Wrinkle-removing and anti-aging essence containing collagen and elastin and preparation method thereof
By designing a two-component system and utilizing the isotonic buffer of component A and the stepwise preparation process of component B, the stability and skin feel issues of active ingredients in anti-wrinkle and anti-aging skincare products caused by differences in properties are solved, achieving a synergistic effect of high stability and excellent skin feel of active ingredients.
Patent Information
- Application Number
- CN202511485177.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-10-17
- Publication Date
- 2025-12-16
AI Technical Summary
Existing anti-wrinkle and anti-aging skincare products contain active ingredients such as collagen and elastin, which have significant differences in physicochemical properties. These ingredients are prone to phase separation, precipitation, or inactivation due to pH value, electrolytes, or high-temperature processes. Furthermore, chemical preservatives may cause skin sensitivity, making it difficult to achieve a balance between ingredient activity, stability, and skin feel.
A two-component system is adopted. Component A is an isotonic buffer solution containing collagen and elastin, and the pH and ionic strength are regulated by phosphate buffer and inorganic salt. Component B is a complex carrier system prepared in steps, which uses thickeners, solubilizers and antioxidants to protect the active ingredients, and controls the temperature and feeding sequence to ensure stability and activity.
It achieves high stability and safety of collagen and elastin, while providing an excellent skin feel, ensuring synergistic effects of active ingredients and overall product stability.
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Figure BDA0005640717990000181
Abstract
Description
TECHNICAL FIELD
[0001] The present application relates to the field of cosmetics, in particular to a wrinkle-removing and anti-aging essence containing collagen and elastin and a preparation method. BACKGROUND
[0002] In order to achieve significant effects, wrinkle-removing and anti-aging skin care products often need to compound multiple active ingredients, such as collagen and elastin for supplementing structural proteins, and various skin conditioners with antioxidant and lightening functions. However, these ingredients have significant differences in physical and chemical properties, and simple coexistence in a single system can easily lead to phase separation, precipitation or inactivation due to pH value, electrolytes or high-temperature processes, especially heat-sensitive ingredients such as alpha-arbutin are more likely to degrade during preparation, which seriously affects the stability and efficacy of the final product. On the other hand, systems rich in nutrients have strict requirements for microbial stability, and excessive reliance on chemical preservatives can also cause skin sensitivity problems. In addition, how to ensure the activity of ingredients while considering the light and non-sticky skin feel of the product, and making its pH value compatible with the physiological environment of the skin to reduce irritation, has also become a key to improving user experience. Therefore, developing a comprehensive solution that can synergistically enhance the stability and safety of each active ingredient and provide excellent skin feel has become a technical bottleneck that needs to be broken through in the field. SUMMARY
[0003] In order to make up for the above shortcomings, the present application provides a wrinkle-removing and anti-aging essence containing collagen and elastin and a preparation method, which obtains an essence that can synergistically enhance the stability and safety of each active ingredient and provide excellent skin feel by optimizing the component ratio and simultaneously adjusting the preparation process.
[0004] In order to achieve the above purpose, the present application adopts the following technical solutions:
[0005] A wrinkle-removing and anti-aging essence containing collagen and elastin, comprising component A and component B in a mass ratio of 0.3-3:1;
[0006] wherein, the component A consists of the following components by mass fraction:
[0007] water 90-98 parts,
[0008] a combination of collagen and elastin 2-5 parts,
[0009] moisturizing agent 1-3 parts,
[0010] inorganic salt 0.5-1.5 parts,
[0011] pH buffer 0.1-0.2 parts;
[0012] wherein, the component B consists of the following components by total mass 100 parts:
[0013] 15-25 parts moisturizer
[0014] 5-10 parts of solubilizer
[0015] 5-15 parts skin conditioning agent
[0016] Antioxidant 0.5-2 parts,
[0017] Thickener 0.3-1 part,
[0018] Chelating agent 0.1-0.5 parts,
[0019] pH adjuster 0.5-1.5 parts,
[0020] The remainder is water.
[0021] In this solution, component A is essentially an isotonic buffer solution tailored for proteins. The pH buffer is crucial, responsible for stabilizing the system within the neutral range and preventing collagen and elastin from undergoing charge neutralization, flocculation, and precipitation due to pH fluctuations to their isoelectric points. Inorganic salts, at specific concentrations, not only provide suitable osmotic pressure but also help maintain the solubility of proteins through their ionic atmosphere. However, if these concentrations exceed the appropriate range, high ionic strength can trigger a "salting-out" effect, leading to protein inactivation. The humectant here serves a dual purpose: in addition to basic moisturizing, it stabilizes protein conformation and acts as an adjunct preservative.
[0022] Moving to component B, the system is more complex, making process control particularly critical. Thickeners must be dispersed and dissolved at room temperature to form a uniform three-dimensional network structure; high-temperature treatment can lead to uneven hydration or degradation, thus losing their ability to achieve the desired viscosity of the product. Subsequently, during the heating stage, the solubilizer's role is to insert its lipophilic end into the oil phase component, forming micelles at the interface, thereby achieving stable dispersion of the heat-resistant skin conditioning agent in the aqueous phase. Antioxidants, at this time, protect these lipid components from thermal oxidation. A key cooling step in the process is designed for heat-sensitive skin conditioning agents; excessively high temperatures can damage their molecular structure, leading to inactivation. Finally, pH adjusters precisely adjust the pH of component B to a slightly acidic level, which not only matches the physiological pH of the skin to reduce irritation but also creates conditions for many active ingredients to exert their optimal activity. Chelating agents, by complexing with metal ions, interrupt the pathways of metal ion-catalyzed oxidation reactions and the promotion of microbial growth, improving the system's chemical stability and preservative efficacy.
[0023] Preferably, the humectant in component A is 1,2-pentanediol; the inorganic salt is sodium chloride; and the pH buffer is a mixture of disodium hydrogen phosphate and sodium dihydrogen phosphate.
[0024] Preferably, the skin conditioning agents in component B include heat-resistant skin conditioning agents and heat-sensitive skin conditioning agents; the heat-resistant skin conditioning agents include squalane, tocopherol, bisabolol, and tetrahydropiperine; the heat-sensitive skin conditioning agents include α-arbutin, glycyrrhizin, and ginseng root extract.
[0025] Preferably, the mass ratio of the heat-resistant skin conditioner to the heat-sensitive skin conditioner is 0.5-2:1.
[0026] If the proportion of heat-resistant skin conditioning agent is too low (<0.5:1), the oil phase core formed at high temperatures is too weak, failing to provide sufficient interaction interfaces for the solubilizer to form a stable micelle system. This not only leads to a decrease in the stability of the entire oil phase dispersion, but also makes it difficult for this fragile system to provide effective buffering protection when heat-sensitive ingredients are subsequently added, potentially exacerbating the risk of molecular degradation or precipitation of heat-sensitive ingredients (such as α-arbutin), ultimately affecting the product's advanced efficacy. Conversely, if the proportion of heat-resistant skin conditioning agent is too high (>2:1), new challenges arise. Excessive lipid components significantly increase the burden on the solubilizer, potentially exceeding its solubilization capacity critical point, leading to oil phase separation, turbidity, or oil seepage in the paste. Simultaneously, excessive oil components interfere with the rheological network constructed by the thickener, potentially making the product texture greasy and viscous, affecting skin feel. In terms of processing, a high oil phase proportion also means requiring higher emulsification energy or longer homogenization time, increasing production difficulty and instability risks.
[0027] Preferably, the humectant in component B is butylene glycol and glycerin; the solubilizer is PEG-40 hydrogenated castor oil and PEG-60 hydrogenated castor oil; and the antioxidant is tocopherol.
[0028] Preferably, the thickener in component B is hydroxyethyl cellulose and carbomer; the chelating agent is disodium EDTA; and the pH adjuster is citric acid.
[0029] This solution also proposes a method for preparing the above-mentioned anti-wrinkle and anti-aging essence containing collagen and elastin, including the following steps:
[0030] S1. Preparation of component A: Heat the water in component A to 40-60℃, add inorganic salts and pH buffer and stir to dissolve. After cooling to 30-40℃, add the combination of collagen and elastin and moisturizer, homogenize and adjust the pH value to 6.5-7.5 to obtain component A;
[0031] S2. Preparation of component B:
[0032] S21. Preparation of component B1: Mix water accounting for 30%-60% of the total water volume of component B with a thickener, stir at room temperature until completely dissolved, and obtain component B1;
[0033] S22. Preparation of component B2: Heat the remaining water of component B to 50-70℃, add moisturizer, solubilizer, antioxidant, chelating agent and heat-resistant skin conditioning agent in sequence, and stir to dissolve; after cooling to 40-50℃, add heat-sensitive skin conditioning agent and stir to dissolve; finally add pH adjuster to adjust the pH of the system to 5.0-6.0 to obtain component B2;
[0034] S23. Sterilized component B1 and filtered sterilized component B2 are mixed under stirring conditions, wherein component B2 is added to component B1 and stirred evenly to obtain component B;
[0035] S3. Mixing: Mix component A and component B in proportion and at room temperature until homogeneous.
[0036] The core of the two-component system constructed in this invention lies in creating optimal molecular-scale ecological environments for different active ingredients through physical separation and process synergy, thereby achieving synergistic effects and avoiding compatibility risks. During the preparation process, the primary key is to strictly control the temperature and the order of addition at each stage, as this directly affects the stability of protein conformation and the preservation of the activity of heat-sensitive components. When preparing component A, inorganic salts and a pH buffer are first dissolved in water at 40-60℃ to establish a basic medium with stable ionic strength and pH. Then, the temperature is lowered to 30-40℃ before adding a collagen and elastin composition and a humectant. This operation effectively prevents protein denaturation and aggregation due to high temperatures. The inorganic salts provide the necessary osmotic pressure environment at a precise concentration, but excessive amounts can trigger salting-out, leading to protein precipitation. The pH buffer maintains the system within a neutral and mild range; deviations from this range may trigger protein isoelectric point flocculation.
[0037] The preparation of component B begins with the preparation of a thickener aqueous solution (B1) at room temperature to prevent viscosity degradation or agglomeration of the polymer at high temperatures, ensuring a uniform and stable final texture. The preparation of B2 strictly follows a thermodynamic gradient, first dissolving heat-resistant components (such as solubilizers, antioxidants, and heat-resistant conditioners) at 50-70°C. This temperature promotes the full encapsulation of the oil phase components by the solubilizer. Then, the temperature is lowered to the critical window of 40-50°C before adding the heat-sensitive conditioner, thereby minimizing its thermal decomposition and deactivation. The synergistic effect of the thickener and solubilizer is to construct a suitable rheological system; excessive amounts result in a sticky feel, while insufficient amounts may lead to system instability or even stratification. Finally, by separately sterilizing B1 with ultraviolet light and B2 with membrane filtration, and then adding B2 to B1 under stirring, microbial contamination and shear force damage to the constructed colloidal network structure are avoided.
[0038] Preferably, in step S23, component B1 is sterilized by ultraviolet light, and component B2 is sterilized by filtration through a 0.22-micron microporous membrane.
[0039] Preferably, step S3 is followed by a settling and defoaming process and a filtration process.
[0040] Compared to existing technologies, the advantages of this solution are:
[0041] 1. This formulation employs a two-component system. Component A, an isotonic buffer microenvironment specifically designed for proteins, provides optimal charge stability and solubility for collagen and elastin through precise regulation of the phosphate buffer system and inorganic salts, preventing protein inactivation due to pH fluctuations or inappropriate ionic strength. Component B constructs a complex and sophisticated carrier system, in which solubilizers, thickeners, antioxidants, and chelating agents work together to protect, stabilize, and deliver the heat-resistant and heat-sensitive skin conditioning agents. By controlling the ratio of heat-resistant to heat-sensitive conditioning agents within the optimal range of 0.5-2:1, a sufficient oil phase is ensured to stabilize the micelle system while avoiding the burden of excessive lipids, achieving an optimal balance between efficacy and stability.
[0042] 2. From the stepwise preparation of component B (B1 and B2), temperature control (room temperature, 50-70℃, 40-50℃) to stepwise sterilization (ultraviolet light and filtration sterilization), each process step is closely aligned with the physicochemical properties of its corresponding component, maximizing the protection of the activity of various ingredients during processing. Components A and B are only mixed at room temperature in the final stage of the process. This crucial step ensures that their pre-optimized and stable systems remain independent and intact before combination, ultimately endowing the product with excellent overall stability, efficacy, and safety. Detailed Implementation
[0043] The technical solutions of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of the present invention.
[0044] Example 1
[0045] An anti-wrinkle and anti-aging serum containing collagen and elastin, comprising component A and component B in a mass ratio of 1:1;
[0046] Component A, by mass, comprises the following components:
[0047] 94 parts water
[0048] A composition of collagen and elastin, 3.5 parts.
[0049] 2 parts of 1,2-pentanediol
[0050] 1 part sodium chloride,
[0051] 0.15 parts of pH buffer, which is a mixture of disodium hydrogen phosphate and sodium dihydrogen phosphate in a mass ratio of 1:2;
[0052] Component B, based on a total mass of 100 parts, consists of the following components:
[0053] The mass ratio of butanediol and glycerol is 1:2, 20 parts each.
[0054] 7.5 parts by mass of PEG-40 hydrogenated castor oil and PEG-60 hydrogenated castor oil in a ratio of 1:1.5.
[0055] Five parts of a heat-resistant skin conditioning agent, comprising 2 parts squalane, 1.5 parts tocopherol, 1 part bisabolol, and 0.5 parts tetrahydropiperine.
[0056] Five parts of a heat-sensitive skin conditioning agent, including two parts of α-arbutin, two parts of glycyrrhizin, and one part of ginseng root extract.
[0057] Tocopherol 1.25 parts,
[0058] Hydroxyethyl cellulose and carbomer in a mass ratio of 1:1.5, 0.65 parts,
[0059] 0.3 parts of disodium EDTA
[0060] 1 part citric acid
[0061] The remainder is water;
[0062] The preparation method of the above-mentioned anti-wrinkle and anti-aging serum containing collagen and elastin includes the following steps:
[0063] S1. Preparation of component A: 94 parts of water were heated to 50°C, 1 part of sodium chloride and 0.15 parts of pH buffer were added and stirred to dissolve. The pH buffer was a mixture of disodium hydrogen phosphate and sodium dihydrogen phosphate in a mass ratio of 1:2. After cooling to 35°C, 3.5 parts of a combination of collagen and elastin and 2 parts of 1,2-pentanediol were added. The mixture was homogenized at 3000 r / min for 5 minutes and the pH was adjusted to 7.0 to obtain component A.
[0064] S2. Preparation of component B:
[0065] S21. Preparation of component B1: Mix 45% of the total water content of component B with 0.65 parts of hydroxyethyl cellulose and carbomer in a mass ratio of 1:1.5, stir at room temperature for 30 minutes until completely dissolved to obtain component B1;
[0066] S22. Preparation of Component B2: Heat the remaining water in Component B to 60°C, then add 20 parts by mass ratio of 1:2 butylene glycol and glycerin, 7.5 parts by mass ratio of 1:1.5 PEG-40 hydrogenated castor oil and PEG-60 hydrogenated castor oil, 1.25 parts by mass ratio of tocopherol, 0.3 parts by mass ratio of disodium EDTA, and 5 parts by mass ratio of heat-resistant skin conditioning agent, wherein the heat-resistant skin conditioning agent comprises 2 parts by mass ratio of squalane, 1.5 parts by mass ratio of tocopherol, 1 part by mass ratio of bisabolol, and 0.5 parts by mass ratio of tetrahydropiperine, and stir to dissolve; after cooling to 45°C, add 5 parts by mass ratio of heat-sensitive skin conditioning agent, wherein the heat-sensitive skin conditioning agent comprises 2 parts by mass ratio of α-arbutin, 2 parts by mass ratio of glycyrrhizin, and 1 part by mass ratio of ginseng root extract, and stir to dissolve; finally, add 1 part by mass ratio of citric acid to adjust the pH of the system to 5.5 to obtain Component B2;
[0067] S23. Mix component B1, which has been sterilized by ultraviolet light for 30 minutes, and component B2, which has been sterilized by filtration through a 0.22-micron microporous membrane, under stirring conditions at a stirring speed of 200 r / min. Component B2 is slowly added to component B1, and stirring is continued for 15 minutes until homogeneous to obtain component B.
[0068] S3. Mixing: Mix component A and component B at a mass ratio of 1:1 at room temperature until homogeneous, let stand to defoam for 2 hours, and filter with a 5-micron filter membrane to obtain an anti-wrinkle and anti-aging essence containing collagen and elastin.
[0069] Example 2
[0070] An anti-wrinkle and anti-aging serum containing collagen and elastin, comprising component A and component B in a mass ratio of 0.3:1;
[0071] Component A, by mass, comprises the following components:
[0072] 90 parts water
[0073] Two parts of a composition of collagen and elastin.
[0074] 1 part of 1,2-pentanediol,
[0075] 0.5 parts sodium chloride,
[0076] 0.1 parts of pH buffer, which is a mixture of disodium hydrogen phosphate and sodium dihydrogen phosphate in a mass ratio of 1:1;
[0077] Component B, based on a total mass of 100 parts, consists of the following components:
[0078] The mass ratio of butanediol and glycerol is 1:1, 15 parts each.
[0079] Five parts by mass of PEG-40 hydrogenated castor oil and PEG-60 hydrogenated castor oil in a 1:1 ratio.
[0080] A heat-resistant skin conditioning agent of 1.67 parts, comprising 0.7 parts squalane, 0.5 parts tocopherol, 0.3 parts bisabolol, and 0.17 parts tetrahydropiperine.
[0081] The thermal skin conditioning agent contains 3.33 parts, including 1.5 parts α-arbutin, 1.2 parts glycyrrhizin, and 0.63 parts ginseng root extract.
[0082] Tocopherol 0.5 parts,
[0083] Hydroxyethyl cellulose and carbomer in a 1:1 mass ratio of 0.3 parts.
[0084] 0.1 parts of disodium EDTA
[0085] Citric acid 0.5 parts,
[0086] The remainder is water;
[0087] The preparation method of the above-mentioned anti-wrinkle and anti-aging serum containing collagen and elastin includes the following steps:
[0088] S1. Preparation of component A: Heat 90 parts of water to 40°C, add 0.5 parts of sodium chloride and 0.1 parts of pH buffer and stir to dissolve. The pH buffer is a mixture of disodium hydrogen phosphate and sodium dihydrogen phosphate in a mass ratio of 1:1. After cooling to 30°C, add 2 parts of a collagen and elastin composition and 1 part of 1,2-pentanediol, homogenize at 2500 r / min for 3 minutes and adjust the pH value to 6.5 to obtain component A.
[0089] S2. Preparation of component B:
[0090] S21. Preparation of component B1: Mix 30% of the total water content of component B with 0.3 parts of hydroxyethyl cellulose and carbomer in a mass ratio of 1:1, stir at room temperature for 20 minutes until completely dissolved to obtain component B1;
[0091] S22. Preparation of Component B2: Heat the remaining water in Component B to 50°C, then add 15 parts by mass ratio of 1:1 butylene glycol and glycerin, 5 parts by mass ratio of 1:1 PEG-40 hydrogenated castor oil and PEG-60 hydrogenated castor oil, 0.5 parts by mass ratio of 0.1 ...
[0092] S23. Mix component B1, which has been sterilized by ultraviolet light for 20 minutes, and component B2, which has been sterilized by filtration through a 0.22-micron microporous membrane, under stirring conditions at a stirring speed of 150 r / min. Component B2 is slowly added to component B1, and stirring is continued for 10 minutes until homogeneous to obtain component B.
[0093] S3. Mixing: Mix component A and component B at a mass ratio of 0.3:1 at room temperature until homogeneous, let stand to defoam for 1 hour, and filter with a 5-micron filter membrane to obtain an anti-wrinkle and anti-aging essence containing collagen and elastin.
[0094] Example 3
[0095] An anti-wrinkle and anti-aging serum containing collagen and elastin, comprising component A and component B in a mass ratio of 3:1;
[0096] Component A, by mass, comprises the following components:
[0097] 98 parts water
[0098] Five parts of a composition of collagen and elastin.
[0099] 3 parts of 1,2-pentanediol
[0100] 1.5 parts sodium chloride,
[0101] 0.2 parts of pH buffer, which is a mixture of disodium hydrogen phosphate and sodium dihydrogen phosphate in a mass ratio of 1:3;
[0102] Component B, based on a total mass of 100 parts, consists of the following components:
[0103] The mass ratio of butanediol to glycerol is 1:3, which is 25 parts.
[0104] Ten parts by mass of PEG-40 hydrogenated castor oil and PEG-60 hydrogenated castor oil in a ratio of 1:2
[0105] Ten parts of a heat-resistant skin conditioning agent, including 4 parts squalane, 3 parts tocopherol, 2 parts bisabolol, and 1 part tetrahydropiperine.
[0106] Five parts of a heat-sensitive skin conditioning agent, including 2.5 parts α-arbutin, 1.5 parts glycyrrhizin, and 1 part ginseng root extract.
[0107] Two portions of tocopherol.
[0108] One part by weight of hydroxyethyl cellulose and carbomer in a ratio of 1:2
[0109] 0.5 parts of disodium EDTA
[0110] Citric acid 1.5 parts,
[0111] The remainder is water;
[0112] The preparation method of the above-mentioned anti-wrinkle and anti-aging serum containing collagen and elastin includes the following steps:
[0113] S1. Preparation of component A: 98 parts of water were heated to 60°C, and 1.5 parts of sodium chloride and 0.2 parts of pH buffer were added and stirred to dissolve. The pH buffer was a mixture of disodium hydrogen phosphate and sodium dihydrogen phosphate in a mass ratio of 1:3. After cooling to 40°C, 5 parts of a collagen and elastin composition and 3 parts of 1,2-pentanediol were added. The mixture was homogenized at 3500 r / min for 8 minutes and the pH was adjusted to 7.5 to obtain component A.
[0114] S2. Preparation of component B:
[0115] S21. Preparation of component B1: Mix 60% of the total water content of component B with 1 part of hydroxyethyl cellulose and carbomer in a mass ratio of 1:2, stir at room temperature for 40 minutes until completely dissolved to obtain component B1;
[0116] S22. Preparation of Component B2: Heat the remaining water in Component B to 70°C, then add 25 parts of butylene glycol and glycerin in a 1:3 mass ratio, 10 parts of PEG-40 hydrogenated castor oil and PEG-60 hydrogenated castor oil in a 1:2 mass ratio, 2 parts of tocopherol, 0.5 parts of disodium EDTA, and 10 parts of a heat-resistant skin conditioning agent, comprising 4 parts of squalane, 3 parts of tocopherol, 2 parts of bisabolol, and 1 part of tetrahydropiperine, and stir to dissolve. After cooling to 50°C, add 5 parts of a heat-sensitive skin conditioning agent, comprising 2.5 parts of α-arbutin, 1.5 parts of glycyrrhizin, and 1 part of ginseng root extract, and stir to dissolve. Finally, add 1.5 parts of citric acid to adjust the pH of the system to 6.0 to obtain Component B2.
[0117] S23. Mix component B1, which has been sterilized by ultraviolet light for 40 minutes, and component B2, which has been sterilized by filtration through a 0.22-micron microporous membrane, under stirring conditions at a stirring speed of 250 r / min. Component B2 is slowly added to component B1, and stirring is continued for 20 minutes until homogeneous to obtain component B.
[0118] S3. Mixing: Mix component A and component B at a mass ratio of 3:1 at room temperature until homogeneous, let stand to defoam for 3 hours, and filter with a 5-micron filter membrane to obtain an anti-wrinkle and anti-aging essence containing collagen and elastin.
[0119] Comparative Example 1
[0120] The only difference from Example 1 is that component B is absent.
[0121] Comparative Example 2
[0122] The only difference from Example 1 is that component A is absent.
[0123] Comparative Example 3
[0124] The only difference from Example 1 is that the mass ratio of component A to component B is 5:1.
[0125] Comparative Example 4
[0126] The only difference from Example 1 is that the heat-resistant skin conditioning agent, comprising 12 parts, includes 5 parts squalane, 4 parts tocopherol, 2 parts bisabolol, and 1 part tetrahydropiperine.
[0127] Three parts of a heat-sensitive skin conditioning agent, including 1.5 parts of α-arbutin, 1 part of glycyrrhizin, and 0.5 parts of ginseng root extract.
[0128] Comparative Example 5
[0129] The only difference from Example 1 is that the sodium chloride content is increased to 3 parts and the solubilizer content is increased to 15 parts.
[0130] Comparative Example 6
[0131] The only difference from Example 1 is that the composition of component A and component B is stirred together to obtain the product.
[0132] Comparative Example 7
[0133] The only difference from Example 1 is that, when preparing component A, the components are directly mixed.
[0134] Comparative Example 8
[0135] The only difference from Example 1 is that, when preparing component B, the components are directly mixed.
[0136] Detection method:
[0137] 1. Appearance and color inspection: Take an appropriate amount of essence sample (component A, component B and finished product) and put them into clean colorimetric tubes, filling the tubes to 2 / 3 of their volume; under natural light, observe the clarity of the sample, whether there is layering, turbidity, precipitation, foreign matter, etc., and record the appearance characteristics; compare with the standard colorimetric card, describe the color of the sample, and judge whether the color is uniform.
[0138] Judgment criteria: The sample should be clear and transparent (or conform to the appearance of the formula design), without layering, turbidity, sediment, foreign matter, and uniform color.
[0139] 2. Viscosity testing: Select an appropriate rotor and speed according to the expected viscosity of the sample, and preheat the viscometer to 25℃±0.5℃;
[0140] Place the serum sample (component A, component B, and finished product) in a constant temperature water bath at 25℃±0.5℃ for equilibration for 30 minutes to ensure the sample is uniform and free of air bubbles. Slowly immerse the rotor into the sample until it reaches the rotor mark line, start the viscometer, and record the viscosity value after the reading stabilizes. Perform three parallel measurements and take the average value as the final result.
[0141] 3. HPLC method for detecting protein concentration:
[0142] Preparation of standard solutions: Accurately weigh an appropriate amount of collagen standard, dissolve it in purified water and make up to volume, prepare a series of standard stock solutions of different concentrations, filter them through a 0.22μm filter membrane and set aside for use.
[0143] Sample pretreatment: Accurately weigh 1.0g of essence sample (component A or finished product), add 10mL of purified water, extract by sonication for 30 minutes, centrifuge (5000rpm, 10 minutes), take the supernatant, filter through a 0.22μm filter membrane to obtain the sample solution.
[0144] Chromatographic conditions: C18 column (250 mm × 4.6 mm, 5 μm) was used; the mobile phase was acetonitrile-0.1% trifluoroacetic acid aqueous solution (gradient elution, such as initial acetonitrile ratio of 10%, gradually increasing to 40%); flow rate was 1.0 mL / min; column temperature was 30℃; detection wavelength was 220 nm.
[0145] Determination: Inject 10 μL of standard solution and sample solution into the high performance liquid chromatograph, record the chromatogram, calculate the concentration of collagen in the sample according to the standard curve, perform the determination in parallel 3 times, and take the average value.
[0146] 4. ELISA method for detecting protein integrity:
[0147] Sample pretreatment: Accurately weigh an appropriate amount of the essence sample (component A or finished product), and dilute it according to the kit instructions to ensure that the sample concentration is within the detection range of the kit.
[0148] Coating: Dilute the coating antibody according to the kit instructions and add 100 μL to each well of a microplate. Incubate overnight at 4°C.
[0149] Blocking: Discard the coating solution, wash the microplate three times with washing solution for three minutes each time, pat dry, add blocking solution, 200 μL per well, and incubate at 37°C for 1 hour.
[0150] Sample addition: Discard the blocking solution, wash, and add 100 μL of standard solution and sample solution to each well. Incubate at 37°C for 1 hour.
[0151] Add enzyme-labeled antibody: Discard the sample solution, wash and add 100 μL of enzyme-labeled antibody per well, and incubate at 37°C for 1 hour.
[0152] Color development: Discard the enzyme-labeled antibody solution, wash, add substrate solution, 100 μL per well, and incubate at 37°C in the dark for 15-30 minutes.
[0153] Termination and Measurement: Add 50 μL of stop solution to each well, gently shake to mix, and measure the absorbance of each well at 450 nm using a microplate reader. Calculate the collagen / elastin content and integrity-related indicators in the sample based on the standard curve.
[0154] 5. Microbial limit test:
[0155] Sample preparation: Accurately weigh 10g of the essence sample and add it to 90mL of sterile physiological saline containing a neutralizing agent. Shake thoroughly to mix and prepare a 1:10 sample dilution. Based on the expected microbial contamination level, further prepare a series of dilutions such as 1:100 and 1:1000.
[0156] Inoculation and incubation: Take 1 mL of sample dilution at different dilutions and inject it into a sterile petri dish. Perform two replicates for each dilution. For total bacterial count determination, add nutrient agar medium melted and cooled to 45℃±1℃, shake well, and after the agar solidifies, invert the dish and incubate at 36℃±1℃ for 48 hours±2 hours. For total mold and yeast count determination, add rose red sodium agar medium melted and cooled to 45℃±1℃, shake well, and after the agar solidifies, invert the dish and incubate at 28℃±1℃ for 72 hours±2 hours (extend to 5 days if necessary).
[0157] Colony counting: After the culture is completed, select petri dishes with colony counts between 30-300 CFU for counting, and calculate the total number of bacteria, molds and yeasts per gram of sample.
[0158] Judgment criteria: The total number of bacteria in cosmetics should be ≤1000 CFU / g(mL), and the total number of molds and yeasts should be ≤100 CFU / g(mL).
[0159] 6. Accelerated stability test:
[0160] Sample preparation: Dispense the finished essence into clean sampling bottles, seal them, and divide them into two groups. One group is used for accelerated testing at 40℃±2℃ and relative humidity of 75%±5%, and the other group is used for freezing testing at -20℃±2℃. At the same time, retain one sample as a control (stored at room temperature).
[0161] Sampling and testing: Samples were taken at 0, 30, 60 and 90 days, and the appearance, color, odor, pH value, viscosity and active ingredient content of the samples were tested to compare the differences at different time points and with the control sample.
[0162] Freeze-thaw cycle test: The sample is frozen at -20℃±2℃ for 24 hours, and then thawed at room temperature for 24 hours. This is one cycle. After repeating 3 cycles, the above indicators are measured.
[0163] 7. Heat / Cold Cycling Test: Sample Preparation: Dispense the finished essence into clean sampling bottles, seal them, and divide them into several portions.
[0164] Cyclic operation: First, place the sample in a constant temperature incubator at 45℃±2℃ for 8 hours, and then transfer it to a low temperature freezer at -15℃±2℃ for 16 hours. This constitutes one cycle, and three cycles are repeated.
[0165] Testing: After each cycle, the sample is removed and equilibrated at room temperature for 30 minutes. The appearance, color, odor, pH value, viscosity, and active ingredient content of the sample are then tested.
[0166] Judgment criteria: After 3 hot / cold cycles, the various indicators of the sample showed no significant changes, meeting the judgment criteria in the accelerated stability test, and the sample was judged to be qualified for hot / cold cycle stability.
[0167] 8. Skin elasticity and firmness test:
[0168] Subject preparation: Select healthy volunteers (usually 30-50 people, aged 35-60 years, with obvious wrinkles or loose skin). Within 24 hours before the test, the subjects should not use any cosmetics or skin care products on the test area (such as the corners of the eyes and forehead). On the day of the test, wash the skin of the test area and adapt to it in a constant temperature and humidity laboratory for 30 minutes.
[0169] Baseline value determination: Using a skin elastometer, mark three different test points on the test site and measure the skin elasticity parameters (such as R0, R1, R2, R3, R7, etc.) at each test point. R2 usually represents the total elasticity of the skin and R7 represents the biological elasticity of the skin. Each test point is measured three times, and the average value is taken as the baseline value.
[0170] Sample use and measurement: Subjects used the serum sample according to the prescribed method (e.g., apply an appropriate amount to the test area and massage it in after use once in the morning and once in the evening). They returned to the laboratory at 2, 4 and 8 weeks after use, and the skin elasticity parameters at each test point were measured under the same conditions. The rate of change of each parameter from the baseline value was calculated.
[0171] Judgment criteria: After 8 weeks of use, if the total elasticity parameter (R2) and bioelasticity parameter (R7) of the skin increased by ≥10% compared with the baseline value, the sample was deemed to have the effect of improving skin elasticity and firmness. The test results are shown in Table 1.
[0172] Table 1. Test results of the examples and comparative examples.
[0173]
[0174]
[0175] The core advantage of this embodiment lies in the construction of a two-component synergistic system. Component A acts as a dedicated isotonic buffer environment for collagen and elastin, stabilizing the system in the neutral range through a mixed buffer of disodium hydrogen phosphate and sodium dihydrogen phosphate, preventing protein flocculation due to pH fluctuations to the isoelectric point. Precisely concentrated sodium chloride provides suitable osmotic pressure to maintain the protein in a dissolved state, while 1,2-pentanediol also stabilizes the protein conformation and acts as an auxiliary preservative. Component B, through a stepwise preparation process, adapts to the characteristics of different components. Dissolving thickeners at room temperature prevents their high-temperature degradation or uneven hydration. When dissolving heat-resistant skin conditioning agents at 50-70°C, the solubilizer can achieve dispersion by inserting its lipophilic end into the oil phase to form stable micelles, thus resisting... Oxidizing agents simultaneously protect lipid components from thermal oxidation. Cooling the temperature to 40-50℃ and adding heat-sensitive components can minimize damage to their molecular structure. Chelating agents can also complex metal ions to cut off oxidation and microbial growth pathways. Furthermore, components A and B are mixed only at room temperature to ensure that their pre-optimized stable systems are not destroyed. In the examples, the mass ratio of components A to B is controlled at 0.3-3:1, and the mass ratio of heat-resistant and heat-sensitive skin conditioning agents is controlled at 0.5-2:1. With a reasonable increase in the proportion of component A, the protein stability and concentration are better. With the adaptation of the process and proportion of component B, the activity of the skin conditioning agent and the rheological properties of the system are more balanced. Overall, the unity of component activity, system stability and anti-aging efficacy is achieved.Comparative Example 1, lacking component B, lacks the synergistic effect of the skin conditioning agent and the stable carrier system constructed by the thickeners and solubilizers in component B. Therefore, it not only fails to exert the antioxidant and brightening effects of the conditioning agent but also suffers from poor skin feel and viscosity due to the absence of necessary rheology-regulating components. Comparative Example 2, lacking component A, completely lacks collagen and elastin, thus losing the core anti-aging mechanism of supplementing structural proteins to improve skin elasticity, and naturally cannot achieve the corresponding firming and wrinkle-reducing effects. Comparative Example 3 has a component A to B mass ratio of 5:1, exceeding the preferred range of 0.3-3:1, indicating that component A is excessively... The excessive amount of component B leads to abnormal ionic strength and viscosity in the system. A relative deficiency in component B results in insufficient stable micelles and carriers for the skin conditioning agent, thus affecting its activity and overall skin feel. In Comparative Example 4, the ratio of heat-resistant to heat-sensitive skin conditioning agent is 4:1, exceeding the preferred range of 0.5-2:1. Excessive heat-resistant lipid components exceed the solubility threshold of the solubilizer, preventing the formation of a stable micelle system. This not only causes turbidity and occasional oil spots but also interferes with the three-dimensional network structure constructed by the thickener, compromising system stability and a refreshing skin feel. In Comparative Example 5, the sodium chloride content exceeds 0.5-1.5%. The optimal range of components was not specified. Excessive ionic strength triggered a "salting-out" effect, disrupting the dissolved state of collagen and elastin, leading to a significant decrease in protein integrity and causing slight turbidity in the system due to protein precipitation. In Comparative Example 6, components A and B were directly mixed without providing suitable microenvironments for the protein and skin conditioning agent. The neutral pH of component A and the weakly acidic pH of component B interfered with each other, causing direct interaction between the protein, conditioning agent, and electrolytes, resulting in protein denaturation and flocculation, system stratification, and accelerated degradation of active ingredients due to interactions. In Comparative Example 7, component A was not pre-treated at 40-60℃. Dissolving inorganic salts and pH buffers to establish a stable ionic strength and pH environment, direct mixing leads to protein denaturation under unsuitable ionic and pH conditions. The system becomes turbid and unevenly colored due to uneven protein dispersion, and the integrity of the protein is significantly reduced. In Comparative Example 8, the temperature and order of addition were not controlled stepwise during the preparation of component B. The high temperature directly contacted the heat-sensitive skin conditioning agent, causing damage to its molecular structure and loss of activity. Furthermore, the thickener was not fully dissolved at room temperature to form a uniform network, and the solubilizer did not fully react with the heat-resistant components to form stable micelles, ultimately affecting the stability of the system and the efficacy of the conditioning agent.
[0176] Finally, it should be noted that the above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art can still modify the technical solutions described in the foregoing embodiments or make equivalent substitutions for some of the technical features. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the protection scope of the present invention.
Claims
1. A wrinkle-reducing and anti-aging serum containing collagen and elastin, characterized in that, Includes component A and component B with a mass ratio of 0.3-3:1; Component A, by mass, comprises the following components: 90-98 parts water A composition of collagen and elastin, 2-5 parts. 1-3 parts moisturizer Inorganic salts 0.5-1.5 parts, 0.1-0.2 parts of pH buffer; Component B, based on a total mass of 100 parts, consists of the following components: 15-25 parts moisturizer 5-10 parts of solubilizer 5-15 parts skin conditioning agent Antioxidant 0.5-2 parts, Thickener 0.3-1 part, Chelating agent 0.1-0.5 parts, pH adjuster 0.5-1.5 parts, The remainder is water.
2. The anti-wrinkle and anti-aging serum as described in claim 1, characterized in that, The humectant in component A is 1,2-pentanediol; the inorganic salt is sodium chloride; and the pH buffer is a mixture of disodium hydrogen phosphate and sodium dihydrogen phosphate.
3. The anti-wrinkle and anti-aging serum as described in claim 1, characterized in that, The skin conditioning agents in component B include heat-resistant skin conditioning agents and heat-sensitive skin conditioning agents; the heat-resistant skin conditioning agents include squalane, tocopherol, bisabolol, and tetrahydropiperine; the heat-sensitive skin conditioning agents include α-arbutin, glycyrrhizin, and ginseng root extract.
4. The anti-wrinkle and anti-aging essence as described in claim 3, characterized in that, The mass ratio of the heat-resistant skin conditioning agent to the heat-sensitive skin conditioning agent is 0.5-2:
1.
5. The anti-wrinkle and anti-aging serum as described in claim 1, characterized in that, The humectants in component B are butylene glycol and glycerin; the solubilizers are PEG-40 hydrogenated castor oil and PEG-60 hydrogenated castor oil; and the antioxidant is tocopherol.
6. The anti-wrinkle and anti-aging serum as described in claim 1, characterized in that, The thickeners in component B are hydroxyethyl cellulose and carbomer; the chelating agent is disodium EDTA; and the pH adjuster is citric acid.
7. A method for preparing an anti-wrinkle and anti-aging serum containing collagen and elastin as described in any one of claims 1-6, characterized in that, Includes the following steps: S1. Preparation of component A: Heat the water in component A to 40-60℃, add inorganic salts and pH buffer and stir to dissolve. After cooling to 30-40℃, add the combination of collagen and elastin and moisturizer, homogenize and adjust the pH value to 6.5-7.5 to obtain component A; S2. Preparation of component B: S21. Preparation of component B1: Mix water accounting for 30%-60% of the total water volume of component B with a thickener, stir at room temperature until completely dissolved, and obtain component B1; S22. Preparation of component B2: Heat the remaining water of component B to 50-70℃, add moisturizer, solubilizer, antioxidant, chelating agent and heat-resistant skin conditioning agent in sequence, and stir to dissolve; after cooling to 40-50℃, add heat-sensitive skin conditioning agent and stir to dissolve; finally add pH adjuster to adjust the pH of the system to 5.0-6.0 to obtain component B2; S23. Sterilized component B1 and filtered sterilized component B2 are mixed under stirring conditions, wherein component B2 is added to component B1 and stirred evenly to obtain component B; S3. Mixing: Mix component A and component B in proportion and at room temperature until homogeneous.
8. The method for producing an anti-wrinkle and anti-aging serum containing collagen and elastin as described in claim 7, characterized in that, In step S23, component B1 is sterilized by ultraviolet light, and component B2 is sterilized by filtration through a 0.22-micron microporous membrane.
9. The method for producing an anti-wrinkle and anti-aging serum containing collagen and elastin as described in claim 7, characterized in that, Step S3 is followed by steps of settling and defoaming, and filtration.