Colloidal Platinum Compositions, Their Preparation and Application
By using a combination of propylene glycol, fatty acids, and organosilanes, the preparation process of colloidal platinum was simplified, resulting in a colloidal platinum composition with high stability and activity, which can be used in cosmetics to enhance anti-aging and wrinkle-reducing effects.
Patent Information
- Application Number
- CN202010951658.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2020-09-11
- Publication Date
- 2025-11-14
- Estimated Expiration
- 2040-09-11
AI Technical Summary
Existing colloidal platinum preparation processes are complex, require sophisticated equipment, and lack sufficient stability and activity, making it difficult to widely apply in the cosmetics field.
Using propylene glycol as a solvent and fatty acids and organosilanes as additives, a colloidal platinum composition with an average particle size of 0.5-5 nm was obtained through a simple preparation method, which included a mixing and heating stirring process of platinum salt, polyvinylpyrrolidone, fatty acids and organosilanes.
The prepared colloidal platinum composition exhibits good stability and high activity, significantly enhancing the anti-aging and wrinkle-reducing effects of cosmetics, forming a transparent and invisible protective film, and elevating the product's luxurious feel.
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Figure CN114159328B_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of cosmetics, specifically to a cosmetic containing colloidal platinum and its preparation and application. Background Technology
[0002] Platinum is a chemical element, commonly known as white gold in its elemental form. Its chemical symbol is Pt, and it is the rarest precious metal in the world. Platinum (Pt) is a naturally occurring white precious metal. Platinum shone brightly in human civilization as early as 700 BC, and throughout its more than 2000-year history of use, it has always been considered one of the noblest metals. In today's society, platinum-containing substances have prominent applications in many fields, such as medicine, food and health, and cosmetics.
[0003] In the pharmaceutical field, platinum-containing active pharmaceutical ingredients (APIs) can be used as anticancer drugs, such as cisplatin, carboplatin, nedaplatin, oxaliplatin, and laboplatin. Cisplatin, in particular, has shown some therapeutic effect on basal cell carcinoma of the skin. In the food and health food sector, patent CN1845807 reports a beverage containing colloidal platinum nanoparticles, wherein the average particle size of the platinum nanoparticles is 1 to 5 nm, and this colloidal platinum exhibits excellent ability to remove reactive oxygen species.
[0004] In the cosmetics industry, due to platinum's preciousness and rarity, colloidal platinum is a raw material used exclusively in top-tier cosmetics. Patent CN106963658 reports a nano-platinum colloid with the ability to scavenge reactive oxygen species in the body. This component is prepared using potassium chloroplatinate, water, polyvinylpyrrolidone, potassium bromide, and L-arginine as raw materials. The preparation process is somewhat complex, involving high-temperature and high-pressure operations. The antioxidant effect of this nano-platinum colloid is superior to coenzyme Q10. Patent CN101569596 reports a nano-platinum colloidal ionized water, obtained by dispersing platinum particles in acidic ionized water, which can be used as a cosmetic raw material for antioxidant effects. The acidic ionized water is obtained through electrolysis using an electric current device. Patent CN103037837 reports an antioxidant composition of platinum colloidal particles and pine bark extract. Cosmetics containing this composition exhibit excellent antioxidant effects and superior sustainability of these effects.
[0005] Organosilicon elastomers (silicone gels) are touted as cosmetic ingredients that can reduce wrinkles in a minute; cosmetics containing this ingredient often offer the effect of filling wrinkles and providing immediate relief. Organosilicon elastomers are prepared through the cross-linking reaction of organosiloxanes, a reaction typically achieved using a platinum-containing catalyst. Patent CN109106616 discloses a method for preparing organosilicon gel for cosmetics, using chloroplatinic acid as a catalyst. Cosmetics using this organosilicon gel as an additive exhibit a uniform texture, smooth application, and high gloss. However, this preparation process requires temperatures above 70°C. US Patent US20070142599 discloses a method for cross-linking organosilicones on the skin to form a transparent, invisible film with waterproof, oil-proof, and tensile strength properties. Forming this film requires both organosilicones and a catalyst; the catalyst used in this patent is a titanium catalyst and a zirconium catalyst.
[0006] In order to expand the scope of colloidal platinum and to overcome the shortcomings of existing technologies, such as complex processes and high equipment requirements in the preparation of colloidal platinum, the primary objective of this invention is to provide a method for preparing colloidal platinum for cosmetics. This method is simple, easy to operate, and produces colloidal platinum with high activity and good long-term stability. Summary of the Invention
[0007] On one hand, this application provides a colloidal platinum composition comprising:
[0008] 0.1-10% by weight of platinum salts,
[0009] 1-20% by weight of fatty acids with 8-30 carbon atoms
[0010] 0.01-5% by weight of organosilanes with 10-60 carbon atoms, and
[0011] A solvent acceptable in the cosmetics industry, wherein the solvent is propylene glycol.
[0012] In a preferred embodiment, the composition further comprises polyvinylpyrrolidone with a K value of 28-34.
[0013] In a preferred embodiment, the platinum salt is selected from: chloroplatinic acid, potassium hexachloroplatinate, sodium chloroplatinate, platinum acetylacetonate, or combinations thereof.
[0014] In a preferred embodiment, the fatty acid is a fatty acid with 12-22 carbon atoms. In a more preferred embodiment, the fatty acid is selected from: palmitic acid, oleic acid, stearic acid, lauric acid, behenic acid, or combinations thereof.
[0015] In a preferred embodiment, the organosilane is an organosilane with 10-20 carbon atoms. In a more preferred embodiment, the organosilane is selected from: trimethoxyoctylsilane, triethoxyoctylsilane, or combinations thereof.
[0016] On the other hand, the present invention provides a method for preparing a colloidal platinum composition, comprising the following steps:
[0017] (a) A first mixture is obtained by mixing a platinum salt, polyvinylpyrrolidone, and propylene glycol.
[0018] (b) Add fatty acids to the first mixture to obtain the second mixture;
[0019] (c) Add organosilane to the second mixture to finally obtain the colloidal platinum composition of the present invention.
[0020] On the other hand, the present invention also relates to the use of colloidal platinum compositions in topical skin agents. In a preferred embodiment, the topical skin agent is used to improve skin elasticity and wrinkle depth. Attached Figure Description
[0021] Figure 1 The average particle size diagram of the colloidal platinum composition prepared in Example 1 is shown.
[0022] Figure 2 The TEM image of the colloidal platinum composition prepared in Example 1 is shown. Detailed Implementation
[0023] This invention is the first to discover that the selection of solvents and additives is crucial in the preparation of colloidal platinum compositions. This invention innovatively discovers that by using specific solvents (e.g., propylene glycol) and additives (e.g., fatty acids and organosilanes), the resulting colloidal platinum compositions exhibit particle sizes in the range of 0.5-5 nm, and the compositions maintain long-term stability.
[0024] To provide a more concise description, some of the quantitative expressions given herein are not modified by the term "approximately". It should be understood that, whether or not the term "approximately" is explicitly used, each quantity given herein is intended to refer to an actual given value, and also to an approximation of such given values that can be reasonably inferred by one of ordinary skill in the art, including approximations of such given values caused by experimental and / or measurement conditions.
[0025] To provide a more concise description, some quantities in this document are described as a range from approximately X to approximately Y. It should be understood that when describing a range, the range is not limited to the upper and lower limits stated, but should include the entire range from approximately X to approximately Y, or any quantities in between.
[0026] Metallic platinum salts
[0027] The present invention aims to provide a colloidal platinum composition for cosmetic use, wherein the composition contains colloidal platinum, a raw material used in top-grade cosmetics, as an active ingredient.
[0028] In embodiments of the present invention, the platinum salt is selected from: chloroplatinic acid (CAS: 16941-12-1, chemical formula: H₂PtCl₆·6H₂O), potassium hexachloroplatinate (CAS: 16921-30-5, chemical formula: K₂PtCl₆), sodium chloroplatinate (CAS: 19583-77-8, chemical formula: Na₂PtCl₆·6H₂O), and platinum acetylacetonate (CAS: 15170-57-7, chemical formula: C₂PtCl₆·6H₂O). 10 H 14 One or a combination thereof (O4Pt). In a preferred embodiment, the platinum salt is chloroplatinic acid.
[0029] In some embodiments of the present invention, the content of platinum salt in the colloidal platinum composition is 0.1-10% by weight. In some embodiments of the present invention, the colloidal platinum composition contains 0.1-8% by weight of platinum salt. In some embodiments of the present invention, the composition contains 0.1-5% by weight of platinum salt. In some embodiments of the present invention, the composition contains 0.1-4% by weight of platinum salt.
[0030] solvent
[0031] Colloidal platinum is a liquid in which negatively charged platinum nanoparticles are suspended. Ethylene glycol is commonly used as a solvent in the preparation of colloidal platinum compositions. For example, the use of ethylene glycol is reported in the literature (Nano Today, 2009, 4, 143-164). However, ethylene glycol has certain toxicity and can damage internal organs such as the kidneys, liver, stomach, and intestines. Furthermore, ethylene glycol is a restricted organic solvent listed in the Appendix II of the 2010 edition of the Chinese Pharmacopoeia.
[0032] Propylene glycol, whose INCI name is PROPYLENE GLYCOL, is used in this application. This application unexpectedly discovers that using propylene glycol as a solvent for preparing colloidal platinum compositions not only retains the advantages of propylene glycol, such as being non-toxic, non-corrosive, biodegradable, and having better safety, but also maintains the stability of the prepared colloidal platinum compositions. Therefore, this application is the first to discover that propylene glycol is the optimal solvent for preparing colloidal platinum compositions.
[0033] In some embodiments of the present invention, the amount of solvent in the colloidal platinum composition is equal to or greater than 50% by weight. In some embodiments of the present invention, the colloidal platinum composition contains 40-95% by weight of solvent. In some embodiments of the present invention, the composition contains 50-90% by weight of solvent. In some embodiments of the present invention, the composition contains 60-90% by weight of solvent. In some embodiments of the present invention, the composition contains 70-90% by weight of solvent.
[0034] additive
[0035] The present invention unexpectedly discovered that fatty acids and organosilanes play a key role in the preparation of colloidal platinum compositions.
[0036] The addition of fatty acids plays a crucial role in controlling the particle size in colloidal platinum.
[0037] Fatty acids are a class of compounds composed of carbon, hydrogen, and oxygen, and are the main components of neutral fats, phospholipids, and glycolipids. Fatty acids can be further classified according to their carbon chain length: short-chain fatty acids, which have fewer than 6 carbon atoms in their carbon chain, also known as volatile fatty acids; medium-chain fatty acids, which have 6-12 carbon atoms in their carbon chain, mainly composed of caprylic acid (C8) and capric acid (C10); and long-chain fatty acids, which have more than 12 carbon atoms in their carbon chain. In a preferred embodiment of the present invention, the additive used is a medium-chain or long-chain fatty acid. In a preferred embodiment, fatty acids with 8-30 carbon atoms are used. In a more preferred embodiment, fatty acids with 10-26 carbon atoms are used. In an even more preferred embodiment, fatty acids with 12-22 carbon atoms are used. In specific embodiments, fatty acids with 12, 14, 16, 18, 20, or 22 carbon atoms are used.
[0038] Fatty acids can be classified into three categories based on the saturation or unsaturation of their hydrocarbon chains: saturated fatty acids, which have no unsaturated bonds on their hydrocarbon chains; monounsaturated fatty acids, which have one unsaturated bond on their hydrocarbon chains; and polyunsaturated fatty acids, which have two or more unsaturated bonds on their hydrocarbon chains. Saturated, monounsaturated, or polyunsaturated fatty acids can be used in the colloidal platinum compositions of this invention.
[0039] In a preferred embodiment, the fatty acid is selected from one or a combination of palmitic acid, oleic acid, stearic acid, lauric acid, and behenic acid. In the most preferred embodiment, the fatty acid is oleic acid.
[0040] In some embodiments of the present invention, the amount of fatty acids in the colloidal platinum composition is 1-20% by weight. In some embodiments of the present invention, the colloidal platinum composition contains 1-15% by weight of fatty acids. In some embodiments of the present invention, the composition contains 2-15% by weight of fatty acids. In some embodiments of the present invention, the composition contains 3-10% by weight of fatty acids. In some embodiments of the present invention, the composition contains 5-10% by weight of fatty acids.
[0041] The addition of organosilanes helps maintain the long-term stability of colloidal platinum activity.
[0042] In some embodiments of the present invention, organosilanes with 10-60 carbon atoms are used. In a preferred embodiment, organosilanes with 10-30 carbon atoms are used. In a more preferred embodiment, organosilanes with 10-26 carbon atoms are used. In an even more preferred embodiment, organosilanes with 10-20 carbon atoms are used. In specific embodiments, organosilanes with 11, 14, 17, or 20 carbon atoms are used.
[0043] In a preferred embodiment, the organosilane is selected from one of trimethoxyoctylsilane, triethoxyoctylsilane, or a combination thereof. In a more preferred embodiment, the organosilane is trimethoxyoctylsilane.
[0044] In some embodiments of the present invention, the amount of organosilane in the colloidal platinum composition is 0.01-5% by weight. In some embodiments of the present invention, the colloidal platinum composition contains 0.01-1% by weight of organosilane. In some embodiments of the present invention, the colloidal platinum composition contains 0.1-2% by weight of organosilane. In some embodiments of the present invention, the composition contains 0.1-1% by weight of organosilane. In some embodiments of the present invention, the composition contains 0.1-0.5% by weight of organosilane.
[0045] Other ingredients
[0046] The colloidal platinum composition of the present invention may also contain other components.
[0047] For example, in one embodiment of the present invention, the composition further comprises polyvinylpyrrolidone (PVP). PVP is a nonionic polymer. PVP is classified into four levels according to its average molecular weight, conventionally represented by the K value. Different K values represent corresponding ranges of average molecular weight of PVP. The K value is actually a characteristic value related to the relative viscosity of PVP aqueous solution, and viscosity is a physical quantity related to the molecular weight of polymers. Therefore, the K value can be used to characterize the average molecular weight of PVP. Generally, the larger the K value, the greater the viscosity and the stronger the adhesion.
[0048] In one specific embodiment, the K value of the polyvinylpyrrolidone contained in the composition is required to be in the range of 28 to 34.
[0049] In some embodiments of the present invention, the amount of polyvinylpyrrolidone in the colloidal platinum composition of this application is 1-30% by weight. In some embodiments of the present invention, the colloidal platinum composition contains 2-30% by weight of polyvinylpyrrolidone. In some embodiments of the present invention, the composition contains 2-20% by weight of polyvinylpyrrolidone. In some embodiments of the present invention, the composition contains 2-15% by weight of polyvinylpyrrolidone. In some embodiments of the present invention, the composition contains 1-10% by weight of polyvinylpyrrolidone.
[0050] Preparation method
[0051] Another object of the present invention is to provide a method for preparing the above-mentioned colloidal platinum composition.
[0052] The colloidal platinum composition of the present invention can be prepared according to the following weight percentages of raw materials: 0.1%-4% platinum salt, 2%-30% polyvinylpyrrolidone, 60%-90% propylene glycol, 5%-15% fatty acid, and 0.01%-1% organosilane.
[0053] Specifically, the method for preparing the colloidal platinum composition of the present invention includes the following steps:
[0054] (a) A first mixture is obtained by mixing a platinum salt, polyvinylpyrrolidone, and propylene glycol.
[0055] (b) Add fatty acids to the first mixture to obtain the second mixture;
[0056] (c) Add organosilane to the second mixture to finally obtain the colloidal platinum composition of the present invention.
[0057] In one specific embodiment, the preparation method of the colloidal platinum composition of the present invention includes the following steps: At room temperature, the platinum salt, polyvinylpyrrolidone, and propylene glycol are mixed uniformly according to the above-mentioned amounts. The mixture is rapidly stirred and heated to 110-200°C, and held at this temperature for 2-8 hours. Fatty acids are added, and the temperature is raised to 120-250°C, with stirring continuing for 30-90 minutes. The temperature is then lowered to 60-80°C, and an organosilane is added, maintaining this temperature while stirring for 30-90 minutes. Finally, the temperature is lowered to room temperature. The colloidal platinum is then discharged, and the preparation is complete. It is stored in a cool, dark place.
[0058] The colloidal platinum composition prepared by this invention has an average particle size of 0.5-5 nm. In a preferred embodiment, the colloidal platinum composition of this invention has an average particle size of 1-5 nm. In a further preferred embodiment, the colloidal platinum composition of this invention has an average particle size of 1-3 nm.
[0059] In the colloidal platinum composition prepared by this invention, more than 75% of the particles have a particle size in the range of 1.75 ± 0.5 nm. In a preferred embodiment, more than 80% of the particles in the composition have a particle size in the range of 1.75 ± 0.5 nm. In a more preferred embodiment, more than 90% of the particles in the composition have a particle size in the range of 1.75 ± 0.5 nm.
[0060] Colloidal platinum's antioxidant effects are comparable to Coenzyme Q10, significantly enhancing the anti-aging and wrinkle-reducing effects of cosmetics. The use of colloidal platinum in cosmetics contributes to a luxurious feel, making it a popular ingredient in high-end products. Applying the technology of this invention allows the efficacy of colloidal platinum to be maximized, forming a transparent, invisible protective film on the skin's surface to lock in the absorption of active ingredients to the greatest extent possible.
[0061] The present invention will be further illustrated below with reference to specific embodiments. It is important to note that these embodiments are for illustrative purposes only and should not be construed as limiting the scope of protection of the invention. Those skilled in the art can make non-essential improvements and adjustments based on the above description of the invention. Test methods in the following embodiments that do not specify specific conditions are generally performed under conventional conditions or as recommended by the manufacturer. Unless otherwise stated, all percentages and parts are by weight.
[0062] Example 1: Preparation of colloidal platinum composition
[0063] At room temperature, 1% chloroplatinic acid, 5% polyvinylpyrrolidone, and 85.5% propylene glycol are mixed thoroughly. The mixture is rapidly stirred and heated to 110°C, held at this temperature for 2 hours. 8% oleic acid is added, the temperature is raised to 120°C, and stirring continues for 30 minutes. The mixture is then cooled to 60°C, and 0.5% trimethoxyoctylsilane is added, maintaining this temperature while stirring for 30 minutes. Finally, the mixture is cooled to room temperature. The colloidal platinum is then discharged and stored in a cool, dark place.
[0064] Comparative Example 1: Preparation of Colloidal Platinum Compositions
[0065] At room temperature, mix 1% chloroplatinic acid, 5% polyvinylpyrrolidone, and 86% propylene glycol thoroughly. Stir rapidly, heat to 110°C, and maintain this temperature for 2 hours. Add 8% oleic acid, raise the temperature to 120°C, and continue stirring for 30 minutes. Finally, cool to room temperature. Discharge the mixture; the colloidal platinum is now ready. Store in a cool, dark place.
[0066] Comparative Example 2: Preparation of Colloidal Platinum Compositions
[0067] At room temperature, 1% chloroplatinic acid, 5% polyvinylpyrrolidone, and 93.5% propylene glycol were mixed thoroughly. The mixture was stirred rapidly and heated to 110°C, maintaining this temperature for 2 hours. The mixture was then cooled to 60°C, and 0.5% trimethoxyoctylsilane was added, while stirring at this temperature for 30 minutes. Finally, the mixture was cooled to room temperature. The colloidal platinum was then discharged and stored in a cool, dark place.
[0068] Comparative Example 3: Preparation of Colloidal Platinum Compositions
[0069] At room temperature, mix 1% chloroplatinic acid, 5% polyvinylpyrrolidone, and 94% propylene glycol thoroughly. Stir rapidly and heat to 110°C, holding for 2 hours. Finally, cool to room temperature. Discharge the mixture; the colloidal platinum is now ready. Store in a cool, dark place.
[0070] Test Example 1: Stability Study of Colloidal Platinum Compositions
[0071] The stability evaluation method is as follows: The colloidal platinum compositions prepared in Example 1 and Comparative Examples 1-3 were placed in a high-temperature (40°C) stable constant temperature chamber and observed for 30 days. The presence of particulate solid precipitation, surface blackening, or layering was observed. If the sample remained normal and unchanged before and after a certain point within the 30-day period, it was considered "ok". The presence of particles indicated "precipitation", localized blackening indicated "blackening", and the appearance of two liquid layers indicated "layering". The results are shown in the table below.
[0072] Table 1: Stability Study of Different Additives
[0073]
[0074] As shown in Table 1, comparing the results of Example 1 and Comparative Example 1, it was found that if no organosilane was added as a stabilizer, the colloidal platinum composition would turn black after 30 days. Comparing the results of Example 1 and Comparative Example 2, it was found that if no fatty acid was added during the preparation of the colloidal platinum composition, solid precipitation and agglomeration would occur after 7 days. Comparing the results of Example 1 and Comparative Example 3, it is shown that the addition of fatty acids and organosilanes plays an important role in the stability of the colloidal platinum composition during the preparation process.
[0075] Example 2: Preparation of colloidal platinum composition
[0076] At room temperature, 0.5% potassium hexachloroplatinate, 3% polyvinylpyrrolidone, and 90.2% propylene glycol were mixed thoroughly. The mixture was stirred rapidly and heated to 110°C, maintaining this temperature for 2 hours. 6% stearic acid was added, and the temperature was raised to 120°C, with stirring continuing for 30 minutes. The mixture was then cooled to 60°C, and 0.3% triethoxyoctylsilane was added, maintaining this temperature while stirring for 30 minutes. Finally, the mixture was cooled to room temperature. The colloidal platinum was then discharged and stored in a cool, dark place.
[0077] Example 3: Preparation of colloidal platinum composition
[0078] At room temperature, 2.5% sodium chloroplatinate, 15% polyvinylpyrrolidone, and 67.5% propylene glycol were mixed thoroughly. The mixture was rapidly stirred and heated to 110°C, maintaining this temperature for 2 hours. 14% lauric acid was added, and the temperature was raised to 120°C, with stirring continuing for 30 minutes. The mixture was then cooled to 60°C, and 1% trimethoxyoctylsilane was added, maintaining this temperature while stirring for 30 minutes. Finally, the mixture was cooled to room temperature. The colloidal platinum was then discharged and stored in a cool, dark place.
[0079] Example 4: Preparation of colloidal platinum composition
[0080] At room temperature, 3% platinum acetylacetonate, 20% polyvinylpyrrolidone, and 66.1% propylene glycol were mixed thoroughly. The mixture was stirred rapidly and heated to 110°C, maintaining this temperature for 2 hours. 10% behenic acid was added, and the temperature was raised to 120°C, with stirring continuing for 30 minutes. The mixture was then cooled to 60°C, and 0.9% triethoxyoctylsilane was added, maintaining this temperature while stirring for 30 minutes. Finally, the mixture was cooled to room temperature. The colloidal platinum was then discharged and stored in a cool, dark place.
[0081] Example 5: Preparation of colloidal platinum composition
[0082] At room temperature, 0.5% chloroplatinic acid, 0.2% platinum acetylacetonate, 10% polyvinylpyrrolidone, and 76.5% propylene glycol were mixed thoroughly. The mixture was rapidly stirred and heated to 110°C, maintaining this temperature for 2 hours. Then, 2% palmitic acid and 10% oleic acid were added, and the temperature was raised to 120°C, with stirring continuing for 30 minutes. The mixture was then cooled to 60°C, and 0.8% trimethoxyoctylsilane was added, maintaining this temperature while stirring for 30 minutes. Finally, the mixture was cooled to room temperature. The colloidal platinum was then discharged and stored in a cool, dark place.
[0083] Example 6: Preparation of colloidal platinum composition
[0084] At room temperature, 0.1% sodium chloroplatinate, 0.1% platinum acetylacetonate, 3% polyvinylpyrrolidone, and 92.7% propylene glycol were mixed thoroughly. The mixture was rapidly stirred and heated to 110°C, maintaining this temperature for 2 hours. 1% stearic acid and 3% oleic acid were added, and the temperature was raised to 120°C, with stirring continuing for 30 minutes. The mixture was then cooled to 60°C, and 0.1% trimethoxyoctylsilane was added, maintaining this temperature while stirring for 30 minutes. Finally, the mixture was cooled to room temperature. The colloidal platinum was then discharged and stored in a cool, dark place.
[0085] Example 7: Preparation of colloidal platinum composition
[0086] At room temperature, mix 2% chloroplatinic acid, 2% sodium chloroplatinate, 30% polyvinylpyrrolidone, and 50% propylene glycol until homogeneous. Stir rapidly and heat to 110°C, maintaining this temperature for 2 hours. Add 15% oleic acid, raise the temperature to 120°C, and continue stirring for 30 minutes. Then cool to 60°C, add 1% trimethoxyoctylsilane, and maintain this temperature while stirring for 30 minutes. Finally, cool to room temperature. Discharge the mixture; the colloidal platinum is now ready. Store in a cool, dark place.
[0087] Test Example 2: Stability Study of Colloidal Platinum Compositions
[0088] The stability evaluation method is as follows: The colloidal platinum compositions prepared in Examples 2-7 were placed in a high-temperature (40℃) stable constant temperature chamber and observed for 30 days. The presence of particulate solid precipitation, surface blackening, or layering was observed. If the sample remained normal and unchanged before and after a certain time within the 30 days, it was considered "ok". The presence of particles indicated "precipitation", localized blackening indicated "blackening", and the appearance of two liquid layers indicated "layering". The results are shown in Table 2 below.
[0089] Table 2: Stability Study of Different Raw Materials
[0090]
[0091] As shown in Table 2, the results of Examples 2 to 5 show that the selected platinum salt in colloidal platinum can be chosen from one of chloroplatinic acid, potassium hexachloroplatinate, sodium chloroplatinate, or platinum acetylacetonate, all of which yield good results. The results of Examples 4, 6, and 7 show that both trimethoxyoctylsilane and triethoxyoctylsilane can yield colloidal platinum compositions with good stability. By comparing all the above results, it is shown that in the process of preparing colloidal platinum, the selection of fatty acids such as palmitic acid, oleic acid, stearic acid, lauric acid, and behenic acid can all achieve satisfactory results.
[0092] The colloidal platinum compositions obtained in the above experiments not only exhibited good stability but also maintained a high level of activity. Since colloidal platinum can promote the cross-linking reaction of siloxanes, a cosmetic containing siloxanes was first used as the first dosage form (dosage form A), and a cosmetic containing the colloidal platinum composition was used as the second dosage form (dosage form B). This study designed a dual-dosage form product, consisting of dosage form A containing siloxanes and dosage form B containing the colloidal platinum composition. When dosage form A is pre-applied to a designated skin area, and then dosage form B is applied to the same area, the colloidal platinum composition promotes the cross-linking of siloxanes on the skin surface, resulting in immediate firming, lifting, and wrinkle-reducing cosmetic effects.
[0093] The following are examples of specific applications of the colloidal platinum compositions of the present invention in topical skin preparations, as well as the formulations and preparation methods of these dosage forms. In the following tables, "-" indicates no additives.
[0094] Table 3: Dosage Form A in Application Examples 1-3
[0095] name Percentage content (%) polydimethylsiloxane 10.00 Hydrogenated polydimethylsiloxane 10.00 Vinyl polydimethylsiloxane 20.00 Dipotassium glycyrrhizate 0.10 Polydimethylsiloxane PEG-10 / 15 cross-linked polymer 4.00 Acrylic (ester) crosspolymers / C10-30 alkanol acrylate crosspolymers 0.50 Tromethamine 0.25 Phenoxyethanol 0.40 Hexanediol 0.50 Deionized water 54.25
[0096] Table 4: Dosage Form B in Application Examples 1-3
[0097]
[0098]
[0099] Application Example 1:
[0100] Preparation of dosage form A
[0101] Within a temperature range of 45℃ to 55℃, polydimethylsiloxane, hydrogenated polydimethylsiloxane, vinyl polydimethylsiloxane, and polydimethylsiloxane PEG-10 / 15 crosslinked polymer are mixed evenly to form the oil phase. 40% deionized water is used to add acrylate / C10-30 alkanol acrylate crosslinked polymer, which is dissolved and swollen completely. After adding glycerol, it is neutralized completely to form the aqueous phase. Dipotassium glycyrrhizate is completely dissolved in the remaining deionized water to form the additive phase. 5% deionized water, phenoxyethanol, and hexanediol are mixed evenly to form the preservative phase. The aqueous phase is slowly added to the oil phase, and the mixture is stirred and homogenized for 5–15 minutes. Then, the additive phase is added, and the mixture is stirred and homogenized for another 5–15 minutes. Finally, the preservative phase is added, and the mixture is stirred and homogenized for 5–15 minutes to form a milky white cream (dosage form A). The product is then cooled, discharged, and stored in a sealed, light-protected container.
[0102] Preparation method of dosage form B:
[0103] Within a temperature range of 45℃ to 60℃, cyclopentamethoxysiloxane, polydimethylsiloxane crosslinked polymer, cetyl PEG / PPG-10 / 1 polydimethylsiloxane, and polydimethylsiloxane PEG-10 / 15 crosslinked polymer were mixed evenly to form the oil phase. Deionized water, glycerol, butanediol, phenoxyethanol, and ethylene glycol were dissolved thoroughly to form the aqueous phase. The colloidal platinum composition of Example 1 was added separately as the additive phase. Within a temperature range of 25℃ to 60℃, the aqueous phase was slowly added to the oil phase, and the mixture was stirred and homogenized for 5 to 15 minutes; then the additive phase was added, and the mixture was stirred and homogenized for another 5 to 15 minutes; an opaque gel was formed, yielding dosage form B product, which was sealed and stored away from light.
[0104] Application Example 2:
[0105] Preparation of dosage form A
[0106] Within a temperature range of 45℃ to 55℃, polydimethylsiloxane, hydrogenated polydimethylsiloxane, vinyl polydimethylsiloxane, and polydimethylsiloxane PEG-10 / 15 crosslinked polymer are mixed evenly to form the oil phase. 40% deionized water is used to add acrylate / C10-30 alkanol acrylate crosslinked polymer, which is dissolved and swollen completely. After adding glycerol, it is neutralized completely to form the aqueous phase. Dipotassium glycyrrhizate is completely dissolved in the remaining deionized water to form the additive phase. 5% deionized water, phenoxyethanol, and hexanediol are mixed evenly to form the preservative phase. The aqueous phase is slowly added to the oil phase, and the mixture is stirred and homogenized for 5–15 minutes. Then, the additive phase is added, and the mixture is stirred and homogenized for another 5–15 minutes. Finally, the preservative phase is added, and the mixture is stirred and homogenized for 5–15 minutes to form a milky white cream (dosage form A). The product is then cooled, discharged, and stored in a sealed, light-protected container.
[0107] Preparation method of dosage form B:
[0108] Within a temperature range of 45℃ to 60℃, cyclopentamethoxysiloxane, polydimethylsiloxane crosslinked polymer, cetyl PEG / PPG-10 / 1 polydimethylsiloxane, and polydimethylsiloxane PEG-10 / 15 crosslinked polymer were mixed evenly to form the oil phase. Deionized water, glycerol, butanediol, phenoxyethanol, and ethylene glycol were dissolved thoroughly to form the aqueous phase. The colloidal platinum composition of Example 2 was added separately as the additive phase. Within a temperature range of 25℃ to 60℃, the aqueous phase was slowly added to the oil phase, and the mixture was stirred and homogenized for 5 to 15 minutes; then the additive phase was added, and the mixture was stirred and homogenized for another 5 to 15 minutes; an opaque gel was formed, yielding dosage form B product, which was sealed and stored away from light.
[0109] Application Example 3:
[0110] Preparation of dosage form A
[0111] Within a temperature range of 45℃ to 55℃, polydimethylsiloxane, hydrogenated polydimethylsiloxane, vinyl polydimethylsiloxane, and polydimethylsiloxane PEG-10 / 15 crosslinked polymer are mixed evenly to form the oil phase. 40% deionized water is used to add acrylate / C10-30 alkanol acrylate crosslinked polymer, which is dissolved and swollen completely. After adding glycerol, it is neutralized completely to form the aqueous phase. Dipotassium glycyrrhizate is completely dissolved in the remaining deionized water to form the additive phase. 5% deionized water, phenoxyethanol, and hexanediol are mixed evenly to form the preservative phase. The aqueous phase is slowly added to the oil phase, and the mixture is stirred and homogenized for 5–15 minutes. Then, the additive phase is added, and the mixture is stirred and homogenized for another 5–15 minutes. Finally, the preservative phase is added, and the mixture is stirred and homogenized for 5–15 minutes to form a milky white cream (dosage form A). The product is then cooled, discharged, and stored in a sealed, light-protected container.
[0112] Preparation method of dosage form B:
[0113] Within a temperature range of 45℃ to 60℃, cyclopentamethoxysiloxane, polydimethylsiloxane crosslinked polymer, cetyl PEG / PPG-10 / 1 polydimethylsiloxane, and polydimethylsiloxane PEG-10 / 15 crosslinked polymer were mixed evenly to form the oil phase. Deionized water, glycerol, butanediol, phenoxyethanol, and ethylene glycol were dissolved thoroughly to form the aqueous phase. The colloidal platinum composition of Example 3 was added separately as the additive phase. Within a temperature range of 25℃ to 60℃, the aqueous phase was slowly added to the oil phase, and the mixture was stirred and homogenized for 5 to 15 minutes; then the additive phase was added, and the mixture was stirred and homogenized for another 5 to 15 minutes; an opaque gel was formed, yielding dosage form B product, which was sealed and stored away from light.
[0114] Test Example 3: Improvement rate of skin elasticity and average wrinkle depth
[0115] Product efficacy was evaluated by comparing improvements in crow's feet and skin elasticity. Wrinkle testing used the Primos Pico instrument, while skin elasticity was tested using a Cutometer instrument. The Primos Pico for skin wrinkles is described below: The Primos rapid 3D skin imaging system is a digital optical 3D image analysis instrument developed based on a digital microscopic stripe projector. The Cutometer for skin elasticity works on the principle of suction and stretching. A negative pressure is created on the surface of the skin being tested, drawing the skin into a specific test probe. The depth to which the skin is drawn into the probe is measured by a non-contact optical testing system. The measurement indicators and meanings of the Primos Pico for skin wrinkles and the Cutometer for skin elasticity are summarized in the table below:
[0116] Table 5
[0117]
[0118]
[0119] The evaluation method for the skin elasticity improvement rate was as follows: Application Example 1, Application Example 2, and Application Example 3 were used respectively. The testing method for human efficacy is as follows:
[0120] 1. Skin test volunteers first cleansed their faces with facial cleanser, and then adapted to the environment of constant temperature and humidity for 15 minutes.
[0121] 2. Record the initial value of the skin elasticity around the eyes using a Cutometer instrument. Record the average wrinkle depth around the eyes using a PrimosPico instrument as an initial value.
[0122] 3. Apply the product around the eyes. First, apply 70 microliters of formulation A to the crow's feet area and wait 3-5 minutes until fully absorbed. Then, apply 100 microliters of formulation B over the area containing formulation A and wait 3-10 minutes.
[0123] 4. After all samples have been applied, let them rest for 15 minutes in a constant temperature and humidity environment before conducting a second test and recording the elasticity value and average wrinkle depth.
[0124] 5. Test complete, end.
[0125] The calibration improvement rate reflects the percentage of skin changes; the higher the value, the greater the improvement.
[0126]
[0127] Table 6
[0128] serial number Application examples R2 R7 Average wrinkle depth improvement rate 1 Application Example 1 18.88% 16.17% 10.34% 2 Application Example 2 12.05% 11.81% 8.62% 3 Application Example 3 17.62% 15.87% 9.59%
[0129] As shown in the table above, when dosage form A and dosage form B containing different colloidal platinum were used in combination, both skin elasticity and average wrinkle depth were significantly improved after 15 minutes. Application Examples 1, 2, and 3 all demonstrated good efficacy, with the highest improvement rate in average wrinkle depth reaching 10.34% after 15 minutes (Application Example 1), and skin elasticity increasing by approximately 12-18%.
[0130] Application Example 4:
[0131] Preparation of dosage form A
[0132] Within a temperature range of 45℃ to 55℃, 10% polydimethylsiloxane, 10% hydrogenated polydimethylsiloxane, 20% vinyl polydimethylsiloxane, and 4% polydimethylsiloxane PEG-10 / 15 crosslinked polymer are mixed evenly to form the oil phase. 40% deionized water is added to an acrylate / C10-30 alkanol acrylate crosslinked polymer, dissolved and swollen completely, then neutralized completely with tromethamine to form the aqueous phase. 0.2% bismuth oxychloride and 1% CI 77891 are thoroughly dispersed in 6% glycerol to form the additive phase. The remaining deionized water, phenoxyethanol, and hexanediol are mixed evenly to form the preservative phase. The aqueous phase is slowly added to the oil phase, stirred and homogenized for 5–15 minutes; then the additive phase is added, and stirring and homogenization are continued for 5–15 minutes; finally, the preservative phase is added, stirred and homogenized for 5–15 minutes, forming a milky white cream (dosage form A). The product is then cooled, discharged, and stored in a sealed, light-protected container.
[0133] Preparation method of dosage form B:
[0134] Within a temperature range of 45℃ to 60℃, cyclopentamethoxysiloxane, polydimethylsiloxane crosslinked polymer, cetyl PEG / PPG-10 / 1 polydimethylsiloxane, and polydimethylsiloxane PEG-10 / 15 crosslinked polymer were mixed evenly to form the oil phase. Deionized water, glycerol, butanediol, phenoxyethanol, and ethylene glycol were dissolved thoroughly to form the aqueous phase. The colloidal platinum composition of Example 3 was added separately as the additive phase. Within a temperature range of 25℃ to 60℃, the aqueous phase was slowly added to the oil phase, and the mixture was stirred and homogenized for 5 to 15 minutes; then the additive phase was added, and the mixture was stirred and homogenized for another 5 to 15 minutes; an opaque gel was formed, yielding dosage form B product, which was sealed and stored away from light.
[0135] Application Example 5:
[0136] Preparation of dosage form A
[0137] Within a temperature range of 45℃ to 55℃, 10% polydimethylsiloxane, 10% hydrogenated polydimethylsiloxane, 20% vinyl polydimethylsiloxane, and 4% polydimethylsiloxane PEG-10 / 15 crosslinked polymer were mixed evenly to form the oil phase. 40% deionized water was taken, and acrylate / C10-30 alkanol acrylate crosslinked polymer was added, dissolved and swollen completely, then neutralized completely with tromethamine to form the aqueous phase. 0.12% silicon-treated iron oxide yellow SA-Y-8 and 0.07% silicon-treated iron oxide red SAS-RPS-10 were thoroughly dispersed evenly with 6% glycerol to form the additive phase. The remaining deionized water, phenoxyethanol, and hexanediol were mixed evenly to form the preservative phase. Slowly add the aqueous phase to the oil phase, stir and homogenize for 5-15 minutes; then add the additive phase, continue stirring and homogenizing for 5-15 minutes; finally add the preservative phase, stir and homogenize for 5-15 minutes to form a milky white cream (dosage form A), cool down and discharge, seal and store away from light.
[0138] Preparation method of dosage form B:
[0139] Within a temperature range of 45℃ to 60℃, cyclopentamethoxysiloxane, polydimethylsiloxane crosslinked polymer, cetyl PEG / PPG-10 / 1 polydimethylsiloxane, and polydimethylsiloxane PEG-10 / 15 crosslinked polymer were mixed evenly to form the oil phase. Deionized water, glycerol, butanediol, phenoxyethanol, and ethylene glycol were dissolved thoroughly to form the aqueous phase. The colloidal platinum composition of Example 3 was added separately as the additive phase. Within a temperature range of 25℃ to 60℃, the aqueous phase was slowly added to the oil phase, and the mixture was stirred and homogenized for 5 to 15 minutes; then the additive phase was added, and the mixture was stirred and homogenized for another 5 to 15 minutes; an opaque gel was formed, yielding dosage form B product, which was sealed and stored away from light.
Claims
1. A colloidal platinum composition comprising: 0.1-10% by weight of a platinum metal salt or chloroplatinic acid, wherein the platinum metal salt is selected from: potassium hexachloroplatinate, sodium chloroplatinate, platinum acetylacetonate, or combinations thereof. 1-20% by weight of fatty acids with 8-30 carbon atoms. 0.01-5% by weight of organosilanes with 10-60 carbon atoms, and A solvent acceptable in the cosmetics industry, wherein the solvent is propylene glycol.
2. The colloidal platinum composition according to claim 1, characterized in that, The composition also contains polyvinylpyrrolidone with a K value of 28-34.
3. The colloidal platinum composition according to claim 1 or 2, characterized in that, The fatty acid is a fatty acid with 12-22 carbon atoms.
4. The colloidal platinum composition according to claim 3, characterized in that, The fatty acid is selected from: palmitic acid, oleic acid, stearic acid, lauric acid, behenic acid, or a combination thereof.
5. The colloidal platinum composition according to claim 1 or 2, characterized in that, The organosilane is an organosilane with 10-20 carbon atoms.
6. The colloidal platinum composition according to claim 5, characterized in that, The organosilane is selected from: trimethoxyoctylsilane, triethoxyoctylsilane, or combinations thereof.
7. The method for preparing the colloidal platinum composition according to claim 2, comprising the following steps: (a) Mixing a platinum salt or chloroplatinic acid, polyvinylpyrrolidone, and propylene glycol yields a first mixture; (b) Add fatty acids to the first mixture to obtain the second mixture; (c) Add organosilane to the second mixture to finally obtain a colloidal platinum composition.
Citation Information
Patent Citations
Cosmetic compositions having in-situ silicone condensation cross-linking
US20070142599A1
Nano-platinum contained cosmetic composition
CN106963658A