Composition containing tectorigenin and application of composition in whitening and anti-aging cosmetics
By constructing a physical UV barrier and a thermosensitive micelle structure, the problem of poor photostability of irisin in cosmetics was solved, achieving the stability and continuous release of active ingredients and improving the efficacy of whitening and anti-aging products.
Patent Information
- Application Number
- CN202511786152.3
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-12-01
- Publication Date
- 2026-01-30
AI Technical Summary
Iris aglycone has poor photostability in cosmetics and is easily degraded and inactivated, leading to a decrease in the content of active ingredients and product quality problems.
A physical UV barrier is constructed by combining a complex of irisinogen and poloxamer 407 with modified hyaluronic acid and hydroxyapatite microspheres. The active ingredients are locked at low temperatures and released at skin temperature by utilizing the thermosensitive micelle structure of poloxamer 407.
It significantly improves the photostability of irisin, ensuring the product maintains high activity throughout its shelf life, avoiding burst release stimulation, prolonging the continuous release time of active ingredients, and enhancing the whitening and anti-aging effects.
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Abstract
Description
TECHNICAL FIELD
[0001] The application belongs to the technical field of cosmetics, and relates to a composition containing iridin and application thereof in whitening and anti-aging cosmetics. BACKGROUND
[0002] With the increasing demand of consumers for natural and efficient skin care ingredients, plant-derived active substances are increasingly widely used in the field of cosmetics. Iridin, as a highly potential isoflavone compound, has attracted high attention in the industry. Iridin is mainly extracted from the dried rhizomes of Iris L. plants, and its chemical name is 5,7,4'-trihydroxy-6-methoxy isoflavone. The molecule structure of iridin is rich in active groups such as phenolic hydroxyl groups, which endows iridin with excellent whitening, anti-aging and antioxidant effects. In terms of whitening, iridin can effectively improve skin problems such as color spots and dullness by competitively inhibiting the activity of tyrosinase and reducing the biosynthesis of melanin. In the field of anti-aging, iridin can specifically activate retinoic acid receptor RAR-gamma in the skin, promote the synthesis of collagen and elastin, and inhibit the degradation of collagen by matrix metalloproteinase, thereby delaying the production of wrinkles and skin relaxation.
[0003] However, the phenolic hydroxyl groups and methoxyl groups in the molecule structure of iridin have high chemical activity. Under the conditions of ultraviolet irradiation or long-term exposure to natural light, photooxidation, isomerization and degradation reactions easily occur, which leads to the destruction of the molecular structure of iridin and the loss of its original biological activity. This photo-instability not only causes the content of active ingredients in cosmetics containing iridin to decrease during production, storage and transportation, but also may cause quality problems such as color change and abnormal odor of the product due to the generation of degradation products. SUMMARY
[0004] The purpose of the present application is to provide a composition containing iridin and application thereof in whitening and anti-aging cosmetics, which can effectively solve the problems of poor photo-stability and easy degradation of iridin in cosmetics.
[0005] The purpose of the present application can be achieved by the following technical solutions.
[0006] In a first aspect, the present application provides a composition containing iridin, which comprises the following raw materials by weight: 1-2 parts of composite iridin, 2-3 parts of hydroxyapatite microspheres, 0.8-1.2 parts of modified hyaluronic acid, and 70-80 parts of deionized water.
[0007] The composite iridin is a complex formed by iridin and poloxamer 407.
[0008] The modified hyaluronic acid is cholesteryl-modified hyaluronic acid.
[0009] Preferably, the mass ratio of the iridin to poloxamer 407 in the composite iridin is 1:1-1.5.
[0010] Preferably, the particle size of the hydroxyapatite microspheres is 180-220 nm.
[0011] Preferably, 2-5 parts of D-limonene microemulsion having a particle size of 50-100 nm are further included.
[0012] Preferably, 3-6 parts of glycerol, 2-5 parts of 1,3-propanediol, 0.1-0.4 parts of carbomer 940, 0.15-0.25 parts of triethanolamine, 0.6-1.2 parts of preservative, 0.15-0.25 parts of disodium EDTA, and 0.1-0.6 parts of sodium citrate are further included.
[0013] Preferably, the preservative is a mixture of phenoxyethanol and ethylhexylglycerin, and the mass ratio of the phenoxyethanol to ethylhexylglycerin is 9:1.
[0014] Preferably, the preparation of the composition comprises the following steps:
[0015] S1, adding carbomer 940 to deionized water, standing and swelling, then adding glycerol, 1,3-propanediol, disodium EDTA and sodium citrate in sequence, stirring until uniform, adjusting pH, and obtaining an aqueous phase matrix;
[0016] S2, mixing the composite iridin with deionized water, stirring uniformly at 40±1℃, then adding 1,3-propanediol, and stirring while heating to 60±1℃, and obtaining a composite iridin dispersion;
[0017] S3, dispersing the hydroxyapatite microspheres in deionized water, ultrasonic treatment, then adding modified hyaluronic acid, and stirring uniformly at 30±0.5℃, and obtaining a nanosphere-hyaluronic acid composite;
[0018] S4, stirring the D-limonene microemulsion and the aqueous phase matrix uniformly, then adding the composite iridin dispersion and stirring uniformly, and then adding the nanosphere-hyaluronic acid composite and stirring uniformly, and obtaining a composite system;
[0019] S5, subjecting the composite system to microfluidic homogenization treatment, then adding triethanolamine and stirring uniformly, adjusting pH, then refrigerating to form a gel, then adding a preservative and stirring uniformly, and finally filtering and sterilizing to obtain the iridin-containing composition.
[0020] Preferably, in step S4, the following temperature control procedure is followed: first, heat the aqueous phase matrix to 35±0.5℃ at a heating rate of 1±0.2℃ / min, add the D-limonene microemulsion and stir until uniform; then add the complex iridoid dispersion and stir until uniform; then cool to 25±0.5℃ at a cooling rate of 1±0.2℃ / min, and finally add the nanosphere-hyaluronic acid complex, stir until uniform at 25±0.5℃, to obtain the complex system.
[0021] Preferably, in step S5, the microfluidization pressure is 8000±200 psi, the number of cycles of homogenization is 3-5, and the refrigeration temperature is 4±0.5℃, and the refrigeration time is 12-14 hours.
[0022] In a second aspect, the present application provides a whitening and anti-aging cosmetic product comprising the iridoid-containing composition described above, the cosmetic product being in the form of a gel, emulsion, serum, or cream.
[0023] The beneficial effects of the present application are:
[0024] (1) Through the specific adsorption of the cholesterol groups of the modified hyaluronic acid to the surface of the hydroxyapatite microspheres, and the multiple hydrogen bond network formed by the carboxyl and hydroxyl groups on the molecular chain of the modified hyaluronic acid and the PEO segments in the poloxamer 407 molecules, the hydroxyapatite microspheres can form a dense monolayer aggregation structure on the surface of the complex iridoid, thereby constructing a physical ultraviolet barrier. During product production, filling, storage, and transportation, this structure can effectively block the direct irradiation of ultraviolet light on the internal iridoid, significantly reducing the occurrence of photooxidation, isomerization, and degradation reactions, effectively solving the long-standing problem of light instability of iridoid in cosmetic applications, and ensuring the high activity and stability of the product throughout the shelf life.
[0025] (2) The complex formed by poloxamer 407 and iridoid in a mass ratio of 1:1-1.5 serves as the core, and the three-dimensional spatial network structure constructed by the modified hyaluronic acid, under low temperature conditions (below 25℃), the PPO segments and PEO segments of the poloxamer 407 molecules form a tightly ordered micellar arrangement, and the hydrophilic region of the modified hyaluronic acid is crosslinked by hydrogen bonds, together locking the position of the hydroxyapatite microspheres on the surface of the complex, forming a highly stable protection system; when the product comes into contact with the skin (32-37℃), the poloxamer 407 undergoes a temperature-sensitive phase transition, the PPO segments shrink due to dehydration, and the PEO segments change in conformation, causing the entire network structure to gradually loosen, and the hydroxyapatite microspheres to sequentially detach from the surface, and the internal iridoid to be gradually released. This temperature-triggered intelligent release mechanism allows the active ingredients to rapidly take effect in the initial stage of application, while also being able to be continuously and stably released subsequently, avoiding the irritation caused by burst release and prolonging the effective action time, greatly improving the product use experience and efficacy sustainability.
[0026] (3) D-limonene microemulsion is dispersed in the system by the hydrophobic region of poloxamer 407, and interacts with the hydrophobic region of poloxamer 407, synergistically promotes the penetration of the stratum corneum when the product is applied to the skin, and significantly enhances the whitening and anti-aging effects. DETAILED DESCRIPTION
[0027] In order to further illustrate the technical means and effects adopted by the present application to achieve the predetermined purpose of the application, the specific embodiments, structures, features and effects according to the present application are described in detail as follows in combination with examples.
[0028] Some of the raw materials involved in the following examples and comparative examples are described as follows:
[0029] The preparation of modified hyaluronic acid specifically includes the following steps: 5 parts of sodium hyaluronate with a molecular weight of 200 kDa are dissolved in 50 parts of deionized water, and stirred at 4℃ for 30 minutes until completely dissolved; 1.2 parts of cholesteryl succinic acid monoester are dissolved in 50 parts of anhydrous DMF, 1.15 parts of EDC and 0.65 parts of NHS are added, and stirring is carried out at room temperature for 2 hours under nitrogen protection to complete the activation; the activated solution is added to the hyaluronic acid solution at a speed of 1 mL / min, the pH is adjusted to 5.2, and the reaction is carried out at 4℃ and 800 rpm for 24 hours; the reaction solution is dialyzed through a dialysis bag with a molecular weight cutoff of 12 kDa for 72 hours, the dialysis water is replaced every 6 hours during the period, 2 times the volume of anhydrous acetone is added for precipitation, centrifuged at 10,000 rpm for 15 minutes to collect the precipitate, washed with acetone for 3 times, and then freeze-dried to obtain the modified hyaluronic acid.
[0030] In addition to the raw materials specifically mentioned above, the remaining raw materials not specifically described are conventional industrial-grade products, which can be conveniently obtained through market channels.
[0031] Example 1
[0032] A composition containing iridin includes the following raw materials by weight: 1.5 parts of composite iridin, 2.5 parts of hydroxyapatite microspheres, 1 part of modified hyaluronic acid, 75 parts of deionized water, 3.5 parts of D-limonene microemulsion, 4.5 parts of glycerol, 3.5 parts of 1,3-propanediol, 0.25 parts of carbomer 940, 0.2 parts of triethanolamine, 0.9 parts of preservative, 0.2 parts of disodium EDTA and 0.35 parts of sodium citrate.
[0033] The preservative is a mixture of phenoxyethanol and ethylhexylglycerin, the mass ratio of phenoxyethanol to ethylhexylglycerin is 9:1, and the particle size of the hydroxyapatite microspheres is 200 nm.
[0034] The preparation of the composite iridin, specifically comprising the following steps: 1 part of iridin and 1.2 parts of poloxamer 407 are dissolved in 5 parts of anhydrous ethanol at 60°C, 200W ultrasonic treatment for 30 minutes, then 1.0 mL / min speed is added to the pre-cooled deionized water in an ice bath at 4°C, when the system turbidity reaches 25 NTU, stop adding water, continue stirring for 10 minutes to form a uniform suspension, finally the suspension is pre-frozen at-80°C for 2 hours, transferred to the freeze dryer for 24 hours freeze-drying treatment at-50°C, 8Pa, the freeze-drying process is divided into three stages: first at-30°C for 8 hours to perform preliminary sublimation, then warmed to-10°C for 6 hours to complete the main sublimation, finally at 25°C for 10 hours to perform desorption drying, crushed through 120 mesh sieve, to obtain the composite iridin.
[0035] The preparation of the D-limonene microemulsion, specifically comprising the following steps: 1.0 parts of 1,3-propanediol is mixed with 0.5 parts of D-limonene, stirred at 300 rpm for 5 minutes, 2.0 parts of deionized water is added at a speed of 1L / min, stirred at 500 rpm for 10 minutes to form a coarse emulsion; the coarse emulsion is sheared at 10000 rpm for 3 minutes, then ultrasonically treated at 150W, 20kHz for 2 minutes to obtain the D-limonene microemulsion, the particle size of the D-limonene microemulsion is 75nm, the temperature is 4°C, and the D-limonene microemulsion is ready for use.
[0036] A method for preparing a composition containing iridin, specifically comprising the following steps:
[0037] S1, water phase matrix preparation: 55 parts of deionized water is added to the reaction kettle, 0.25 parts of carbomer 940 is slowly added at a rate of 0.4 parts / min under stirring at 300 rpm, and is left to swell for 2 hours; then the stirring speed is increased to 600 rpm, 4.5 parts of glycerol, 2 parts of 1,3-propanediol, 0.2 parts of disodium EDTA, and 0.35 parts of sodium citrate are added in sequence, and are stirred for 30 minutes until the system is uniform; the pH is adjusted to 6.0 to obtain the water phase matrix, which is ready for use at 25°C.
[0038] S2, preparation of composite iridin dispersion: 10 parts of deionized water is added to the reaction tank, heated to 40°C, 1.5 parts of composite iridin is added, and is stirred at 800 rpm for 20 minutes until completely dispersed; 1.5 parts of 1,3-propanediol is added, heated to 60°C, and continues to be stirred for 10 minutes, and is ready for use at 60°C, to obtain the composite iridin dispersion.
[0039] S3, preparation of nanosphere-hyaluronic acid complex: 2.5 parts of hydroxyapatite microspheres is dispersed in 10 parts of deionized water, transferred to a 30°C constant temperature water bath reaction tank, and is ultrasonically treated at 100W, 20kHz for 10 minutes; then 1 part of modified hyaluronic acid is added, and is stirred at 1000 rpm for 30 minutes, and is ready for use at 25°C, to obtain the nanosphere-hyaluronic acid complex.
[0040] S4. Construction of the composite system: The aqueous matrix was transferred to an emulsification tank and heated to 35°C at 1°C / min. 3.5 parts of D-limonene microemulsion were added and stirred at 600 rpm for 5 minutes. The composite irisin dispersion was slowly added and stirred at 800 rpm for 12 minutes. Then the temperature was lowered to 25°C at 1°C / min, and the nanosphere-hyaluronic acid complex was added and stirred at 1500 rpm for 20 minutes to obtain the composite system.
[0041] S5. Homogenization and post-treatment: The composite system was kept at 25°C and homogenized three times under 8000psi pressure. Then, 0.2 parts of triethanolamine were added, and the mixture was stirred at 500rpm for 10 minutes to adjust the pH to 6.3. The mixture was then transferred to a stainless steel storage tank and refrigerated at 4°C for 12 hours to form a gel. The temperature was then raised to 20°C within 2 hours, and 0.9 parts of preservative were added. The mixture was stirred at 300rpm for 15 minutes. Finally, the mixture was filtered through a 0.45μm filter membrane for sterilization to obtain a composition containing irisinin.
[0042] Example 2
[0043] A composition containing irisinin comprises the following raw materials in parts by weight: 1 part of complex irisinin, 2 parts of hydroxyapatite microspheres, 0.8 parts of modified hyaluronic acid, 70 parts of deionized water, 2 parts of D-limonene microemulsion, 3 parts of glycerol, 2 parts of 1,3-propanediol, 0.1 parts of carbomer 940, 0.15 parts of triethanolamine, 0.6 parts of preservative, 0.15 parts of disodium EDTA, and 0.1 parts of sodium citrate.
[0044] The preservative is a mixture of phenoxyethanol and ethylhexylglycerin, with a mass ratio of 9:1, and the hydroxyapatite microspheres have a particle size of 180 nm.
[0045] The preparation of the compound irisinogen includes the following steps: 1 part by weight of irisinogen and 1 part by weight of poloxamer 407 are dissolved in 5 parts by weight of anhydrous ethanol at 58°C. The mixture is ultrasonically treated at 180W for 35 minutes. Then, pre-cooled deionized water is added dropwise at a rate of 0.9 mL / min in an ice bath at 4°C. When the turbidity of the system reaches 23 NTU, the addition of water is stopped, and stirring is continued for 12 minutes to form a homogeneous suspension. Finally, the suspension is pre-frozen at -80°C for 2.5 hours and transferred to a freeze dryer for 24 hours at -50°C and 8 Pa. The freeze-drying process is divided into three stages: first, initial sublimation is carried out at -30°C for 8 hours; then, the temperature is raised to -10°C and maintained for 6 hours to complete the main sublimation; finally, desorption and drying are carried out at 25°C for 10 hours. The mixture is then pulverized through a 120-mesh sieve to obtain the compound irisinogen.
[0046] The preparation of the D-limonene microemulsion specifically includes the following steps: 0.8 parts of 1,3-propanediol is mixed with 0.4 parts of D-limonene, stirred at 280 rpm for 6 minutes, 1.6 parts of deionized water is added at a speed of 0.9 L / min, and stirred at 480 rpm for 12 minutes to form a coarse emulsion; the coarse emulsion is sheared at 9500 rpm for 3.5 minutes, and then ultrasonically treated at 140 W and 20 kHz for 2.5 minutes to prepare the D-limonene microemulsion, the particle size of the D-limonene microemulsion is 50 nm, and the D-limonene microemulsion is stored at 4°C for standby.
[0047] A preparation method of a composition containing tectorigenin, specifically including the following steps:
[0048] S1, water phase matrix preparation: 54 parts of deionized water is added to a reaction kettle, 0.1 parts of carbomer 940 is slowly added at a rate of 0.35 parts / min under stirring at 280 rpm, and is left to swell for 2.5 hours; then the stirring speed is increased to 580 rpm, 3 parts of glycerol, 1.5 parts of 1,3-propanediol, 0.15 parts of disodium EDTA, and 0.1 parts of sodium citrate are sequentially added, and stirred for 35 minutes until the system is uniform; the pH is adjusted to 5.8 to obtain a water phase matrix, which is stored at 24°C for standby.
[0049] S2, preparation of composite tectorigenin dispersion: 8 parts of deionized water is added to a reaction tank, heated to 39°C, 1 part of composite tectorigenin is added, and stirred at 780 rpm for 22 minutes until completely dispersed; 0.5 parts of 1,3-propanediol is added, heated to 59°C, and continuously stirred for 12 minutes, and maintained at 59°C for standby, to obtain a composite tectorigenin dispersion.
[0050] S3, preparation of nanosphere-hyaluronic acid complex: 2 parts of hydroxyapatite microspheres are dispersed in 8 parts of deionized water, transferred to a 30°C constant temperature water bath reaction tank, ultrasonically treated at 95 W and 20 kHz for 12 minutes; then 0.8 parts of modified hyaluronic acid is added, and stirred at 980 rpm for 35 minutes, and cooled to 24°C for standby, to obtain a nanosphere-hyaluronic acid complex.
[0051] S4, composite system construction: the water phase matrix is transferred to an emulsification tank, heated to 34.5°C at a rate of 0.8°C / min, 2 parts of D-limonene microemulsion is added, and stirred at 580 rpm for 6 minutes; the composite tectorigenin dispersion is slowly added, and stirred at 780 rpm for 10 minutes; then the temperature is decreased to 24.5°C at a rate of 0.8°C / min, the nanosphere-hyaluronic acid complex is added, and stirred at 1450 rpm for 22 minutes, to obtain a composite system.
[0052] S5. Homogenization and post-treatment: The composite system was kept at 24.5℃ and homogenized 5 times under a pressure of 7800psi. Then, 0.15 parts of triethanolamine were added, and the mixture was stirred at 480rpm for 12 minutes to adjust the pH to 6.1. The mixture was then transferred to a stainless steel storage tank and refrigerated at 4℃ for 14 hours to form a gel. The temperature was then raised to 19℃ over 2.5 hours, and 0.6 parts of preservative were added. The mixture was stirred at 280rpm for 18 minutes. Finally, the mixture was filtered through a 0.45μm filter membrane for sterilization to obtain a composition containing irisin.
[0053] Example 3
[0054] A composition containing irisinin comprises the following raw materials in parts by weight: 2 parts of complex irisinin, 3 parts of hydroxyapatite microspheres, 1.2 parts of modified hyaluronic acid, 80 parts of deionized water, 5 parts of D-limonene microemulsion, 6 parts of glycerol, 5 parts of 1,3-propanediol, 0.4 parts of carbomer 940, 0.25 parts of triethanolamine, 1.2 parts of preservative, 0.25 parts of disodium EDTA, and 0.6 parts of sodium citrate.
[0055] The preservative is a mixture of phenoxyethanol and ethylhexylglycerin, with a mass ratio of 9:1. The hydroxyapatite microspheres have a particle size of 220 nm.
[0056] The preparation of the compound irisinogen includes the following steps: 1 part by weight of irisinogen and 1.5 parts by weight of poloxamer 407 are dissolved in 6 parts by weight of anhydrous ethanol at 62℃. The mixture is ultrasonically treated at 220W for 25 minutes. Then, pre-cooled deionized water is added dropwise at a rate of 1.1 mL / min in an ice bath at 4℃. When the turbidity of the system reaches 27 NTU, the addition of water is stopped, and stirring is continued for 8 minutes to form a homogeneous suspension. Finally, the suspension is pre-frozen at -80℃ for 1.8 hours and transferred to a freeze dryer for 24 hours at -50℃ and 8 Pa. The freeze-drying process is divided into three stages: first, initial sublimation is carried out at -30℃ for 8 hours; then, the temperature is raised to -10℃ and maintained for 6 hours to complete the main sublimation; finally, the mixture is desorbed and dried at 25℃ for 10 hours. The resulting product is then pulverized through a 120-mesh sieve to obtain the compound irisinogen.
[0057] The preparation of D-limonene microemulsion specifically includes the following steps: 1.5 parts of 1,3-propanediol and 0.75 parts of D-limonene are mixed and stirred at 320 rpm for 4 minutes. 3.0 parts of deionized water are added at a rate of 1.1 L / min, and the mixture is stirred at 520 rpm for 8 minutes to form a crude emulsion. The crude emulsion is sheared at 10500 rpm for 2.5 minutes and then ultrasonically treated at 160 W and 20 kHz for 1.5 minutes to obtain D-limonene microemulsion with a particle size of 100 nm. The microemulsion is kept at 4 °C for later use.
[0058] A method for preparing a composition containing irisinogen specifically includes the following steps:
[0059] S1, water phase matrix preparation: 56 parts of deionized water was added into the reaction kettle, 0.4 parts of carbomer 940 was slowly added at a rate of 0.45 parts / min under stirring at 320 rpm, and was left to swell for 1.8 hours; then the stirring speed was increased to 620 rpm, 6 parts of glycerol, 3 parts of 1,3-propanediol, 0.25 parts of disodium EDTA, and 0.6 parts of sodium citrate were added in sequence, and the system was stirred for 25 minutes until it was uniform; the pH was adjusted to 6.2, and the water phase matrix was obtained and was kept at 26°C for standby.
[0060] S2, composite iridin dispersion liquid preparation: 12 parts of deionized water was added into the reaction kettle, and was heated to 41°C; 2 parts of composite iridin was added, and was stirred at 820 rpm for 18 minutes until it was completely dispersed; 2 parts of 1,3-propanediol was added, and was heated to 61°C, and was continuously stirred for 8 minutes, and was kept at 61°C for standby, and the composite iridin dispersion liquid was obtained.
[0061] S3, nanosphere-hyaluronic acid complex preparation: 3 parts of hydroxyapatite microspheres was dispersed in 12 parts of deionized water, and was transferred into a 30°C constant temperature water bath reaction kettle, and was ultrasonically treated at 105 W and 20 kHz for 8 minutes; then 1.2 parts of modified hyaluronic acid was added, and was stirred at 1020 rpm for 25 minutes, and was cooled to 26°C for standby, and the nanosphere-hyaluronic acid complex was obtained.
[0062] S4, composite system construction: the water phase matrix was transferred into an emulsification kettle, and was heated to 35.5°C at a rate of 1.2°C / min, and 5 parts of D-limonene microemulsion was added, and was stirred at 620 rpm for 4 minutes; the composite iridin dispersion liquid was slowly added, and was stirred at 820 rpm for 15 minutes; then the nanosphere-hyaluronic acid complex was added after the temperature was decreased to 25.5°C at a rate of 1.2°C / min, and was stirred at 1550 rpm for 18 minutes, and the composite system was obtained.
[0063] S5, homogeneous gelation and post-treatment: the composite system was kept at 25.5°C, and was homogenized for 4 times by pressure cycling at 8200 psi; then 0.25 parts of triethanolamine was added, and was stirred at 520 rpm for 8 minutes, and the pH was adjusted to 6.5; then it was transferred into a stainless steel storage tank, and was refrigerated at 4.5°C for 13 hours to form a gel; then it was heated to 21°C in 1.8 hours, and 1.2 parts of a preservative was added, and was stirred at 320 rpm for 12 minutes; finally it was filtered through a 0.45 μm filter membrane to remove bacteria, and the composition containing iridin was obtained.
[0064] Comparative Example 1
[0065] The difference from Example 1 is that no hydroxyapatite microspheres was added, and the rest of the ingredients and preparation methods are the same as those of Example 1.
[0066] Comparative Example 2
[0067] The difference from Example 1 is that the modified hyaluronic acid was replaced with an equal amount of ordinary hyaluronic acid (without cholesterol modification), while the other components and preparation methods were the same as in Example 1.
[0068] Comparative Example 3
[0069] The difference from Example 1 is that the complex irisinogen is replaced with an equal amount of uncomplexed irisinogen (i.e., it does not form a complex with poloxamer 407, and the raw irisinogen is used directly), while the other components and preparation methods are the same as in Example 1.
[0070] Comparative Example 4
[0071] The difference from Example 1 is that the mass ratio of irisin to poloxamer 407 in the compound irisin was adjusted to 1:0.8, while the other components and preparation methods were the same as in Example 1.
[0072] Test case
[0073] 1. Light stability test
[0074] Test samples: The compositions prepared in Examples 1-3 and Comparative Examples 1-4 were selected as test subjects. Each sample was accurately weighed at 5.0 g and placed into 10 mL transparent quartz sample bottles and sealed. Three parallel samples were set up for each sample, and a blank matrix without irisin was used as a negative control. All samples were equilibrated at 25 °C in a light-protected environment for 24 h before the test.
[0075] Test Method: An accelerated irradiation system was constructed using a UV-Vis composite aging test chamber. The UV (290-400nm) irradiation intensity was set at 0.8W / m², and the visible (400-800nm) irradiation intensity was set at 2.0W / m². The temperature inside the test chamber was controlled at 25±1℃, the relative humidity at 50±3%, and the sample rack rotation speed at 5r / min to ensure uniform irradiation. The samples were placed in the test chamber for continuous irradiation. The samples were removed at 0h, 24h, 48h, 72h, 96h, and 120h, and allowed to stand in the dark for 30min before the performance indicators were measured.
[0076] Test index: The index is the retention rate of irisin, which is determined by high performance liquid chromatography (HPLC). The chromatographic conditions are as follows: C18 column (4.6 mm × 250 mm, 5 μm), mobile phase is methanol-0.1% phosphoric acid aqueous solution (55:45, v / v), detection wavelength is 260 nm, column temperature is 30 ℃, flow rate is 1.0 mL / min, injection volume is 20 μL, and the retention rate is calculated as the percentage of the content at each time point to the initial content at 0 h.
[0077] The data from the photostability test are shown in Table 1.
[0078] Table 1
[0079]
[0080] As shown in Table 1, the compositions prepared in Examples 1-3 of this invention exhibited excellent photostability, with a irisin retention rate of 92.5%-93.8% after 120 hours of continuous light irradiation. In contrast, the retention rates of Comparative Examples 1-4 (deleted hydroxyapatite microspheres, used ordinary hyaluronic acid, used directly without irisin, and with altered poloxamer 407 ratio) significantly decreased to 27.6%-49.5%. This fully demonstrates that the physical ultraviolet barrier formed synergistically by hydroxyapatite microspheres and modified hyaluronic acid in this invention can effectively protect irisin from photodegradation.
[0081] 2. Temperature response release test
[0082] Test samples: The compositions containing irisin prepared in Examples 1, 2 and 3, as well as the compositions prepared in Comparative Examples 1, 2, 3 and 4, were selected. Each sample was accurately weighed 2.0 g and placed in a dialysis bag (molecular weight cutoff of 10 kDa). After sealing, it was used as a test unit. Three sets of parallel test units were set up for each sample.
[0083] Test Method: An in vitro dialysis method was used to simulate the temperature changes before and after skin contact. Two release systems were set up: a low-temperature release system (25℃, simulating storage conditions) and a body-temperature release system (37℃, simulating skin contact conditions). The release medium for both systems was phosphate-buffered saline (PBS) at pH 7.4, with a volume of 50 mL. The magnetic stirring speed was controlled at 100 rpm. The test unit was placed in the release medium at both temperatures. At 0.5 h, 1 h, 2 h, 4 h, 8 h, and 12 h of release, 1 mL of the release solution was accurately aspirated from the release system, and an equal volume of fresh PBS buffer was added to maintain a constant system volume. The aspirated release solution was filtered through a 0.22 μm filter membrane, and the content of irisinogen was determined by high-performance liquid chromatography (HPLC). The chromatographic conditions were: C18 column (4.6 mm × 250 mm, 5 μm), mobile phase: methanol-0.1% phosphoric acid aqueous solution (55:45, v / v), detection wavelength: 260 nm, column temperature: 30℃, flow rate: 1.0 mL / min, injection volume: 20 μL. The theoretical total content was obtained by taking an equal amount of sample (2.0g), ultrasonically extracting it with 10mL of methanol for 30 minutes, centrifuging it at 10000rpm for 10 minutes, collecting the supernatant, and determining the total amount of iris aglycone under the same HPLC conditions.
[0084] Test index: Calculate the cumulative release rate of irisin in the sample at each time point. Cumulative release rate = actual cumulative release amount / theoretical total content × 100%.
[0085] The data from the temperature response release test are shown in Tables 2 and 3.
[0086] Table 2
[0087]
[0088] Table 3
[0089]
[0090] As shown in Table 2, under simulated storage conditions at 25°C, the cumulative release rate of irisin in Examples 1-3 was only 13.9%-15.2% after 12 hours, indicating a slow release rate; while the cumulative release rate of Comparative Examples 1-4 was as high as 52.8%-89.3%. This demonstrates that the formulation structure of the present invention (especially the three-dimensional network constructed from poloxamer 407 and modified hyaluronic acid) can effectively lock in the active ingredients under low-temperature conditions, significantly reducing activity loss during storage and ensuring that the product maintains high activity throughout its shelf life.
[0091] As shown in Table 3, under simulated skin contact conditions at 37°C, Examples 1-3 achieved a cumulative release rate of 88.5%-93.2% of irisin within 12 hours, indicating sufficient release. While Comparative Example 3 also reached 99.2%, it released 32.7% within 0.5 hours, exhibiting a significant burst release phenomenon. The compositions of this invention demonstrate ideal temperature response characteristics, enabling continuous and stable release of active ingredients at skin temperature, avoiding the irritation caused by burst release, while extending the effective duration of action, thus improving the user experience and the duration of efficacy.
[0092] In summary, this invention successfully solves the industry problem of poor photostability and easy degradation and inactivation of irisin in cosmetics by constructing a physical ultraviolet barrier with hydroxyapatite microspheres, forming a temperature-sensitive carrier with poloxamer 407, enhancing structural stability with modified hyaluronic acid, and promoting transdermal absorption with D-limonene microemulsion. At the same time, it achieves intelligent delivery of "low-temperature locking and body temperature release", providing an innovative technical solution for the development of highly efficient and stable whitening and anti-aging cosmetics.
[0093] The above description is merely a preferred embodiment of the present invention and is not intended to limit the present invention in any way. Although the present invention has been disclosed above with reference to preferred embodiments, it is not intended to limit the present invention. Any person skilled in the art can make some modifications or alterations to the above-disclosed technical content to create equivalent embodiments without departing from the scope of the present invention. Any simple modifications, equivalent changes and alterations made to the above embodiments based on the technical essence of the present invention without departing from the scope of the present invention shall still fall within the scope of the present invention.
Claims
1. A composition comprising irilone, wherein the composition is characterized by, The raw materials include the following weight parts: 1-2 parts of composite iridin, 2-3 parts of hydroxyapatite microspheres, 0.8-1.2 parts of modified hyaluronic acid, and 70-80 parts of deionized water; The composite iridin is a complex of iridin and poloxamer 407; The modified hyaluronic acid is cholesterol-modified hyaluronic acid.
2. The composition containing iridin according to claim 1, characterized by, In the composite iridin, the mass ratio of iridin to poloxamer 407 is 1:1-1.
5.
3. The composition containing iridin of claim 1, wherein the composition is a cosmetic composition. The particle size of the hydroxyapatite microspheres is 180-220 nm.
4. The composition containing iridin of claim 1, wherein the composition is a cosmetic composition. It also includes 2-5 parts of D-limonene microemulsion, and the particle size of the D-limonene microemulsion is 50-100 nm.
5. The composition containing iridin of claim 4, wherein the composition is a cosmetic composition. It also includes 3-6 parts of glycerol, 2-5 parts of 1,3-propanediol, 0.1-0.4 parts of carbomer 940, 0.15-0.25 parts of triethanolamine, 0.6-1.2 parts of preservative, 0.15-0.25 parts of disodium EDTA, and 0.1-0.6 parts of sodium citrate.
6. The composition containing iridin of claim 5, wherein the composition is a cosmetic composition. The preservative is a mixture of phenoxyethanol and ethylhexylglycerin, and the mass ratio of phenoxyethanol to ethylhexylglycerin is 9:
1.
7. The composition containing iridin of claim 5, wherein the composition is a cosmetic composition. The preparation of the composition includes the following steps: S1, add carbomer 940 to deionized water, stand for swelling, then add glycerol, 1,3-propanediol, disodium EDTA and sodium citrate in sequence, stir until uniform, adjust pH, and obtain an aqueous phase matrix; S2, mix the composite iridin with deionized water, stir uniformly at 40±1℃, then add 1,3-propanediol, heat to 60±1℃, and stir to obtain a composite iridin dispersion; S3, disperse the hydroxyapatite microspheres in deionized water, ultrasonic treatment, then add modified hyaluronic acid, stir uniformly at 30±0.5℃, and obtain a nanosphere-hyaluronic acid complex; S4, stir the D-limonene microemulsion and the aqueous phase matrix uniformly, then add the composite iridin dispersion and stir uniformly, and then add the nanosphere-hyaluronic acid complex and stir uniformly, and obtain a composite system; S5, subject the composite system to microfluidization treatment, then add triethanolamine and stir uniformly, adjust pH, then refrigerate to form a gel, then add a preservative and stir uniformly, and finally filter and sterilize to obtain the composition containing iridin.
8. The composition containing iridin of claim 7, wherein the composition is a cosmetic composition. In step S4, the following temperature control program is used: first heat the aqueous phase matrix to 35±0.5℃ at a heating rate of 1±0.2℃ / min, add the D-limonene microemulsion and stir uniformly; then add the composite iridin dispersion and stir uniformly; then cool to 25±0.5℃ at a cooling rate of 1±0.2℃ / min, and finally add the nanosphere-hyaluronic acid complex and stir uniformly at 25±0.5℃ to obtain the composite system.
9. The composition comprising iridin of claim 7, wherein the composition is a cosmetic composition. In step S5, the microfluidization pressure is 8000±200psi, the number of circulation homogenization is 3-5 times, the refrigeration temperature is 4±0.5℃, and the refrigeration time is 12-14 hours.
10. A whitening anti-aging cosmetic, characterized by, The cosmetic product contains the composition as claimed in any one of claims 1-9, and the dosage form of the cosmetic product is a gel, an emulsion, a serum, or a cream.