 50 100 / B-sample control group 50 50 / 100 C-blank group / 50 100 50 D-blank control group / 50 / 150
[0091] (3) Each solution was added to a 96-well plate according to Table 4, and incubated at room temperature for 60 min. The absorbance was measured at 410 nm using a microplate reader, and the data was recorded and saved. The elastase inhibition rate was calculated according to Formula (I),
[0092] Formula (I): Elastase inhibition rate (%) = [1 - (OD A - OD B ) / (OD C - OD D )] x 100%,
[0093] In Formula (I), OD A is the absorbance value of the sample group (containing enzyme and substrate);
[0094] OD B is the absorbance value of the sample control group (containing enzyme but not containing substrate);
[0095] OD C is the absorbance value of the blank group (containing enzyme and substrate but not containing sample);
[0096] OD D is the absorbance value of the blank control group (containing enzyme but not containing substrate and sample).
[0097] 4. Precision: The absolute difference between two independent results obtained under repeatability conditions shall not exceed 10% of the arithmetic mean.
[0098] The results of the elastase inhibition rate test are shown in Table 5 below,
[0099] Table 5
[0100] Sample Elastase inhibition rate (%) Sample Elastase inhibition rate (%) Example 1 27.32±1.36 Example 11 67.91±0.29 Example 2 33.97±0.51 Example 12 77.82±1.24 Example 3 40.93±1.13 Example 13 76.25±0.78 Example 4 46.37±0.35 Example 14 77.45±0.52 Example 5 53.73±0.86 Comparative Example 1 13.32±0.68 Example 6 57.89±0.83 Comparative Example 2 15.32±0.82 Example 7 60.49±0.39 Comparative Example 3 10.32±0.35 Example 8 68.25±1.43 Comparative Example 4 23.12±0.24 Example 9 70.89±0.52 Comparative Example 5 22.09±1.53 Example 10 50.97±0.46 Comparative Example 6 20.24±0.93
[0101] The results of Table 5 show that the tea fermentation energy compositions of the examples can significantly inhibit elastase, i.e. have good anti-wrinkle efficacy. The tea fermentation energy composition of Example 12 has the best effect, i.e. the optimal ratio of the tea fermentation energy composition is 10 parts of black tea fermentation liquor, 2 parts of Artemia extract and 0.5 parts of hydrolyzed sodium hyaluronate. The sum of the elastase inhibition rates of Comparative Examples 1, 2 and 3 is less than that of Example 12, indicating that the combination of black tea fermentation liquor, Artemia extract and hydrolyzed sodium hyaluronate has a synergistic effect. The content of the three components in Comparative Example 4 exceeds the range of the examples, and the corresponding elastase inhibition rate is only 23.12%, which is lower than that of Examples 1-14. In Comparative Example 5, acetylated sodium hyaluronate is used to replace hydrolyzed sodium hyaluronate, and the elastase inhibition rate is only 22.09%, which is lower than that of Example 12. In Comparative Example 6, Chlorella extract is used to replace Artemia extract, and the elastase inhibition rate is only 20.24%, which is lower than that of Example 12.
[0102] Application Example
[0103] The tea fermentation energy compositions of the examples are combined with excipients to prepare emulsions.
[0104] An emulsion, by weight percentage, comprises 2.15%-14% of the tea fermentation energy composition described above, 23.02%-30.45% of excipients and the balance of deionized water.
[0105] The excipients include one or more of skin conditioning agents, humectants, emulsifiers, chelating agents, preservatives or thickening agents; the skin conditioning agents include one or more of caprylic / capric triglyceride, hydrogenated polyisobutene, cyclopentasiloxane, dimethicone or cetearyl alcohol; the chelating agent is disodium EDTA; the humectants include one or more of glycerin, butylene glycol, 1,2-hexanediol or dipropylene glycol; the preservatives include one or both of phenoxyethanol or ethylhexylglycerin; the emulsifiers include one or both of PEG-100 stearate or glyceryl stearate; and the thickening agents include one or both of xanthan gum or carbomer.
[0106] The composition components of the emulsions 1-14 are shown in Table 6 below,
[0107] Table 6
[0108]
[0109]
[0110] Comparative emulsion 1: same as emulsion 12, the only difference is that the active is replaced by 10% of red tea fermentation liquor.
[0111] Comparative emulsion 2: same as emulsion 12, the only difference is that the active is replaced by 2% of artemia extract.
[0112] Comparative emulsion 3: same as emulsion 12, the only difference is that the active is replaced by 0.5% of hydrolyzed sodium hyaluronate.
[0113] Comparative emulsion 4: same as emulsion 12, the only difference is that the active is replaced by 20% of red tea fermentation liquor, 4% of artemia extract, and 2% of hydrolyzed sodium hyaluronate.
[0114] Comparative emulsion 5: same as emulsion 12, the only difference is that the active is replaced by 10% of red tea fermentation liquor, 2% of artemia extract, and 0.5% of acetylated sodium hyaluronate.
[0115] Comparative emulsion 6: same as emulsion 12, the only difference is that the active is replaced by 10% of red tea fermentation liquor, 2% of chlorella extract, and 0.5% of hydrolyzed sodium hyaluronate.
[0116] The preparation method of the emulsions 1-11, 13-14 includes the following steps:
[0117] S1, put caprylic / capric triglyceride, hydrogenated polyisobutylene, cyclopentadimethyl siloxane, dimethyl silicone, cetyl stearyl alcohol, glyceryl stearate, PEG-100 stearate into the oil phase pot, heat to 75-80℃, stir until completely dissolved and transparent to obtain an oil phase mixture.
[0118] S2, pre-disperse xanthan gum with glycerol to obtain a xanthan gum glycerol solution, the weight ratio of xanthan gum to glycerol being 0.2:1; then heat deionized water to 75-80℃, add butylene glycol, dipropylene glycol, 1,2-hexanediol, disodium EDTA, the xanthan gum glycerol solution, carbomer (slowly added), and the remaining portion of glycerol, and stir at a high speed of 800-1200 rpm for 20 min until no particles are present to obtain an aqueous phase mixture.
[0119] S3, slowly draw the oil phase mixture into the aqueous phase mixture, homogenize at 2200-2800 rpm for 5 min, and keep the temperature at 75℃ for 10 min while stirring at 600-1000 rpm. Cool to 42-48℃, adjust the pH value to 5.8-6.2, and obtain a water-oil mixture auxiliary material.
[0120] S4, the hydrolyzed sodium hyaluronate is uniformly pre-dispersed with 3 times its weight of butanediol; the Artemia extract is uniformly pre-dispersed with 3 times its weight of 1,2-hexanediol; the hydrolyzed sodium hyaluronate is slowly added to the water-oil mixing auxiliary material, and stirred at 800-1000 rpm for 10 min until dissolved uniformly; then, the temperature is lowered to 35-40°C, the preservative (phenoxyethanol, ethylhexylglycerin) is added, and stirred at 600-1000 rpm for 10 min until mixed uniformly; then, the black tea fermentation liquor and the Artemia extract are added, and stirred at a low speed of 300 rpm for 15 min until mixed uniformly. The temperature is lowered to 30-35°C, and filtered through a 100-mesh sieve to obtain the emulsion.
[0121] The preparation method of the emulsion 12 and the comparative emulsions 1-6 includes the following steps:
[0122] S1, the caprylic / capric triglyceride, hydrogenated polyisobutylene, cyclopentasiloxane, dimethicone, cetyl stearyl alcohol, glyceryl stearate, and PEG-100 stearate are put into an oil phase pot, heated to 80°C, and stirred until completely dissolved and transparent to obtain an oil phase mixture.
[0123] S2, the xanthan gum is pre-dispersed with glycerol to obtain a xanthan gum glycerol solution, and the weight ratio of the xanthan gum to the glycerol is 0.2:1; then, the deionized water is heated to 80°C, and then the butanediol, dipropylene glycol, 1,2-hexanediol, disodium EDTA, the xanthan gum glycerol solution, carbomer (slowly added), and the remaining portion of glycerol are added, and stirred at a high speed of 1200 rpm for 20 min until no particles are present to obtain an aqueous phase mixture.
[0124] S3, the oil phase mixture is slowly drawn into the aqueous phase mixture, homogenized at 2600 rpm for 5 min, and stirred at 75°C for 10 min under the stirring condition of 800 rpm. The temperature is lowered to 45°C, the pH value is adjusted to 6.0, and an oil-water mixing auxiliary material is obtained.
[0125] S4, the hydrolyzed sodium hyaluronate (or acetylated sodium hyaluronate) is uniformly pre-dispersed with 3 times its weight of butanediol; the Artemia extract is uniformly pre-dispersed with 3 times its weight of 1,2-hexanediol; the hydrolyzed sodium hyaluronate (or acetylated sodium hyaluronate) is slowly added to the oil-water mixing auxiliary material, and stirred at 800 rpm for 10 min until dissolved uniformly; then, the temperature is lowered to 35°C, the preservative (phenoxyethanol, ethylhexylglycerin) is added, and stirred at 800 rpm for 10 min until mixed uniformly; then, the black tea fermentation liquor and the Artemia extract (or Chlorella extract) are added, and stirred at a low speed of 300 rpm for 15 min until mixed uniformly. The temperature is lowered to 30°C, and filtered through a 100-mesh sieve to obtain the emulsion.
[0126] The pH values of the prepared emulsions 1-14 meet the requirements in the Cosmetics Safety Technical Specifications (2015 edition).
[0127] Test Example 4
[0128] Stability test.
[0129] Test samples: tea ferment energy compositions of Examples 1-14, application example emulsions 1-14.
[0130] Composition or emulsion, stability test, specific test method as follows:
[0131] Normal temperature test group, 25℃ normal temperature for 3 months;
[0132] Heat resistance test group, 40℃-45℃ high temperature for 3 months;
[0133] Cold resistance test group, -15℃--10℃ low temperature for 3 months;
[0134] Observe test samples on the 7th day, 30th day, 60th day, 90th day after treatment, and the observation items are the appearance state, color, odor of the test samples.
[0135] The tea ferment energy compositions of Examples 1-14 and the application example emulsions 1-14 have good stability at low temperature, normal temperature and high temperature, and can all meet the stability requirements of the Cosmetic Safety Technical Specifications (2015 edition). The stability test results of emulsion 12 and the tea ferment energy composition of Example 12 are shown in Tables 7-1 and 7-2.
[0136] Table 7-1
[0137]
[0138] Table 7-2
[0139]
[0140] Test Example 5
[0141] Cell proliferation test (EDU555) was carried out with the tea ferment energy compositions of Examples 1-14 as drugs.
[0142] Experimental instrument: fluorescence microscope (Olympus), experimental reagent: EdU-555 cell proliferation detection kit (Bi Yun Tian).
[0143] Cell line: HFB cells; culture solution: high-sugar DMEM culture medium containing 10% fetal bovine serum; culture conditions: 37℃, 5% CO2, saturated humidity conditions. The negative control group (Control) replaces the corresponding drug with an equal amount of deionized water.
[0144] EDU working solution: 5-ethynyl-2'-deoxyuridine; EDU detection solution: Click Reaction Buffer: CuSO4: Azide 555: Click Additive Solution = 430 μL: 20 μL: 1 μL: 50 μL.
[0145] Experimental steps:
[0146] HFB cells were seeded in 96-well cell culture plates at 1.0 x 10 5 cells / mL, 100 μL per well, and 6000 cells per well, and incubated in a 37°C cell culture incubator for 24 h. After the cells adhered, the corresponding drugs were incubated for 24 h, and 100 μL of the drugs was added to each well of the 96-well plate.
[0147] The drug medium was removed, and the cells were washed twice with PBS. Then the cells were fixed with 4% paraformaldehyde for 5 min, and DAPI staining solution was diluted to a final concentration of 50 μmol / L, 100 μL was added to each well, and the cells were stained at room temperature for 20 min in the dark. After washing with PBS, the cell morphology was observed under a fluorescence microscope. EDU working solution at 10 μM was added to label the cells for 2 h, and the EDU reaction, staining, and other steps were performed according to the EDU cell proliferation detection kit instructions, and then the cells were observed under a fluorescence microscope. Through the co-localization of DAPI nuclear staining (blue) and EdU-555 dye (red), the cells were accurately identified.
[0148] The EDU relative fluorescence intensity test results are shown in Table 8. The greater the EDU fluorescence intensity, the more active the cell proliferation. The fluorescence pictures corresponding to the tests of the tea fermentation energy compositions of Examples 1, 5, and 9 are shown in Figure 1 , the bar graphs of the EDU relative fluorescence intensity corresponding to the tests of the tea fermentation energy compositions of Examples 1, 5, and 9 are shown in Figure 2 , and
[0149] Table 8
[0150]
[0151]
[0152] The results in Table 8 show that the EDU relative fluorescence intensity of the composition of Example 12 is higher than that of the negative control group, indicating that the composition has the best effect on promoting the proliferation of human skin fibroblasts, and that the tea fermentation energy composition has a significant cell proliferation effect, i.e., good cell repair efficacy.
[0153] Test Example 6
[0154] Human anti-wrinkle and repair barrier efficacy test
[0155] Recruit 100 volunteers, 5 people in each group, a total of 20 groups, respectively using the application example of the emulsion 28 days, through the skin water loss tester test volunteer skin transepidermal water loss rate (TEWL) and skin fast optical imaging system test volunteer skin wrinkle parameters, the average value of each group.
[0156] 1. Volunteer inclusion criteria:
[0157] ① 35-55 year-old Chinese healthy women (at the beginning of the trial);
[0158] ② Dry and dull, rough, wrinkled skin on the face;
[0159] ③ Poor facial skin barrier, easy to blush, loose skin;
[0160] ④ Can be well coordinated to use the sample, understand and fill in the project questionnaire and cooperate with the staff;
[0161] ⑤ Can be well coordinated with the test, can maintain the regularity of life during the study period;
[0162] ⑥ Can read and understand all the contents of the informed consent form, and voluntarily sign the informed consent form;
[0163] ⑦ Agree not to use any cosmetics, drugs and health products that affect the results during the trial period.
[0164] 2. Exclusion criteria:
[0165] ① Have allergic constitution, allergic dermatitis, etc., have a history of skin disease or disease (serious freckles, atopic dermatitis, psoriasis, eczema, severe acne, etc.), and personnel who are not suitable for participating in the project according to clinical evaluation;
[0166] ② There are large areas of birthmarks, scratches, leukoplakia, pigmented nevi, scar nodules and other skin manifestations that affect the test on the test site;
[0167] ③ Pregnant, lactating, menopausal or fertile women;
[0168] ④ Within two months, the test site has used any anti-inflammatory drugs;
[0169] ⑤ Participated in other clinical trials within 2 months;
[0170] ⑥ The test responsible person judges that the population is not suitable for the test.
[0171] During the trial, volunteers should maintain the same lifestyle and eating habits as before participating in the trial; prohibited from treating the test site that affects the test; prohibited from using other skin care products and other products that affect the test; daily necessities should be consistent with those used before the trial began, and should not be replaced.
[0172] 3. Test method
[0173] Environmental requirements: temperature, 21.0 ± 1.0 °C; humidity, 50% ± 10%.
[0174] Test instruments: Tewameter TM300 (Courage + Khazaka, Germany), skin rapid optical imaging system PRIMOS CR (CANFIELD, USA).
[0175] Test time nodes: D0 (before use), D28 (after use).
[0176] Test site: left or right cheek (Tewameter TM300), left or right corner of the eye (PRIMOS CR).
[0177] Test procedure:
[0178] ① D0: recruit volunteers according to the requirements, and the subjects visit the laboratory. After the subjects are selected according to the facial cleaning standard, they sit in the constant temperature and humidity room for 30 min. The laboratory staff screen the subjects according to the test requirements, and the qualified subjects sign the written informed consent form.
[0179] Qualified subjects enter the test, and the test order is as follows: Tewameter TM300 (left or right cheek) → Primos CR (left or right corner of the eye). Record the data as D0.
[0180] After the subjects complete the test, the staff distribute the test products and provide guidance on the use method and amount of the products.
[0181] ② D28: The subjects return to visit after using the products at home for 28 days. After the subjects clean their faces with water, they enter the constant temperature and humidity room and sit for 30 min.
[0182] Check the subjects' usage records, weigh the usage amount of the products, and recover the samples.
[0183] Test the data after use, and the test order is as follows: Tewameter TM300 (left or right cheek) → Primos CR (left or right corner of the eye). Record the data as D28. Calculate the improvement rate according to the data before and after use, and the formula is as follows:
[0184] Improvement rate (%) = (D28-D0) / D0*100%
[0185] In the formula:
[0186] D0--The skin parameter base value before the test area uses the sample, unit: g / m 2 h;
[0187] D28 - Skin parameter value after 28 days of test area sample use, unit: g / m 2 h;
[0188] The improvement rate of skin trans-epidermal water loss and the improvement rate of skin fish tail number are calculated by the same formula, except that the unit of D0 and D28 in the improvement rate of skin trans-epidermal water loss is g / m. 2 h; the unit of D0 and D28 in the improvement rate of skin fish tail number is strip.
[0189] The detection results of TEWL and fish tail number are shown in Table 9-1 and Table 9-2 as follows,
[0190] Table 9-1
[0191]
[0192]
[0193] Table 9-2
[0194]
[0195] As shown in the results of Table 9-1 and Table 9-2, the tea fermentation energy composition has a significant effect of improving the rate of skin trans-epidermal water loss and reducing the number of fish tail, that is, it has good repair and anti-wrinkle efficacy.
[0196] Among them, the tea fermentation energy composition of Example 12 has the best effect, that is, the best ratio of the tea fermentation energy composition is 10 parts of black tea fermentation liquor, 2 parts of Artemia extract, and 0.5 parts of hydrolyzed sodium hyaluronate. After replacing the hydrolyzed sodium hyaluronate with acetylated sodium hyaluronate in Comparative Example 5, the improvement rate of skin trans-epidermal water loss is only -9.22%, and the improvement rate of skin fish tail number is only -13.41%, which is lower than that of Example 12; after replacing the Artemia extract with Chlorella extract in Comparative Example 6, the improvement rate of skin trans-epidermal water loss is only -9.42%, and the improvement rate of skin fish tail number is only -13.13%, which is lower than that of Example 12.
[0197] Finally, it should be noted that the above examples are only used to illustrate the technical solutions of the present application and do not limit the protection scope of the present application. Although the present application has been described in detail with reference to the preferred embodiments, those skilled in the art should understand that the technical solutions of the present application can be modified or replaced by equivalents without departing from the essence and scope of the technical solutions of the present application.
Claims
1. A tea fermentation energy composition with anti-wrinkle and repairing properties, characterized in that: The invention is composed of the following ingredients in parts by weight: 2-10 parts of black tea fermentation liquid, 0.1-3 parts of artemia extract and 0.05-1 part of hydrolyzed sodium hyaluronate.
2. The tea fermentation energy composition according to claim 1, characterized in that The black tea fermentation liquid comprises golden flower black tea fermentation liquid, yeast and Acetobacter xylinum black tea fermentation liquid or Eurotium cristatum K8824 and yeast black tea fermentation liquid.
3. Use of the tea fermentation energy composition according to claim 1 or 2 in the preparation of cosmetics.
4. A cosmetic, characterized in that: The invention comprises the tea fermentation energy composition according to claim 1 or 2 and auxiliary materials.
5. The cosmetic according to claim 4, wherein The cosmetics include facial cleansing products, lotions, creams or facial masks.
6. An emulsion, characterized in that Calculated by weight percentage, the tea fermentation energy composition comprises 2.15% to 14% of the tea fermentation energy composition according to claim 1 or 2, 23.02% to 30.45% of auxiliary materials and the balance water.
7. The emulsion according to claim 6, wherein The excipients include one or more of a skin conditioner, a moisturizer, an emulsifier, a chelating agent, a preservative or a thickener.
8. The emulsion according to claim 7, wherein The skin conditioning agent includes one or more of caprylic / capric triglyceride, hydrogenated polyisobutene, cyclopentasiloxane, dimethicone, or cetearyl alcohol; and / or, the chelating agent is disodium EDTA; and / or, the humectant comprises one or more of glycerin, butylene glycol, 1,2-hexanediol or dipropylene glycol; and / or, the preservative comprises one or both of phenoxyethanol and ethylhexylglycerin; and / or, the emulsifier comprises one or both of PEG-100 stearate or glyceryl stearate; And / or, the thickener includes one or both of xanthan gum and carbomer.
9. The emulsion according to claim 7 or 8, wherein Calculated by weight percentage, the emulsion comprises 2.15% to 14% of the tea ferment energy composition according to claim 1 or 2, 9% to 10% of a moisturizer, 0.3% to 0.45% of a thickener, 0.02% to 0.1% of a chelating agent, 1% to 3% of an emulsifier, 12% to 16% of a skin conditioner, 0.7% to 0.9% of a preservative, and the remainder being water.
10. The method for preparing the emulsion according to any one of claims 7 to 9, characterized in that: The following steps are involved: S1. Mix a skin conditioner and an emulsifier, heat to 75°C to 80°C, and dissolve until completely transparent to obtain an oil phase mixture; S2. After heating the water to 75°C to 80°C, add the moisturizer, chelating agent, and thickener, and mix until there are no particles to obtain an aqueous phase mixture; S3, mixing the oil phase mixture and the water phase mixture, homogenizing, cooling to 42-48° C., and adjusting the pH value to 5.8-6.2 to obtain a water-oil mixed auxiliary material; S4. Mix the water-oil mixed auxiliary material with hydrolyzed sodium hyaluronate, cool to 35° C. to 40° C. after dissolving evenly, add preservatives, and mix evenly; then add black tea fermentation liquid and Artemia extract, mix evenly; cool to 30° C. to 35° C., filter, and obtain the emulsion.
Citation Information
Patent Citations
Method for improving anti-aging effect of eurotium cristatum tea compound fermentation liquor
CN119818402A