A supramolecular whitening composition Yves X White and its preparation method and application
A supramolecular complex system of vine tea extract, resveratrol, nicotinamide, and arbutin was constructed using high-pressure homogenization and ultrafiltration technologies. This solved the problem of poor solubility of vine tea extract and resveratrol in high-concentration aqueous solutions, achieving stable synergistic effects of multiple active ingredients and improving whitening effects and product stability.
Patent Information
- Application Number
- CN202610172927.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2026-02-06
- Publication Date
- 2026-07-10
AI Technical Summary
In existing technologies, vine tea extract and resveratrol have poor solubility and are easily oxidized in solutions with high water content, resulting in poor whitening effects. Furthermore, traditional multi-active ingredient mixture systems are prone to stratification and precipitation.
Using high-pressure homogenization and ultrafiltration technology, a supramolecular whitening composition YvesXWhite is formed by combining vine tea extract, resveratrol, nicotinamide and arbutin. The orderly self-assembly of multiple active ingredients is achieved by utilizing π–π stacking, hydrogen bonding and hydrophobic interactions to form a stable supramolecular system.
It improves the solubility and stability of the supramolecular whitening composition, enhances the whitening effect, significantly increases the melanin production inhibition rate, and extends the product's shelf life and expiration date.
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Abstract
Description
Technical Field
[0001] This invention belongs to the field of cosmetic preparation technology, specifically relating to a supramolecular whitening composition YvesXWhite, its preparation method, and its application. Background Technology
[0002] In recent years, skin whitening has become a key area of research and development in cosmetics, attracting widespread attention from consumers and the scientific community worldwide. Traditionally, fair and radiant skin is a symbol of beauty in Eastern cultures, while in Western markets, even skin tone and reduced pigmentation are equally important skincare needs. The main cause of skin pigmentation is the excessive production of melanin and its abnormal distribution in the epidermis. Research indicates that tyrosinase is the key rate-limiting enzyme in melanin biosynthesis; therefore, inhibiting tyrosinase activity has become a primary strategy in whitening product development. Commonly used whitening active ingredients both domestically and internationally include vitamin C and its derivatives, arbutin, kojic acid, azelaic acid, and niacinamide. These ingredients exert their effects through multiple pathways, such as inhibiting melanin production, promoting keratinocyte renewal, and providing antioxidant benefits. With the rise of safety and natural sourcing concepts, more and more research is focusing on the whitening potential of plant extracts and natural compounds, such as glycyrrhizic acid, resveratrol, and flavonoids. The development trend in the whitening field will place greater emphasis on multi-target regulatory mechanisms and the construction of skin barrier-friendly formulas to achieve gentle, safe, and long-lasting whitening effects. However, some naturally occurring whitening compounds are often poorly soluble in water or safe organic solvents, such as dihydromyricetin and resveratrol. Therefore, developing a supramolecular composition with good solubility, multiple whitening effects, and synergistic effects to further enhance the whitening effect is of great significance in the cosmetics industry. Summary of the Invention
[0003] To overcome the shortcomings and deficiencies of the existing technology and solve the problems of low solubility, easy precipitation, and easy oxidation of vine tea extract and resveratrol in solutions with a water content higher than 50 wt%, the primary objective of this invention is to provide a method for preparing the supramolecular whitening composition YvesXWhite. In the raw material combination process, the pre-dissolution step of this invention can avoid the "hydrophobic cage" effect. Dihydromyricetin serves as the framework and bridging core, resveratrol serves as the π-π support and hydrophobic assembly core, arbutin serves as the hydrophilic linker and interface regulator, and nicotinamide serves as the polar regulator and hydrogen bond bridger. This results in a supramolecular whitening composition with good solubility, resistance to oxidation and precipitation, and stronger biological activity than single substances. When used in cosmetic whitening products, it can significantly enhance the whitening effect.
[0004] Another object of the present invention is to provide a supramolecular whitening composition YvesXWhite prepared by the above preparation method.
[0005] Another object of the present invention is to provide the application of the above-mentioned supramolecular whitening composition YvesXWhite.
[0006] Another object of the present invention is to provide a whitening essence water prepared from the above-mentioned supramolecular whitening composition YvesXWhite.
[0007] The objective of this invention is achieved through the following technical solution: A method for preparing a supramolecular whitening composition YvesXWhite includes the following steps: using vine tea extract, resveratrol, nicotinamide and arbutin as active ingredients, pre-dissolving the alcoholic solution of the active ingredients by high-pressure homogenization, then stirring under water bath conditions to obtain a mixed solution of supramolecular whitening composition, and finally purifying by ultrafiltration to obtain the supramolecular whitening composition YvesXWhite.
[0008] The preparation method of the above-mentioned supramolecular whitening composition YvesXWhite specifically includes the following steps: (1) Preparation of vine tea extract: Vine tea powder and water were mixed at a mass ratio of 1:(10~15), and the mixture was stirred in a water bath at 20~25℃ for 20~30 min for decolorization. The filter residue was vacuum dried at 45~50℃. The dried powder was mixed with 95% ethanol at a mass ratio of 1:(20~25), and the mixture was stirred in a water bath at 50~55℃ for 60~90 min for extraction. The extract was then concentrated, water-precipitated, and centrifuged to obtain a precipitate. The precipitate was freeze-dried to obtain vine tea extract. (2) High-pressure homogenization pre-dissolution: The vine tea extract, resveratrol, nicotinamide, arbutin and butylene glycol obtained in step (1) are mixed in a mass ratio of (2~5):(1~3):(3~6):(1~3):(35~85), and then homogenized using a high-pressure homogenizer to obtain a pre-solution; the homogenization is carried out under the following conditions: pressure of 50~80 MPa, number of cycles of 1~3, and cycle temperature of 10~25℃; (3) Preparation of supramolecular whitening composition mixed solution: The pre solution obtained in step (2) is mixed with water at a mass ratio of 1: (1~5), and then stirred in a water bath at 50~55℃ for 20~30min. Then, it is centrifuged at 5000~6000r / min for 3~5min. The supernatant is taken as the supramolecular whitening composition mixed solution. (4) Ultrafiltration purification: The mixed solution of supramolecular whitening composition obtained in step (3) is separated using a 900 Da hollow fiber ultrafiltration membrane, and the retentate is taken to obtain the supramolecular whitening composition YvesXWhite.
[0009] The separation in step (4) is performed using a 900 Da hollow fiber ultrafiltration membrane because the molecular weight of the supramolecular whitening composition formed by dihydromyricetin (molecular weight 320.25), resveratrol (molecular weight 228.24), nicotinamide (molecular weight 122.12), and arbutin (molecular weight 272.25) is definitely greater than 900 Da. The retentate obtained after separation by the 900 Da hollow fiber ultrafiltration membrane is the supramolecular whitening composition product required by the present invention, while the molecular weight of other impurities or unreacted substances cannot reach 900 Da, and therefore they are filtered out by the 900 Da hollow fiber ultrafiltration membrane.
[0010] A supramolecular whitening composition, YvesXWhite, prepared according to the above preparation method.
[0011] The application of the above-mentioned supramolecular whitening composition YvesXWhite in the preparation of cosmetics.
[0012] A whitening essence water prepared from the above-mentioned supramolecular whitening composition YvesXWhite, wherein the whitening essence water is prepared according to the following steps: (1) Mix water, glycerol, disodium ethylenediaminetetraacetate and p-hydroxyacetophenone in a mass ratio of 70:29.4:0.1:0.5 evenly, put them into the main pot, heat to 85~90℃, homogenize for 1~4 min, keep warm for 20~30 min, and then cool down to 45~50℃ to obtain phase A; (2) Weigh the above supramolecular whitening composition YvesXWhite, 1,2-hexanediol and deionized water in a mass ratio of 1:4:5 and mix them evenly to obtain phase B; (3) Add phase B, which accounts for 5% of the mass fraction of phase A, to phase A, stir evenly, filter the material through a 400-mesh filter cloth, and obtain whitening essence water.
[0013] The principle of this invention: This invention provides a supramolecular whitening composition, YvesXWhite, which exhibits good solubility in aqueous alcohol solutions and enhances whitening effects through high-pressure homogenization and ultrafiltration technologies. This supramolecular whitening composition is derived from vine tea extract (mainly dihydromyricetin), resveratrol, arbutin, and niacinamide through various interactions. The formation process and final morphology of the supramolecular whitening composition are described below. Figure 1As shown, its formation mechanism includes: (1) The nonpolar parts of each molecule (such as aromatic ring skeleton, thiobenzoyl group, etc.) tend to aggregate in water to reduce contact with water molecules. This driving force causes the hydrophobic regions of the molecules to aggregate inward to form a hydrophobic core, while the hydrophilic groups face the water phase. Therefore, due to the hydrophobic effect, the nonpolar parts of each molecule spontaneously approach each other to form a hydrophobic aggregate; (2) The hydrogen bonds contained on the molecules of dihydromyricetin, resveratrol and arbutin with multiple hydroxyl groups form a network of weak bonds with the amide and hydroxyl groups contained on nicotinamide through intermolecular interactions; (3) Through the π-π superposition on the aromatic ring structure of resveratrol, it interacts with the polyhydroxy molecules in other components to enhance intermolecular contact; (4) It forms a eutectic or eutectic structure, thereby changing the melting point and improving the tendency of thermal, light and oxidative degradation; (5) Butanediol is used as a carrier to assist the formation of microstructures of each raw material molecule together with the carrier, thereby restricting the free movement of single molecules and reducing external damage. The supramolecular whitening composition obtained by this invention retains the functions of a single active substance while reducing the amount of alcohol used (i.e., indirectly enhancing the solubility of the active substance). At the same time, the active molecules are in a "protected" state in the supramolecular structure, which can reduce denaturation caused by degradation, oxidation, light, heat, and humidity, thereby improving stability and bioavailability.
[0014] The present invention has the following advantages and beneficial effects compared with the prior art: (1) This invention first constructed a supramolecular composite system of vine tea extract, resveratrol, nicotinamide and arbutin; through the π–π stacking effect, hydrogen bond and hydrophobic interaction between molecules, the orderly self-assembly of multiple active components is achieved to form a stable supramolecular whitening system, overcoming the problems of easy layering and precipitation in traditional multi-active mixed systems.
[0015] (2) This invention uses dihydromyricetin in vine tea extract as a supramolecular framework and bridging core to achieve structural assembly innovation; dihydromyricetin serves as a support center and forms an organic synergistic molecular network with resveratrol, nicotinamide and arbutin, thereby improving the spatial stability and synergistic bioactivity of the supramolecular whitening composition.
[0016] (3) This invention achieves maximum synergistic effect by clearly defining the functional division of molecules: resveratrol provides hydrophobic π–π support, arbutin acts as a hydrophilic interface regulator, and nicotinamide acts as a polarity regulator and hydrogen bond bridging agent, thereby improving the dispersibility and solubility of the supramolecular whitening composition in an aqueous environment.
[0017] (4) The present invention uses high pressure homogenization pre-dissolution technology to achieve molecular-level premixing and dissolution of a variety of poorly soluble active substances; cyclic homogenization at 50~80 MPa and 10~25℃ effectively breaks the hydrophobic cage effect, avoids thermal degradation and oxidation reaction, and significantly improves the uniformity and stability of supramolecular whitening composition.
[0018] (5) The supramolecular whitening composition prepared by the present invention has good solubility, is not easy to precipitate, and has good antioxidant properties. It solves the problems of poor solubility and easy oxidation of vine tea extract and resveratrol in high water content systems, and extends the shelf life and shelf life of the product.
[0019] (6) The supramolecular whitening composition of the present invention exhibits a significant synergistic enhancement effect. Compared with single components, the supramolecular whitening composition has a significant improvement in whitening and exhibits a higher melanin production inhibition rate.
[0020] (7) The supramolecular whitening composition constructed by the present invention through high pressure homogenization and ultrafiltration technology breaks through the technical bottleneck of limited solubility and stability of traditional active ingredients in aqueous system, and realizes systematic innovation from molecular design, process innovation to product application, with significant scientific value and industrial application prospects. Attached Figure Description
[0021] Figure 1 This diagram illustrates the formation process and final morphology of the supramolecular whitening composition YvesXWhite of this invention.
[0022] Figure 2 This is the total ion spectrum in negative ion mode of the supramolecular whitening composition YvesXWhite of the present invention.
[0023] Figure 3 This is the total ion spectrum in positive ion mode of the supramolecular whitening composition YvesXWhite of the present invention.
[0024] Figure 4 This is a fragment ion diagram of arbutin in negative ion mode.
[0025] Figure 5 This is a fragment ion diagram of dihydromyricetin in negative ion mode.
[0026] Figure 6 This is a fragment ion diagram of resveratrol in negative ion mode.
[0027] Figure 7 This is a fragment ion diagram of nicotinamide in positive ion mode.
[0028] Figure 8 A comparison chart showing the changes in penetration volume between supramolecular whitening composition solutions and simple mixed solutions. Detailed Implementation
[0029] The following specific embodiments further illustrate the content of the present invention, but should not be construed as limiting the present invention.
[0030] Example 1 (1) Preparation of vine tea extract: Vine tea powder and water were mixed at a mass ratio of 1:10 and stirred in a water bath at 25°C for 30 min for decolorization. The filter residue was vacuum dried at 50°C. The dried powder was mixed with 95% ethanol at a mass ratio of 1:20 and stirred in a water bath at 55°C for 60 min for extraction. The extract was then concentrated, water-precipitated and centrifuged to obtain a precipitate. The precipitate was freeze-dried to obtain vine tea extract. (2) High-pressure homogenization pre-dissolution: The vine tea extract, resveratrol, nicotinamide, arbutin and butylene glycol obtained in step (1) are mixed in a mass ratio of 2:1:3:1:35, and then homogenized using a high-pressure homogenizer to obtain a pre-solution; the homogenization is carried out under the following conditions: pressure of 50 MPa, number of cycles of 2, and cycle temperature of 10℃; (3) Preparation of supramolecular whitening composition mixed solution: The pre-solution obtained in step (2) is mixed with water at a mass ratio of 1:1, and then stirred in a water bath at 55°C for 30 min. After that, it is centrifuged at 5000 r / min for 5 min and the supernatant is taken, which is the supramolecular whitening composition mixed solution. (4) Ultrafiltration purification: The mixed solution of supramolecular whitening composition obtained in step (3) is separated using a 900 Da hollow fiber ultrafiltration membrane, and the retentate is taken to obtain the supramolecular whitening composition YvesXWhite.
[0031] Example 2 The other steps in this embodiment are the same as in Example 1, except that in step (2), vine tea extract, resveratrol, nicotinamide, arbutin and butylene glycol are mixed in a mass ratio of 5:1:3:1:35; the supramolecular whitening composition YvesXWhite is finally obtained in this embodiment.
[0032] Example 3 The other steps in this embodiment are the same as in embodiment 1, except that the number of cycles in the homogenization condition described in step (2) is 1; the supramolecular whitening composition YvesXWhite is finally obtained in this embodiment.
[0033] Example 4 The other steps in this embodiment are the same as in embodiment 1, except that: resveratrol is not added in step (2), and the hollow fiber ultrafiltration membrane used in step (4) is 500 Da, and the retentate is taken.
[0034] Example 5 The other steps in this embodiment are the same as in embodiment 1, except that: nicotinamide is not added in step (2) and the hollow fiber ultrafiltration membrane used in step (4) is 500 Da, and the retentate is taken.
[0035] Comparative Example 1 The other steps in this embodiment are the same as in Example 1, except that the ultrafiltration purification in step (4) is not performed to obtain the composition.
[0036] Comparative Example 2 The other steps of this comparative example are the same as those of Example 1, except that resveratrol is not added in step (2) and ultrafiltration purification in step (4) is not performed to obtain the composition.
[0037] Comparative Example 3 The other steps of this comparative example are the same as those in Example 1, except that nicotinamide is not added in step (2), and ultrafiltration purification in step (4) is not performed to obtain the composition.
[0038] Comparative Example 4 The other steps of this comparative example are the same as those in Example 1, except that the butanediol used in step (2) is replaced with water, and the ultrafiltration purification in step (4) is not performed to obtain the composition.
[0039] Comparative Example 5 The other steps of this comparative example are the same as those of Example 1, except that: in step (2), high-pressure homogenization and pre-dissolution are not performed. Instead, the vine tea extract, resveratrol, nicotinamide, arbutin and butylene glycol obtained in step (1) are mixed in a mass ratio of 2:1:3:1:35 and then the operation of step (3) is carried out directly. The purification in step (4) is not performed to obtain the composition.
[0040] Example 1: Qualitative Experiment by HPLC-MS The components of the supramolecular whitening composition YvesXWhite obtained in Example 1, and the retentates obtained in Examples 4 and 5 were qualitatively analyzed by HPLC-MS in both positive and negative ion modes. The results showed that no active ingredients were detected in the retentates of Examples 4 and 5, indicating that all substances were filtered out by the 500 Da hollow fiber ultrafiltration membrane. Therefore, to avoid the removal of active substances and the inability to perform data comparison, ultrafiltration purification was not used in subsequent comparative examples. The total ion chromatogram of the supramolecular whitening composition obtained in Example 1 by HPLC-MS is shown below. Figure 2-3 As shown, the fragment spectrum is as follows Figure 4-7 As shown.
[0041] Depend on Figure 2-3 and Figure 4-7The data confirms that the supramolecular whitening composition contains active ingredients such as arbutin, dihydromyricetin, resveratrol, and nicotinamide. In Example 1, the supramolecular whitening composition solution prepared by mixing the raw materials was purified using a 900Da hollow fiber ultrafiltration membrane. This method utilizes the principle that the molecular weight of the supramolecular whitening composition is greater than 900, while the molecular weight of any single component or combination of non-four substances is less than 900. This process removes raw materials or other impurities that did not participate in the formation of the supramolecular whitening composition, ensuring that the obtained product is a supramolecular composition and avoiding interference from single components during detection. The HPLC-MS detection results in this example confirm that the supramolecular composition obtained by this invention consists of four components: arbutin, dihydromyricetin, resveratrol, and nicotinamide. Combined with the purification step, this further proves that the substance obtained by the preparation process of this invention is a supramolecular composition, rather than a simple mixture of single substances such as arbutin, dihydromyricetin, resveratrol, and nicotinamide.
[0042] Qualitative analysis by HPLC-MS revealed that the supramolecular whitening composition prepared in this invention simultaneously contained multiple functional small molecule components, including arbutin, dihydromyricetin, resveratrol, and nicotinamide. The actual retention times of these components were consistent with their corresponding standards (deviation < 0.02 min), and their parent ion and fragment ion characteristics were clear, with a stable fragmentation pattern, indicating that each component exists in its complete structure within the supramolecular whitening composition system of this invention. Based on the dual detection results of positive and negative ion modes, the composition of this invention exhibits the characteristic of stable coexistence of multiple hydrophilic and hydrophobic small molecules in the same system, demonstrating the highly stable nature of the constructed supramolecular structure. The HPLC-MS results further verified that the technical solution of this invention can achieve synergistic immobilization and controlled release of multiple active components, providing a foundation for subsequent efficacy studies.
[0043] Example 2: Permeability Test (Franz Diffusion Cell) The supramolecular whitening composition YvesXWhite obtained in Example 1 was quantified by HPLC-MS to prepare a supramolecular whitening composition solution with a dihydromyricetin mass fraction of 1%. Simultaneously, a simple mixed solution of dihydromyricetin, resveratrol, nicotinamide, and arbutin was prepared by HPLC-MS, with the dihydromyricetin mass fraction in the simple mixed solution being 1%. The amounts of resveratrol, nicotinamide, and arbutin added were all simulated to those in the aforementioned supramolecular whitening composition solution. Transdermal efficacy tests were performed on the aforementioned supramolecular whitening composition solution and the simple mixed solution, following the specific test methods described below: (1) Use the skin on the back of piglets, carefully peel off the subcutaneous fat layer and connective tissue, rinse it with physiological saline, and place it in physiological saline for later use; (2) Transdermal experiments were conducted using the Franz cell method. In the diffusion cell of the Franz diffusion apparatus, the exposed area of the back skin of the piglets treated in step (1) was 1.2 cm². 2 The receiving chamber has a volume of 15 mL; (3) Take 1 mL each of supramolecular whitening composition solution and simple mixed solution as test solutions and place them on the skin surface of the back of the treated piglets exposed in the diffusion pool; add 15 mL of physiological saline receiving solution to the receiving chamber and place it in a constant temperature water bath at 32±1℃ with a stirring speed of 300 r / min. (4) Subcutaneous sample collection: 1 mL of receiving fluid was collected at 3, 6, 21 and 24 h. 1 mL of receiving fluid was added to the receiving chamber immediately after sampling, and the sample was collected at 24 h. (5) The receiving liquid obtained after 24 hours of sampling was filtered through a 0.22µm microporous membrane and then detected by high performance liquid chromatography (HPLC).
[0044] (6) Test results are as follows Figure 8 As shown: by Figure 8 It can be seen that after 24 hours of transdermal penetration, the permeation amount per unit area of the supramolecular whitening composition solution is 2.26 times that of the simple mixed solution. The results show that the permeation ability of the supramolecular whitening composition is far superior to that of the mixture obtained by simply mixing single raw materials.
[0045] Example 3: Tyrosinase Inhibition Rate Experiment Refer to T / GDCA 006—2021 Test Method for Inhibition of Tyrosinase Activity by Cosmetic Raw Materials (In Vitro Method): A 0.1 mol / L phosphate buffer solution (pH 6.8) was accurately prepared and set as a PBS buffer solution. An L-tyrosine solution with a concentration of 0.5 mg / mL was accurately prepared using the PBS buffer solution. A tyrosinase solution with a concentration of 500 U / mL was accurately prepared using the PBS buffer solution. Using a 1% (w / w) butanediol solution as a solvent, the compositions obtained in Examples 1-3 and Comparative Examples 1-5 were prepared into a sample solution containing a dihydromyricetin concentration of 50 µg / mL, wherein the dihydromyricetin was quantified by HPLC-MS. Subsequently, the samples were added and measured according to the standard method of T / GDCA 006—2021, and the results of the tyrosinase inhibition rate determination are shown in Table 1.
[0046] Table 1 Results of Tyrosinase Inhibition Rate Measurement
[0047] As shown in Table 1, the tyrosinase inhibition effect of the purified supramolecular whitening compositions obtained in Examples 1-3 is greater than that in Comparative Example 1. This is because no purification step was performed in Comparative Example 1, and the resulting composition contained both supramolecular whitening composition and monomeric substances. However, both were quantified during HPLC-MS, which led to a relative decrease in the proportion of supramolecular whitening composition. Therefore, the tyrosinase inhibition effect was significantly worse than that in Examples 1-3. Thus, the test results show that, under the condition that no purification of the composition is performed and the amount of dihydromyricetin added is the same, the purified supramolecular whitening composition is significantly better than the mixture of unpurified supramolecular whitening composition and monomers. In Comparative Examples 2-5, reducing the amount of raw materials, changing the solvent, or altering the extraction method all resulted in a significant decrease in the tyrosinase inhibition rate. This fully demonstrates that reducing any raw material, replacing the solvent butanediol with water, or omitting the high-pressure homogenization pre-dissolution step cannot form a supramolecular composition structure, and therefore cannot achieve the excellent technical effect of the supramolecular whitening composition formed by the process steps of this invention. The compositions obtained in Examples 1-3 all showed greater tyrosinase inhibition effects than the compositions obtained in Comparative Examples 1-5. Therefore, the test results show that the supramolecular whitening composition obtained in the examples of this invention can effectively inhibit tyrosinase activity and has a good whitening effect.
[0048] Example 4: Immediate and Long-Lasting Whitening Effect Test (1) Preparation of instant and long-lasting whitening essence water The compositions obtained in Examples 1-3 and Comparative Examples 1-5 were first prepared into whitening essence water according to the following steps: (1) Mix water, glycerol, disodium ethylenediaminetetraacetate and p-hydroxyacetophenone in a mass ratio of 70:29.4:0.1:0.5 evenly, put them into the main pot, heat to 90℃, homogenize for 4 min, keep warm for 30 min, and then cool down to 45℃ to obtain phase A; (2) Weigh the above composition, 1,2-hexanediol and deionized water in a mass ratio of 1:4:5 and mix them evenly to obtain phase B; (3) Add phase B, which accounts for 5% of the mass fraction of phase A, to phase A, stir evenly, filter the material through a 400-mesh filter cloth, and obtain the whitening essence water.
[0049] (2) Test method Instant whitening effect test: Referring to the testing method for the skin whitening and freckle-removing efficacy of cosmetics (method 2), 60 healthy volunteers aged 18-30 years were selected and randomly divided into 10 groups of 6 people each. They applied essence water made from the supramolecular whitening composition obtained in Examples 1-3, essence water made from the composition obtained in Comparative Examples 1-5, and two commercially available skin whitening and freckle-removing products (where the main active ingredient of commercial product A is glycyrrhizic acid, and the main active ingredient of commercial product B is tea polyphenols) to their faces. The facial color parameters of the subjects were tested using a skin color meter (Colormeter CL400; CK, Germany) at four time points: before use and 10 min, 30 min, and 2 h after use. The skin translucency ITA° of the volunteers was obtained, and the results are shown in Table 2. The calculated values are average values.
[0050] The improvement rate of the immediate whitening effect test results is calculated using the following formula: Improvement rate (%) = (ITA° value after 2 hours of use - ITA° value before use) / ITA° value before use × 100 Table 2. Whitening Test ITA° Values
[0051] A higher ITA° value indicates brighter skin, while a lower ITA° value indicates duller skin, reflecting the skin's brightening and whitening effect. Table 2 shows that the results of Examples 1-3 indicate that the essence water prepared from the purified supramolecular whitening composition obtained in this invention significantly improves the skin's ITA° value before and after use. After 2 hours of application, the skin's ITA° value improves by more than 10%, demonstrating an immediate whitening and brightening effect. Comparative Example 1 shows greater effects than commercially available A and B, but not as good as Examples 1-3. This is because Comparative Example 1 did not purify its composition, so its active ingredients include some supramolecular whitening components and some single components, resulting in a whitening effect between the two. Examples 1-3 show greater whitening effects than Comparative Examples 2-5 because the conditions for forming a four-component supramolecular combination were not met in Comparative Examples 2-5, resulting in a poorer whitening effect. This further demonstrates that the supramolecular whitening composition obtained in this invention has a significant synergistic enhancement effect, significantly improving the whitening effect.
[0052] Long-lasting whitening effect test: The experiment employed a double-blind method with a testing period of 6 weeks. Participants were required to use the test product on their faces daily, and data was collected from their facial skin four times: at weeks 0, 2, 4, and 6. Thirty participants aged 18-30 years were recruited and divided into 10 groups of 3. Each group used an essence water made from the supramolecular whitening compositions obtained in Examples 1-3, an essence water made from the compositions obtained in Comparative Examples 1-5, and two commercially available skin-lightening and whitening products (product A's main active ingredient was glycyrrhizic acid, and product B's main active ingredient was tea polyphenols). During the volunteers' first visit, informed consent was obtained, data was collected at week 0, and samples were distributed. Each time a volunteer visited, they washed their face with the designated cleanser and sat quietly in the testing environment for approximately 20 minutes. After sitting, skin melanin and hemoglobin testing probes (Mexameter MX18) were used to collect skin melanin content (MI value) data, as shown in Table 3.
[0053] The melanin change rate from the long-lasting whitening effect test results was calculated using the following formula: Melanin change rate (%) = (Melanin content at each time point after product use - Melanin content before product use) / Melanin content before product use × 100.
[0054] Table 3 Results of Melanin Change Rate
[0055] The lower the melanin change rate, the lighter the skin color and the lower the melanin content. Therefore, the melanin change rate can be used as an important indicator to evaluate the whitening and spot-fading effects of cosmetics. As shown in Table 3, the melanin change rate of the essence water prepared from the purified supramolecular whitening compositions obtained in Examples 1-3 was greater than 15% after 6 weeks of use. The test results indicate that the essence water prepared from the supramolecular whitening composition of this invention shows a significant change in skin melanin before and after use, indicating that it can effectively inhibit melanin production, fade spots, and significantly improve skin melanin content after 6 weeks of use, demonstrating a long-lasting whitening effect. The long-lasting whitening effects of Comparative Examples 2-5 were all less than those of commercially available A and B. The long-lasting whitening effect of Comparative Example 1 was close to that of commercially available A and slightly higher than that of commercially available B, but less than that of Examples 1-3. This is because Comparative Example 1 did not undergo a purification step, and the effective ingredients in the resulting composition contained some supramolecular whitening composition and some single components. This resulted in a relatively lower proportion of supramolecular whitening composition in the essence water, which indirectly reflects that the supramolecular whitening composition exhibits a significant synergistic enhancement effect. Compared with single components, the supramolecular whitening composition has a significant improvement in long-lasting whitening.
[0056] Example 5: Accelerated Stability Experiment The supramolecular whitening composition YvesXWhite prepared by this invention contains components that are highly sensitive to light and temperature. Therefore, an accelerated stability test was conducted on the supramolecular whitening composition of this invention to verify that the stability of the supramolecular whitening composition is superior to that of a single substance.
[0057] The supramolecular whitening composition YvesXWhite obtained in Example 1, a saturated aqueous solution of dihydromyricetin, and a saturated aqueous solution of resveratrol were centrifuged at high speed and filtered through a 0.22µm filter membrane. Stability tests were then conducted under two conditions: 45°C in the dark and 25°C under light. The mass content retention rate was determined by HPLC-MS. The test periods were set to 1 day, 3 days, 7 days, 14 days, and 28 days. The test results are shown in Tables 4 and 5.
[0058] Content retention rate = (Real-time content measurement value / Initial content measurement value) × 100% Table 4. Content retention rate under light-protected conditions at 45℃
[0059] Table 5 Content retention rate under 25℃ light conditions
[0060] As shown in Tables 4 and 5, the supramolecular whitening composition system of this invention significantly improves the stability of the active ingredients. Regardless of whether under high temperature and light-protected conditions or under light exposure, the retention rates of dihydromyricetin and resveratrol in this inclusion system are significantly higher than their saturated aqueous solutions. Under light-protected conditions at 45℃, after 28 days, the retention rates of dihydromyricetin and resveratrol in the supramolecular whitening composition are both above 90%, while the retention rates of saturated aqueous solutions of dihydromyricetin and resveratrol both drop below 50%. Under light exposure conditions at 25℃, after 28 days, the retention rates of dihydromyricetin in the supramolecular whitening composition are above 90%, and the retention rates of resveratrol are above 85%, while the saturated aqueous solutions of the two are only 18% and 8%, respectively. The data show that light exposure has a significantly greater impact on the degradation of active ingredients than high temperature and light-protected conditions, especially for resveratrol in saturated aqueous solutions, where the content retention rate after 28 days is only 8%, indicating that it has been almost completely degraded. The supramolecular whitening composition system effectively protects the active ingredients under light conditions, significantly slowing down the degradation rate. Resveratrol is more easily degraded than dihydromyricetin, and the supramolecular system provides more significant protection. Data shows that, under different conditions, the supramolecular whitening composition constructed in this invention can increase the resveratrol content retention rate to more than 10 times that of its saturated aqueous solution.
[0061] The above embodiments are preferred embodiments of the present invention, but the embodiments of the present invention are not limited to the above embodiments. Any changes, modifications, substitutions, combinations, or simplifications made without departing from the spirit and principle of the present invention shall be considered equivalent substitutions and shall be included within the protection scope of the present invention.
Claims
1. A method for preparing a supramolecular whitening composition, YvesXWhite, characterized in that... The process includes the following steps: using vine tea extract, resveratrol, nicotinamide, and arbutin as active ingredients, the alcohol solution of the active ingredients is pre-dissolved by high-pressure homogenization, followed by stirring under water bath conditions to obtain a supramolecular whitening composition mixture solution, and finally purified by hollow fiber ultrafiltration membrane to obtain the supramolecular whitening composition YvesXWhite.
2. The preparation method of the supramolecular whitening composition YvesXWhite according to claim 1, characterized in that... Specifically, the following steps are included: (1) Preparation of vine tea extract: Vine tea powder and water were mixed at a mass ratio of 1:(10~15), and the mixture was stirred in a water bath at 20~25℃ for 20~30 min for decolorization. The filter residue was vacuum dried at 45~50℃. The dried powder was mixed with 95% ethanol at a mass ratio of 1:(20~25), and the mixture was stirred in a water bath at 50~55℃ for 60~90 min for extraction. The extract was then concentrated, water-precipitated, and centrifuged to obtain a precipitate. The precipitate was freeze-dried to obtain vine tea extract. (2) High-pressure homogenization pre-dissolution: The vine tea extract, resveratrol, nicotinamide, arbutin and butylene glycol obtained in step (1) are mixed in a mass ratio of (2~5):(1~3):(3~6):(1~3):(35~85), and then homogenized using a high-pressure homogenizer to obtain a pre-solution; the homogenization is carried out under the following conditions: pressure of 50~80 MPa, number of cycles of 1~3, and cycle temperature of 10~25℃; (3) Preparation of supramolecular whitening composition mixed solution: The pre solution obtained in step (2) is mixed with water at a mass ratio of 1: (1~5), and then stirred in a water bath at 50~55℃ for 20~30min. Then, it is centrifuged at 5000~6000r / min for 3~5min. The supernatant is taken as the supramolecular whitening composition mixed solution. (4) Ultrafiltration purification: The mixed solution of supramolecular whitening composition obtained in step (3) is separated using a 900 Da hollow fiber ultrafiltration membrane, and the retentate is taken to obtain the supramolecular whitening composition YvesXWhite.
3. A supramolecular whitening composition, YvesXWhite, prepared by the preparation method according to claim 1 or 2.
4. The application of the supramolecular whitening composition YvesXWhite according to claim 3 in the preparation of cosmetics.
5. A whitening essence water prepared from the supramolecular whitening composition YvesXWhite as described in claim 3, characterized in that: The whitening essence water is prepared according to the following steps: (1) Mix water, glycerol, disodium ethylenediaminetetraacetate and p-hydroxyacetophenone in a mass ratio of 70:29.4:0.1:0.5 evenly, put them into the main pot, heat to 85~90℃, homogenize for 1~4 min, keep warm for 20~30 min, and then cool down to 45~50℃ to obtain phase A; (2) Weigh the supramolecular whitening composition YvesXWhite described in claim 3, 1,2-hexanediol, and deionized water in a mass ratio of 1:4:5 and mix them evenly to obtain phase B; (3) Add phase B, which accounts for 5% of the mass fraction of phase A, to phase A, stir evenly, filter the material through a 400-mesh filter cloth, and obtain whitening essence water.
