Polypeptide-coated anti-wrinkle composition containing camellia japonica extract and application of polypeptide-coated anti-wrinkle composition
Through low-energy emulsification technology, the problem of insufficient solubility and compatibility of polypeptides in existing skin care products is solved, and efficient anti-wrinkle effect and stability are achieved Sex, suitable for a variety of cosmetic types.
Patent Information
- Application Number
- CN202411635806.8
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-11-15
- Publication Date
- 2025-01-07
- Estimated Expiration
- 2044-11-15
AI Technical Summary
The solubility and compatibility issues of palmitoyl polypeptide in existing skin care products lead to insufficient permeability and stability on the skin, affecting the anti-wrinkle effect, and the high-pressure homogenization process is complex and energy-consuming and not suitable for transparent product development.
Low-energy emulsification technology is used to wrap palmitoyl tripeptide-5 and palmitoyl tetrapeptide-7 with red camellia extract. By carefully screening solvents and polyols, a polypeptide-wrinkle composition with nanoparticle size is formed to enhance its dissolution. Sexual and skin permeability.
It significantly improves the solubility and stability of palmitoyl polypeptide, obtains a flowing liquid with a transparent appearance, enhances anti-wrinkle effect, promotes collagen production, and inhibits elastase activity. It is suitable for a variety of cosmetics types.
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Figure CN119257989A_ABST
Abstract
Description
Technical Field
[0001] The invention relates to the technical field of skin care products, and in particular to a polypeptide-wrapped anti-wrinkle composition containing red camellia extract and application thereof. Background Art
[0002] Skin aging is a physiological or pathological phenomenon of degenerative changes in skin morphology and function caused by the combined action of multiple factors. It is generally affected by both internal and external factors. External factors are mainly environmental factors, such as ultraviolet rays, blue light and other damage to the skin, which leads to the production of matrix metalloproteinases and the degradation of various skin proteins. Internal factors mainly refer to the degradation of the skin's extracellular matrix ECM with age, especially the continuous loss of collagen in the dermis, which leads to wrinkles, loss of elasticity, and sagging skin. There are many types of collagen, among which type I collagen is the most common structural protein, accounting for about 80-85%. Adequate collagen can keep the skin plump and elastic.
[0003] Bioactive peptides, also known as functional peptides, are recognized as highly effective and safe active ingredients for preventing and resisting skin aging. They are widely used in the field of beauty and skin care, such as skin anti-aging. Peptides are a class of compounds with a molecular structure between amino acids and proteins. They are formed by two or more amino acids connected by dehydration condensation to form peptide bonds. Each active peptide has a unique structure and function, and its mechanism of action and target on the skin are relatively clear, and the added amount has a significant effect at the ppm level. At present, the peptides involved in the cosmetics industry are mainly small molecule active peptides, which have anti-wrinkle, firming, soothing and other effects, such as tripeptides, tetrapeptides, pentapeptides, hexapeptides, etc. With the continuous increase in consumer demand, peptides have great potential in the field of beauty and skin care.
[0004] Palmitoyl-modified small molecule peptides are a type of peptide that is currently sold in large quantities on the market. They usually exist in the form of hydrochlorides or acetates and are crystalline solids. However, this type of peptide has difficulties in product development and application, mainly because of its poor solubility. It is difficult to dissolve in water and oil. It has a certain alcohol solubility, but it also has a certain selectivity for the type of polyol. For example, the solubility of palmitoyl tripeptide-5 in dimethyl sulfoxide is 30 mg / mL, and the solubility in ethanol is 30 mg / mL, but dimethyl sulfoxide and ethanol are not suitable for conventional cosmetic development and are prone to cause skin allergies. Palmitoyl peptides are prone to precipitation problems when they are not fully dissolved, which reduces the efficacy of the peptide and affects the stability of the product, which also limits its application in actual formula development.
[0005] CN 116370331 A discloses a polypeptide anti-wrinkle composition and its application, comprising carnosine, acetyl hexapeptide-8, palmitoyl pentapeptide-4 and dipalmitoyl hydroxyproline, which has the effects of anti-oxidation, scavenging free radicals, promoting collagen synthesis, etc., and can be used in cosmetics of various dosage forms. However, it has the following problems: the invention does not consider the solubility of different peptides, their compatibility with each other and the permeability of peptides on the skin.
[0006] CN 117379335 A discloses a polypeptide liposome composition and its application, including acetyl heptapeptide-4, palmitoyl tripeptide-8, oligopeptide-1, phospholipids, PPG-13-decyltetradecanol polyether-24 and glycerol, and the polypeptide is encapsulated by the phospholipid component through a high-pressure homogenization process, and the product has high stability and is easy to be absorbed through the skin. However, the efficacy of the peptide involved in the patent focuses on repair and soothing. Secondly, the preparation process used for encapsulating liposomes in the patent must use high pressure and multiple homogenization methods, which is complicated, time-consuming and energy-consuming, and the liposomes finally obtained are in the form of emulsions, non-transparent liquids, and are not suitable for use in the development of transparent products.
[0007] CN201910957516.8 discloses an anti-aging matrix, which is made of the following components in weight percentage: 1,2-pentanediol 3-5%, acetyl hexapeptide-8 10-20%, palmitoyl tripeptide-1 5-7%, palmitoyl tetrapeptide-7 5-8%, acetyl tetrapeptide-2 1-5%, palmitoyl tripeptide-5 3-6%, pepper seed extract 0.01-0.1%, butylene glycol 10-20%, propylene glycol 5-10%, inositol 1-5%, Koelreuteria paniculata fruit extract 0.05-0.1%, and the balance is deionized water. However, this patent only considers the anti-aging effect of the ingredients and the dissolution of the peptides. Moreover, the amount of polyol added to dissolve the peptides is very high, the cost is high, the solubility of the peptides is not good enough, and the encapsulation and penetration of the peptides are not taken into account, and the bioavailability of the peptides is not high.
[0008] CN109846787A discloses a composition and its application in the preparation of cosmetics for repairing the physiological and / or biochemical structure of the skin. In the composition provided by the present invention, the components are selected from any two or more combinations of palmitoyl oligopeptides, flaxseed extract, hydrolyzed collagen, yarrow extract, fructose, and inulin. It adopts the compounding of multiple active ingredients to achieve skin repair and barrier function improvement; however, its preparation method mainly involves conventional cosmetic preparation processes such as dissolution and mixing, and does not consider the encapsulation of palmitoyl peptides and the particle size of the composition. Although ethylhexylglycerol and 1,2-hexanediol are used to assist the dissolution of palmitoyl peptides, active ingredients such as palmitoyl peptides are not effectively encapsulated. The molecular size and morphology of the active ingredients that have not been encapsulated are not conducive to the effective penetration and absorption of the skin. This leads to a reduction in the efficacy of the cosmetics. Even if the formula contains efficient repair ingredients, it is difficult to achieve the desired effect if they cannot be fully absorbed and utilized by the skin. It also does not mention the control of the particle size of the composition; the size of the particle size directly affects the texture, stability and skin absorption of the product; too large a particle size will result in a rough texture and difficulty in applying the product; while too small a particle size may increase the difficulty and cost of preparation. Its mixing method relies on simple mechanical stirring, which cannot evenly disperse all active ingredients into the matrix, especially when there are interactions or solubility differences between the active ingredients. Summary of the invention
[0009] In view of this, the purpose of the present invention is to provide a polypeptide-encapsulated anti-wrinkle composition containing red camellia extract and its application. First, the solubility problem of palmitoyl peptide is solved, and secondly, the palmitoyl peptide is encapsulated by low-energy emulsification technology, which solves the compatibility problem between red camellia extract and palmitoyl peptide, and obtains a transparent flowing liquid, which is not only more stable and safer, but also has better efficacy and is easy to use, and can also promote collagen production, inhibit the activity of elastase, and better achieve the effect of improving wrinkles and delaying aging.
[0010] The technical solution provided by the present invention is as follows:
[0011] A polypeptide-encapsulated anti-wrinkle composition containing red camellia extract, comprising component A, component B, and component C;
[0012] Wherein, component A includes palmitoyl tripeptide-5, palmitoyl tetrapeptide-7, polyol A, and caprylic / capric triglyceride;
[0013] Component B includes PPG-13-decyltetradecanol polyether-24 and polyol B;
[0014] Component C includes water and red camellia extract.
[0015] The mass ratio of component A, component B and component C is 1:(1-4):(1-6).
[0016] Preferably, the mass ratio of component A, component B and component C is (13-18):(36-44):(38-50).
[0017] The polyol A comprises ethylhexylglycerol and 1,2-hexanediol. The mass ratio of the ethylhexylglycerol to the 1,2-hexanediol is 1:1-6:1.
[0018] Preferably, the mass ratio of the ethylhexylglycerol to 1,2-hexanediol is 3:1-6:1.
[0019] The polyol B comprises glycerol and butylene glycol. The mass ratio of glycerol to butylene glycol is 1:1-7:1.
[0020] Preferably, the mass ratio of glycerol to butanediol is 2.5:1-7:1.
[0021] As one embodiment of the present invention, the polypeptide-encapsulated anti-wrinkle composition containing red camellia extract comprises the following components in mass fractions:
[0022]
[0023] The polyol A comprises ethylhexylglycerol and 1,2-hexanediol. The mass ratio of the ethylhexylglycerol to the 1,2-hexanediol is 1:1-6:1.
[0024] Preferably, the mass ratio of ethylhexylglycerol to 1,2-hexanediol is 3:1-6:1.
[0025] The polyol B comprises glycerol and butylene glycol. The mass ratio of glycerol to butylene glycol is 1:1-7:1.
[0026] Preferably, the mass ratio of glycerol to butanediol is 2.5:1-5:1.
[0027] As one embodiment of the present invention, the polypeptide-encapsulated anti-wrinkle composition containing red camellia extract comprises the following components in mass fractions:
[0028]
[0029] Preferably, the polypeptide-encapsulated anti-wrinkle composition containing red camellia extract comprises the following components in the following mass fractions:
[0030]
[0031] The present invention also provides a method for preparing the polypeptide-encapsulated anti-wrinkle composition containing Camellia sinensis extract as described above, comprising the following steps:
[0032] S1, palmitoyl tripeptide-5, palmitoyl tetrapeptide-7, ethylhexylglycerin and 1,2-hexanediol are mixed and stirred evenly, caprylic acid / capric acid triglyceride is added, and further stirred evenly to obtain a mixture a;
[0033] S2, PPG-13-decyltetradecyl alcohol polyether-24, glycerin and butylene glycol are stirred to form a mixture b;
[0034] S3, stirring and mixing water and red camellia extract to form a mixture c;
[0035] S4. Add mixture a to mixture b and stir evenly, then add mixture c and stir (10-30 min) to obtain the polypeptide-encapsulated anti-wrinkle composition containing Camellia sinensis extract.
[0036] In step S4, the heating temperature is 50-65°C.
[0037] The time for adding mixture a to mixture b is 10-15 minutes.
[0038] The preparation method of red camellia extract refers to the article "Research on the Anti-Aging Effect of Red Camellia Flower and Leaf Extracts in Cosmetics" published in "China Wild Plant Resources" and the article "Research on the Effect of Camellia Extract" published in "Science and Technology Plaza".
[0039] The key points of the present invention are:
[0040] The two palmitoyl-modified peptides are palmitoyl tripeptide-5 and palmitoyl tetrapeptide-7, both of which are signal peptides. Palmitoyl tripeptide-5 is also known as collagen peptide, which promotes the production of various collagens in the extracellular matrix by promoting TGF-β (transforming growth factor), enhancing cell activity, maintaining skin elasticity, reducing skin wrinkles, and making the skin look younger. Palmitoyl tetrapeptide-7 is a fragment of immunoglobulin G, which can reduce the secretion of IL-6 by keratinocytes after UVB exposure, thereby inhibiting the inflammatory process caused by the degradation of the extracellular matrix, stimulating the synthesis of elastin, fibronectin, glycosaminoglycans, and type I, type III, and type IV collagen, improving skin quality and fighting skin aging.
[0041] Camellia sinensis extract is not only rich in flavonoid polyphenols that can scavenge free radicals and has a good antioxidant effect, but also contains a variety of different small molecule peptides that can provide nutrition to the skin and resist skin aging.
[0042] The combination of small molecule peptides with different action mechanisms and the red camellia extract, an effective ingredient of natural origin, can work synergistically, better meet the needs of consumers, and achieve better anti-wrinkle effects. However, the solubility properties of the ingredients are different, and the components of the red camellia extract are complex, resulting in poor stability of the composition obtained by direct mixing and reduced efficacy. Therefore, the present invention uses low-energy emulsification technology to wrap the palmitoyl polypeptide component to protect it from damage by the external environment, while enhancing its penetration and release effect on the skin. The wrapped palmitoyl polypeptide is rationally proportioned with natural active ingredients such as the red camellia extract to ensure synergistic effects between the ingredients and maximize the efficacy of the overall composition.
[0043] Compared with the prior art, the specific innovations of the present invention are embodied in the following aspects:
[0044] 1. The present invention significantly improves the solubility of palmitoyl-modified small molecule polypeptides (such as palmitoyl tripeptide-5 and palmitoyl tetrapeptide-7) by carefully selecting and rationally matching different solvents, so that a high content of small molecule polypeptides can be added to the composition while maintaining excellent stability and avoiding precipitation.
[0045] 2. Furthermore, the low-energy emulsification technology not only solves the compatibility problem when the red camellia extract and the palmitoyl small molecule polypeptide are directly mixed, but also successfully obtains a nanoparticle size composition. This innovation significantly improves the skin permeability of small molecule active peptides and makes their bioavailability reach a higher level. The encapsulation process of the present invention is green, environmentally friendly, low-energy and simple to operate, which is very conducive to scale-up production and achieves the dual goals of high efficiency and environmental protection. In addition, the composition is in the form of an aqueous solution and does not contain preservatives, but by cleverly matching polyols, it also achieves a good antiseptic effect.
[0046] 3. After rigorous testing and verification, the polypeptide-encapsulated anti-wrinkle composition of the present invention exhibits excellent stability, the encapsulated active peptide content remains stable, the particle size is stable and the particle size range is narrow, and it has successfully passed the anti-corrosion challenge test. More importantly, it can also effectively promote the synthesis of collagen and inhibit the activity of matrix metalloproteinases, thereby further enhancing its anti-wrinkle effect. Therefore, this highly effective ingredient can be widely used in various cosmetic types such as water-based agents, essences, creams and lotions, meeting consumers' eternal pursuit of anti-aging and maintaining a youthful state.
[0047] 4. The present invention cleverly combines small molecule peptide anti-aging ingredients with rich skin active ingredients in the plant Camellia japonica, and forms a more stable and more effective polypeptide anti-wrinkle composition through low-temperature emulsification technology, successfully overcoming the difficulties in formula application.
[0048] 5. The encapsulated active ingredients can more easily penetrate the skin barrier and enter the deep layers of the skin to exert their effects. The surface of the encapsulation has a lipid structure similar to that of the skin, which can better blend and penetrate the skin. At the same time, the encapsulation technology can also control the release rate of the active ingredients to achieve continuous and stable efficacy output. The encapsulation technology precisely controls the particle size of the active ingredients, thereby optimizing the texture, stability and skin absorption effect of the product. BRIEF DESCRIPTION OF THE DRAWINGS
[0049] Other features, objects and advantages of the present invention will become more apparent from the detailed description of non-limiting embodiments made with reference to the following drawings:
[0050] Figure 1 This is a sample diagram of Example 1;
[0051] Figure 2 is the room temperature particle size distribution diagram of Example 1;
[0052] Figure 3 This is a graph showing the particle size test of the polypeptide anti-wrinkle composition of Example 1 (under different stability testing conditions). DETAILED DESCRIPTION
[0053] The present invention is described in detail below in conjunction with embodiments. The following embodiments will help those skilled in the art to further understand the present invention, but are not intended to limit the present invention in any form. It should be noted that, for those of ordinary skill in the art, some adjustments and improvements can also be made without departing from the concept of the present invention. These all belong to the protection scope of the present invention.
[0054] Preparation Example 1
[0055] For the preparation process of red camellia extract, please refer to the article "Research on the Anti-Aging Effect of Red Camellia Flower and Leaf Extracts in Cosmetics" published in "China Wild Plant Resources" and the article "Research on the Efficacy of Camellia Extract" published in "Science and Technology Plaza".
[0056] Examples 1-6
[0057] Examples 1-6 provide a polypeptide anti-wrinkle composition and a preparation method thereof.
[0058] 1. Specific information on components and contents is shown in Table 1.
[0059] Table 1 Unit (mass percentage: %)
[0060]
[0061] The preparation method of Examples 1-3 comprises the following steps:
[0062] 1. Mix and stir palmitoyl tripeptide-5, palmitoyl tetrapeptide-7, ethylhexylglycerin and 1,2-hexanediol until the powder is completely dissolved, then add caprylic / capric triglyceride and stir to mix evenly to obtain mixture a;
[0063] 2. PPG-13-decyltetradecyl alcohol polyether-24, glycerin and butylene glycol were stirred and mixed uniformly to obtain mixture b;
[0064] 3. Stir and mix the water and the red camellia extract to obtain a mixture c;
[0065] 4. In a 65℃ water bath, add mixture a to mixture b at a uniform speed within 15 minutes while stirring, stir evenly, then slowly add mixture c in the same way and stir for 10 minutes;
[0066] 5. Stir the mixture and cool it to room temperature, then filter it to obtain a uniform and transparent composition.
[0067] In step 1: first mix palmitoyl tripeptide-5, palmitoyl tetrapeptide-7 with ethylhexylglycerin and 1,2-hexanediol and stir until the powder is completely dissolved. Ethylhexylglycerin and 1,2-hexanediol act as solubilizers, helping the peptides to better and fully dissolve in the system.
[0068] During the mixing process of step 4: slowly add mixture a to mixture b, and then add mixture c and stir. In this process, the temperature and the slow addition method have an impact on the encapsulation effect. The appropriate temperature helps the components maintain good fluidity so that they can be mixed more evenly. Especially for the surfactant PPG-13-decyltetradecanol polyether-24, if the temperature is too low, it will gel, but if the temperature is too high, it will reduce the active content of the active peptide; slow addition can avoid the situation where the local concentration is too high or the reaction is too fast, causing the encapsulation structure to be destroyed or uneven. PPG-13-decyltetradecanol polyether-24 in mixture b is used as the main surfactant, and glycerol and butylene glycol are used as auxiliary surfactants to help reduce the resistance of the emulsifier during self-assembly at the oil-water interface. Mixture b interacts with the components in mixture a to further improve and stabilize the encapsulation structure to form alcohol-in-oil. Then slowly add mixture c to form water-in-oil, and reinforce or optimize the structure of the encapsulated active peptide that has been initially formed, so that it is more tightly and more stable, thereby achieving the effect of stable particle size and narrow range.
[0069] The preparation method of Example 4-6 comprises the following steps:
[0070] 1. Mix and stir palmitoyl tripeptide-5, palmitoyl tetrapeptide-7, ethylhexylglycerin and 1,2-hexanediol until the powder is completely dissolved, then add caprylic / capric triglyceride and stir to mix evenly to obtain mixture a;
[0071] 2. PPG-13-decyltetradecyl alcohol polyether-24, glycerin and butylene glycol were stirred and mixed uniformly to obtain mixture b;
[0072] 3. Stir and mix the water and the red camellia extract to obtain a mixture c;
[0073] 4. In a 55°C water bath, under stirring, slowly add mixture a to mixture b at a uniform speed within 10 minutes, stir evenly, then slowly add mixture c and stir for 30 minutes;
[0074] 5. Stir the mixture and cool it to room temperature, then filter it to obtain a uniform and transparent composition.
[0075] Through the various components, addition amounts and the above-mentioned preparation process, the compositions obtained in Examples 1-6 are all transparent flowing liquids, and the measured particle sizes are all in the range of 30-200 nm.
[0076] Comparative Example 1
[0077] The preparation process of this comparative example is consistent with that of Example 1, the only difference being that no red camellia extract is added to the components. The obtained composition is a transparent flowing liquid with a particle size (D50) of 40 nm, but the anti-wrinkle effect of the composition is not as good as that of Example 1.
[0078] Comparative Example 2
[0079] The preparation process of this comparative example is consistent with that of Example 1, except that the ratio of component A: component B: component C is 3:0.5:2. This ratio cannot be used to prepare a transparent and uniform composition, which does not meet application requirements.
[0080] Comparative Example 3
[0081] Publication patent 202211695584.X relates to a microemulsion and a preparation method thereof, including an emulsifier, a polyol, an oil phase, and water. The emulsifier is PPG-13-decyltetradecyl alcohol polyether-24; the polyol is glycerol and / or diglycerol, and can also carry active substances. The composition was prepared using the preparation method related to oil-soluble active substances in the patent. Experiments have found that whether caprylic / capric triglyceride or camellia seed oil is used, palmitoyl tripeptide-5 and palmitoyl tetrapeptide-7 cannot be dissolved, and a transparent and uniform composition cannot be obtained.
[0082] Comparative Example 4
[0083] The preparation process of this comparative example is consistent with that of Example 1, with the only difference being that butanediol is not added to the components. The obtained composition is a transparent flowing liquid with a particle size (D50) of 60 nm. However, obvious stratification occurs during stability tests at high temperatures of 40°C and 48°C, and the stability test fails.
[0084] Comparative Example 5
[0085] The preparation process of this comparative example is consistent with that of Example 1, with the only difference being that the mass ratio of glycerol to butanediol is 1:2, and the specific addition amounts are 7% and 14% respectively. The obtained composition is a semi-transparent whitish bluish liquid with a particle size (D50) of 250.28nm. In addition, during the stability test, the composition became foggy at low temperatures of 3°C and -18°C, and oil and fat precipitated, and failed the stability test.
[0086] Comparative Example 6
[0087] The preparation process of this comparative example is consistent with that of Example 1, with the only difference being that the dosage ratio of PPG-13-decyltetradecyl alcohol polyether-24 and caprylic / capric triglyceride is 1:2, and the added amounts are 6% and 12%, respectively, to obtain a semi-transparent emulsion-like composition, and the particle size (D50) of the composition is greater than 1000 nm.
[0088] Comparative Example 7
[0089] The preparation process of this comparative example is consistent with that of Example 1, with the only difference being that ethylhexylglycerol is not added to the components. The obtained composition is a nearly transparent flowing liquid with a particle size (D50) of 50 nm. However, solid particles precipitate after being placed at room temperature for 1 week. The precipitates are confirmed to be palmitoyl tripeptide-5 and palmitoyl tetrapeptide-7 by testing. The reason for the analysis is that the palmitoyl peptide is not fully dissolved.
[0090] Comparative Example 8
[0091] The preparation process of this comparative example is consistent with that of Example 1, with the only difference being that ethylhexylglycerin is replaced with tocopherol acetate in the same proportion in the components. In step 1, a transparent and uniform mixture a cannot be obtained, and white powder is present in the semipermeable liquid, which is determined to be palmitoyl tripeptide-5 and palmitoyl tetrapeptide-7 by analysis, indicating that tocopherol acetate cannot dissolve palmitoyl peptide well.
[0092] Comparative Example 9
[0093] The preparation process of this comparative example is consistent with that of Example 1, with the only difference being that ethylhexylglycerin is replaced with 1,2-pentanediol in the same proportion in the components, and the obtained composition is a semi-transparent blue flowing liquid. When placed at room temperature for 1 week, solid particle precipitates appear at the bottom. After testing, it is confirmed that the precipitates are palmitoyl tripeptide-5 and palmitoyl tetrapeptide-7. The reason for the analysis is that the solubility of 1,2-pentanediol in palmitoyl peptide is not good enough.
[0094] Comparative Example 10
[0095] The preparation process of this comparative example is consistent with that of Example 1, with the only difference being that ethylhexylglycerin is replaced with diisopropyl adipate in the same proportion in the components. In step 1, a transparent and uniform mixture a cannot be obtained, and white floccules are present in the semipermeable liquid, which are determined to be palmitoyl tripeptide-5 and palmitoyl tetrapeptide-7 by analysis, indicating that diisopropyl adipate cannot dissolve palmitoyl peptide well.
[0096] Comparative Example 11
[0097] The components and proportions of the composition of this comparative example are the same as those of Example 1, and the only difference is that the preparation method of the composition is different.
[0098] The specific preparation method of this comparative example is:
[0099] At 65°C, water, glycerin, butylene glycol, camellia japonica extract, palmitoyl tripeptide-5, palmitoyl tetrapeptide-7, ethylhexylglycerin, 1,2-hexanediol, acetyl hexapeptide-8, PPG-13-decyltetradecyl alcohol polyether-24 and caprylic / capric triglyceride were added in sequence under stirring and mixed evenly, but a uniform composition could not be obtained.
[0100] Comparative Example 12
[0101] The components and proportions of the composition of this comparative example are the same as those of Example 1, and the only difference is that the preparation method of the composition is different.
[0102] In step 4 of the preparation process, mixture b and mixture c are added to mixture a at the same time, and stirred and mixed evenly, and finally a semi-transparent blue composition is obtained, and the particle size range of the composition is relatively wide and the uniformity is relatively poor.
[0103] Comparative Example 13
[0104] The composition and proportion of this comparative example are the same as those of Example 1, the only difference being that in step 1,
[0105] Palmitoyl tripeptide-5, palmitoyl tetrapeptide-7, ethylhexylglycerin, 1,2-hexanediol, and caprylic / capric triglyceride are mixed and dispersed at the same time as a mixture a. Using this method, a transparent and uniform mixture a cannot be obtained, which ultimately affects the transparency of the composition and causes the palmitoyl peptide to be unable to fully dissolve.
[0106] Performance Test Example 1 Stability Study of Peptide Anti-wrinkle Composition
[0107] The compositions prepared in Examples 1-6 were subjected to a 2-month stability test. The results of the stability test are shown in Table 2.
[0108] Table 2 Results of stability study of polypeptide anti-wrinkle composition
[0109]
[0110]
[0111] From the results in Table 2, it can be seen that the compositions under different conditions all maintain a uniform and transparent liquid state, without precipitation, liquid fogging or unstable stratification, indicating that the stability test has passed.
[0112] Performance Test 2 Particle Size Test of Peptide Anti-Wrinkle Composition
[0113] The particle size test of the composition was performed using a Bettersize 3000 particle size analyzer. The particle size test results of Examples 1-6 are shown in Table 3. Taking Example 1 as a representative example, the original particle size test results and the particle size test results after 2 months of stability inspection are shown in Figure 3. Figure 2 and Figure 3 shown.
[0114] Table 3 Particle size test results of Examples 1-6
[0115]
[0116] The results show that the particle size of the polypeptide-encapsulated anti-wrinkle composition containing Camellia sinensis extract obtained by the present invention is within 200nm, and more within 100nm. After 2 months of stability inspection, the particle size of the polypeptide anti-wrinkle composition is still maintained within 200nm, and more within 100nm, and the particle size changes under different conditions are small, indicating that the composition is very stable.
[0117] Performance Test 3 Determination of polypeptide content in polypeptide anti-wrinkle composition
[0118] Taking Example 1 as a representative example, the content of some small molecule peptides in Example 1 was determined after the stability study was completed.
[0119] Specifically as follows: using a high performance liquid chromatograph (ultraviolet detector), the reagents are acetonitrile (chromatographic grade), phosphoric acid (analytical grade), triethylamine (analytical grade), potassium dihydrogen phosphate, palmitoyl tripeptide-5, and palmitoyl tetrapeptide-7. Accurately aspirate the blank solution, standard solution, and test solution and inject them into the liquid chromatograph to record the chromatogram. The content of palmitoyl tripeptide-5 and palmitoyl tetrapeptide-7 is calculated by the external standard method, and the purity of the test sample is calculated by the area normalization method. The results are shown in Table 4. It can be seen from the results that after the stability test, the content of palmitoyl tripeptide-5 and palmitoyl tetrapeptide-7 encapsulated in the polypeptide anti-wrinkle composition under each condition remains stable.
[0120] Table 4 Determination of the content of palmitoyl tripeptide-5 and palmitoyl tetrapeptide-7 in the polypeptide anti-wrinkle composition
[0121] Test conditions (2 months) Palmitoyl Tripeptide-5 (ppm) Palmitoyl Tetrapeptide-7 (ppm) Room temperature 200.20 200.89 40℃ 198.74 198.16 3℃ 197.69 200.77 -10℃ 199.51 198.79
[0122] Performance Test 4 Transdermal Absorption Test of Peptide Anti-wrinkle Composition
[0123] Transdermal absorption in cosmetics refers to the process in which the functional ingredients in cosmetics act on the skin surface or enter the epidermis or dermis according to the effectiveness of the product, and accumulate and play a role in this part. At present, the most commonly used in vitro method for detecting transdermal absorption of cosmetic ingredients is the diffusion cell method. The ex vivo skin of humans or animals is installed on the diffusion cell, the receiving liquid is taken at regular intervals, the content of the active ingredient is determined by a suitable analytical method, and the transdermal rate is calculated to evaluate the penetration characteristics of the chemical substance.
[0124] This performance test example uses a transdermal absorption diffusion cell, selects Bama Xiang pig abdominal pig skin as ex vivo skin, uses HPLC to detect the target active ingredient, and finally obtains the release and cumulative amount of the active ingredient at different times. Taking Example 1 and Comparative Example 9 as representative examples, the sample amount is 0.5 ml of the stock solution, and the sampling point is 8 hours. The transdermal absorption results are shown in Table 5.
[0125] Table 5 Transdermal absorption test results of palmitoyl tripeptide-5 in polypeptide anti-wrinkle composition
[0126]
[0127] It can be seen from the results that when the sampling test was performed at 8h, the release amount of palmitoyl tripeptide-5 in Example 1 exceeded that of Comparative Example 9, and the retention amount in the skin far exceeded that of Comparative Example 9, indicating that the polypeptide anti-wrinkle composition prepared by the present invention can help the active ingredients to be slowly released, and the ability of transdermal absorption is greatly improved.
[0128] Performance Test 5
[0129] Antiseptic challenge test of polypeptide anti-wrinkle composition:
[0130] The samples of Example 1 were tested according to the general principles of microbial testing methods, total colony count, mold and yeast testing methods in Chapter 5 of the "Technical Specifications for Safety of Cosmetics" (2015 Edition), and the test results should comply with the limit values in the "Technical Specifications for Safety of Cosmetics" (2015 Edition). The antiseptic challenge test adopts a single bacterial strain infection test method, that is, the test sample is artificially contaminated with a bacterial suspension of each test strain, and the amount of surviving bacteria therein is detected at regular intervals, and the challenge of the cosmetic preservative system is judged based on the change in the amount of surviving bacteria. The test method and judgment criteria of this antiseptic challenge experiment were formulated with reference to the United States Pharmacopoeia USP51, the European Pharmacopoeia EP7.0 and the CTFA method. A single inoculation method was adopted, inoculated on the 0th day, and the results were tested on 7 days, 14 days, 21 days and 28 days after inoculation. The experimental results confirmed that the sample passed the antiseptic challenge and had good antiseptic effect. The test results are shown in Tables 6 and 7.
[0131] Table 6 Sterility test results
[0132]
[0133] Table 7 Anticorrosion Challenge Test Results
[0134] Vaccination Type 7d 14d 21d 28d bacteria <10 <10 <10 <10 Fungi 330 60 <10 <10 .
[0135] Performance Test 6
[0136] The reasonable combination of palmitoyl peptide and red camellia extract can better promote collagen synthesis and thus achieve better anti-wrinkle effects.
[0137] The specific test results are shown in Table 8.
[0138] In vitro efficacy test of peptide anti-wrinkle composition: test on promoting type I collagen
[0139] The polypeptide-encapsulated anti-wrinkle compositions prepared in the above Examples 1-6 and Comparative Example 1 were tested for promoting type I collagen. The test method refers to the group standard T / SHRH 031-2020 "Cosmetic Firming and Anti-wrinkle Efficacy Test-In Vitro Fibroblast Type I Collagen Content Determination" issued by the Shanghai Daily Cosmetics Industry Association. HSF cells in the logarithmic growth phase were inoculated in a 3-cm diameter cell culture dish or a 6-well cell culture plate. After the cells were fused to 80%, samples of different concentrations were added to the sample group for culture. After replacing the fresh culture medium, the culture was continued for 24 hours, and the cell supernatant was collected. The content of type I collagen was detected using an ELISA kit. The higher the content, the stronger the anti-wrinkle ability.
[0140] Relative content of type I collagen = T / C × 100%
[0141] Where:
[0142] T—average value of type I collagen content of the test substance;
[0143] C—Average value of type I collagen content in blank / solvent control
[0144] Table 8 Promotes the relative content of type I collagen
[0145] serial number concentration Relative value of type I collagen Normal control / 100.00% Positive Control 50ng / mL 126.33% Example 1 0.01% 119.35% Example 2 0.01% 117.28% Example 3 0.01% 116.97% Example 4 0.01% 124.59% Example 5 0.01% 130.86% Example 6 0.01% 123.22% Comparative Example 1 0.01% 110.77%
[0146] The above describes the specific embodiments of the present invention. It should be understood that the present invention is not limited to the above specific embodiments, and those skilled in the art may make various modifications or variations within the scope of the claims, which do not affect the essence of the present invention.
Claims
1. A polypeptide-encapsulated anti-wrinkle composition containing red camellia extract, characterized in that: It includes component A, component B and component C; Wherein, component A includes palmitoyl tripeptide-5, palmitoyl tetrapeptide-7, polyol A, and caprylic / capric triglyceride; Component B includes PPG-13-decyltetradecanol polyether-24 and polyol B; Component C includes water and red camellia extract.
2. The polypeptide-encapsulated anti-wrinkle composition containing Camellia sinensis extract according to claim 1, characterized in that: The polyol A includes ethylhexylglycerin and 1,2-hexanediol.
3. The polypeptide-encapsulated anti-wrinkle composition containing Camellia sinensis extract according to claim 2, characterized in that: The mass ratio of the ethylhexylglycerol to 1,2-hexanediol is 1:1-6:
1.
4. The polypeptide-encapsulated anti-wrinkle composition containing Camellia sinensis extract according to claim 1, characterized in that: The polyol B includes glycerol and butylene glycol.
5. The polypeptide-encapsulated anti-wrinkle composition containing Camellia sinensis extract according to claim 4, characterized in that: The mass ratio of the glycerol to butanediol is 1:1-7:
1.
6. The polypeptide-encapsulated anti-wrinkle composition containing Camellia sinensis extract according to claim 1, characterized in that: The mass ratio of component A, component B and component C is 1:1-4:1-6.
7. The polypeptide-encapsulated anti-wrinkle composition containing Camellia sinensis extract according to claim 1, characterized in that: The polypeptide-encapsulated anti-wrinkle composition containing red camellia extract comprises the following components in the following mass fractions:
8. A method for preparing a polypeptide-encapsulated anti-wrinkle composition containing Camellia sinensis extract according to any one of claims 1 to 7, characterized in that: The steps include: S1, palmitoyl tripeptide-5, palmitoyl tetrapeptide-7, ethylhexylglycerin and 1,2-hexanediol are mixed and stirred evenly, caprylic acid / capric acid triglyceride is added, and further stirred evenly to obtain a mixture a; S2, PPG-13-decyltetradecyl alcohol polyether-24, glycerin and butylene glycol are stirred to form a mixture b; S3, stirring and mixing the water and the red camellia extract to form a mixture c; S4. Add mixture a to mixture b under heating and stirring, stir evenly, then add mixture c and continue stirring to obtain the polypeptide-wrapped anti-wrinkle composition containing Camellia sinensis extract.
9. The method for preparing the polypeptide-encapsulated anti-wrinkle composition containing Camellia sinensis extract according to claim 8, characterized in that: In step S4, the heating temperature is 50-65°C.
10. An anti-wrinkle composition containing a polypeptide coated with a Camellia sinensis extract as claimed in any one of claims 1 to 7; or an anti-wrinkle composition containing a polypeptide coated with a Camellia sinensis extract prepared by the preparation method according to claim 8 or 9 in cosmetics.
Citation Information
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