Eye essence lotion and preparation method thereof
By combining D-phase components, oil-phase components, aqueous-phase components, and cross-linked silicone gel, an O/W/SI multi-emulsion was prepared, which solved the irritation and stability problems of eye serums, achieving gentleness on the eye area and improved stability of active ingredients, resulting in significant skin repair and anti-aging effects.
Patent Information
- Application Number
- CN202511586450.8
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-11-01
- Publication Date
- 2025-12-19
AI Technical Summary
Existing eye serums are often quite irritating to the skin around the eyes, and their active ingredients have poor stability.
An O/W promulgation was prepared by combining a D-phase component, an oil phase component, an aqueous phase component, and a cross-linked silicone gel, using a bio-emulsifier instead of a traditional emulsifier, and employing a D-phase emulsification method. Vitamin K2 was encapsulated in a non-organosilicone oil, sialic acid and fibronectin were dissolved in the aqueous phase, and the outermost layer was formed by cross-linked silicone gel to form an oxygen barrier layer, thus forming an O/W/SI multi-emulsion.
The product's irritation has been reduced, and the stability of active ingredients has been improved, making it suitable for delicate eye skin. It is especially resistant to deactivation and discoloration under high temperature and light conditions, and has significant repairing, anti-wrinkle, moisturizing, and dark circle-reducing effects.
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Figure CN121154443A_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The present application relates to the cosmetic technical field, and in particular to an eye essence cream and a preparation method thereof. BACKGROUND
[0002] The eye skin is one of the thinnest and most fragile skin areas of the human body, with a thickness of about 0.50 millimeters, lacking sebaceous glands and sweat glands, and the collagen loss rate is 3 times faster than other parts of the face. Therefore, the eye skin is more prone to problems, especially the modern people stay up late, under great pressure and overuse eyes, etc. The eye skin is prone to problems such as dark circles, fine lines, dryness and relaxation.
[0003] The existing eye essence cream usually contains active ingredients such as caffeine, retinol and derivatives thereof. These active ingredients often have greater irritancy, and the stability of the active ingredients is poor. At the same time, when the eye essence cream is prepared by using the traditional emulsification technology, a large amount of traditional emulsifiers need to be used, which brings potential greater irritancy to the eye skin.
[0004] The existing technical solutions in the above have the following defects: the existing eye essence cream has greater irritancy to the eye skin, and the stability of the active ingredients is poor. SUMMARY
[0005] In order to improve the mildness of the eye essence cream and improve the stability of the active ingredients, the present application provides an eye essence cream and a preparation method thereof.
[0006] The first object of the present application is to provide an eye essence cream, which adopts the following technical solution: An eye essence cream, comprising a D-phase component, an oil-phase component, an aqueous-phase component and a cross-linked silicone gel; The D-phase component comprises a biological emulsifier and a first polyol; The oil-phase component comprises vitamin K2 and a non-silicone oil; The aqueous-phase component comprises bird's nest acid, fibronectin, a second polyol, a water-soluble polymer, a preservative, a pH regulator and deionized water; The cross-linked silicone gel comprises an organosilicon cross-linked polymer, a polyether / polyglycerol modified cross-linked organosilicon polymer and an organosilicon oil.
[0007] The vitamin K2 has good affinity with human skin, has soothing, antioxidant, skin barrier functions, and can repair and improve skin aging problems. In particular, it can inhibit abnormal angiogenesis and promote blood circulation, and has a significant effect on improving blood vessel type dark circles. The bird's nest acid has excellent moisturizing, antioxidant, soothing, anti-aging and skin lightening effects. The fibronectin can promote cell adhesion and migration and accelerate skin repair. The synergistic effect of vitamin K2, bird's nest acid and fibronectin makes the eye serum emulsion have good repair, anti-wrinkle, moisturizing and dark circle lightening effects. The biological emulsifier is used instead of the traditional emulsifier, and the O / W primary emulsion is prepared by using the D-phase emulsification method, the vitamin K2 is encapsulated in the non-silicone oil of the O / W primary emulsion, the bird's nest acid and the fibronectin are dissolved in the water phase of the O / W primary emulsion, and the outermost layer uses the cross-linked silicone gel to form an oxygen barrier layer, thereby forming an O / W / SI multiple emulsion, greatly reducing the irritation of the product, improving the mildness of the eye serum emulsion, and making it suitable for delicate eye skin. At the same time, the stability of the active ingredients is effectively improved, so that the active ingredients are not easily inactivated and discolored under high temperature and light conditions.
[0008] The application is further provided that, in terms of the mass percentage of the eye serum emulsion, the D-phase component includes 0.05-5wt% of the biological emulsifier and 1-10wt% of the first polyol; the oil-phase component includes 0.01-0.1wt% of the vitamin K2 and 2-15wt% of the non-silicone oil; the water-phase component includes 0.1-2wt% of the bird's nest acid, 0.005-0.05wt% of the fibronectin, 1-5wt% of the second polyol, 0.1-1wt% of the water-soluble polymer, 0.1-1wt% of the preservative, 0.5-1.5wt% of the pH regulator and 20-70wt% of the deionized water; and the cross-linked silicone gel includes 0.5-5wt% of the silicone cross-linked polymer, 0.5-5wt% of the polyether / polyglycerol modified cross-linked silicone polymer and 25-65wt% of the silicone oil.
[0009] The application is further provided that the biological emulsifier is at least one of the Bacillus fermentation product and the glycolipid prepared by microbial fermentation; the first polyol is at least one of glycerol, butylene glycol and 1,3-propanediol; and the second polyol is at least one of glycerol, butylene glycol and 1,3-propanediol.
[0010] The application is further provided that the non-silicone oil is at least one of caprylic / capric triglyceride and dicaprylyl carbonate; and the silicone oil is at least one of dimethicone and cyclopentadimethylsiloxane.
[0011] By adopting the above technical scheme, the vitamin K2 is easily dissolved, and has high oxidation stability.
[0012] The application is further provided that the water-soluble polymer is at least one of acryloyldimethyltaurate ammonium / VP copolymer, xanthan gum and hydroxyethyl cellulose; the preservative is at least one of phenoxyethanol, ethylhexylglycerin, chlorphenesin and p-hydroxyacetophenone; and the pH regulator is at least one of arginine, triethanolamine, aminomethylpropanol and sodium hydroxide.
[0013] The application is further provided that the silicone cross-linked polymer has a three-dimensional network structure and is at least one of polydimethylsiloxane / vinyl polydimethylsiloxane cross-linked polymer, di-vinyl polydimethylsiloxane / polydimethylsiloxane cross-linked polymer and diphenyl polydimethylsiloxane cross-linked polymer.
[0014] By adopting the above technical solution, the silicone cross-linked polymer does not contain polyether chains or polyglycerol chains in the molecular structure, can form a high-viscosity silicone gel in silicone oil, and can stabilize the oil phase through the three-dimensional network structure.
[0015] The application is further provided that the polyether / polyglycerol modified cross-linked silicone polymer is at least one of polydimethylsiloxane PEG-10 / 15 cross-linked polymer, polydimethylsiloxane PEG-15 cross-linked polymer and polydimethylsiloxane / polyglycerol-3 cross-linked polymer.
[0016] By adopting the above technical solution, the polyether / polyglycerol modified cross-linked silicone polymer has hydrophilicity, lipophilicity and thickening properties, does not contain alkyl chains in the molecular structure, and can prevent vitamin K2 and non-silicone oil in the O / W primary emulsion from migrating to the outer layer.
[0017] The second object of the application is to provide a preparation method of an eye area essence cream, which adopts the following technical solution: The preparation method of an eye area essence cream comprises the following steps: S1. Preparing oil phase components, water phase components, cross-linked silicone gel and D phase components; S2. Adding the oil phase components to the D phase components and mixing to form D phase oil gel; S3. Adding the water phase components to the D phase oil gel and mixing to form O / W primary emulsion; S4. Adding the O / W primary emulsion to the cross-linked silicone gel and mixing to form an eye area essence cream; S5. Performing vacuum defoaming treatment on the eye area essence cream.
[0018] By adopting the above technical scheme, the O / W / SI multiple emulsification technology is adopted, vitamin K2, bird's nest acid and fibronectin are used, the moisture content of eye skin can be significantly improved, the moisturizing effect is good, the skin barrier can be significantly enhanced, the water locking effect is good, the skin elasticity can be significantly enhanced, the anti-wrinkle effect is good, the ITA° value of eye skin can be significantly increased, the skin color can be brightened, and the effect of improving dark circles is certain, and the synergy in improving the problems of eye skin is certain. Compared with the traditional O / W emulsification technology for preparing eye essence milk, the bioavailability of active substances can be effectively improved, and the advantages in increasing the water content of the cuticle layer and promoting skin barrier repair are certain. At the same time, the O / W / SI multiple emulsification technology can effectively solve the problems of easy discoloration and inactivation of active ingredients under high temperature and light conditions, improve the stability of active ingredients, improve the mildness of eye essence milk, and make it suitable for delicate eye skin, and the safety is higher.
[0019] The application is further provided: in step S1, the above amount of non-silicone oil is added to the above amount of vitamin K2, and mixed to form an oil phase component; the above amount of water-soluble polymer is added to the above amount of second polyol, and mixed to form a water-soluble polymer dispersion; the above amount of deionized water is added to the above amount of bird's nest acid, and mixed to form a bird's nest acid solution; the pH of the bird's nest acid solution is adjusted to 6-7 by using the above amount of pH adjuster, and then the above amount of fibronectin, the above amount of preservative and the water-soluble polymer dispersion are added to the bird's nest acid solution, and mixed to form an aqueous phase component; the above amount of silicone oil is added to the above amount of silicone cross-linked polymer and the above amount of polyether / polyglycerol modified cross-linked silicone polymer, and mixed to form a cross-linked silicone gel; the above amount of first polyol is added to the above amount of biological emulsifier, and mixed to form a D-phase component.
[0020] The application is further provided: in step S1, when preparing the cross-linked silicone gel, the stirring speed is 800-1200 r / min; in step S2, the stirring speed is 800-1200 r / min; in step S3, the stirring speed is 800-1200 r / min; in step S4, the stirring speed is 800-1200 r / min; in step S5, the vacuum degree is between-0.08 Mpa and-0.12 Mpa; The oil phase component, the aqueous phase component, the cross-linked silicone gel, the D-phase component, the D-phase oil gel, the O / W primary emulsion and the eye essence milk are prepared at room temperature.
[0021] By adopting the above technical scheme, the vacuum degree is between-0.08 Mpa and-0.12 Mpa, which avoids the catalytic oxidation of active ingredients caused by the oxygen-containing air rolled in by rapid stirring.
[0022] In summary, the beneficial technical effects of the present application are: 1. Vitamin K2 has good affinity with human skin, has soothing, antioxidant, skin barrier function, and can repair and improve skin aging problems. Especially it can inhibit abnormal angiogenesis and promote blood circulation, and has significant effect on improving blood vessel type dark circles. Bird's nest acid has excellent moisturizing, antioxidant, soothing, anti-aging and skin lightening effects. Fibronectin can promote cell adhesion and migration and accelerate skin repair. The synergistic effect of vitamin K2, bird's nest acid and fibronectin makes the eye serum cream have good repair, anti-wrinkle, moisturizing and dark circle lightening effects. Biological emulsifiers are used instead of traditional emulsifiers, and D-phase emulsification method is used to prepare O / W primary emulsion, vitamin K2 is encapsulated in the non-silicone oil of O / W primary emulsion, bird's nest acid and fibronectin are dissolved in the water phase of O / W primary emulsion, and the outermost layer uses cross-linked silicone gel to form an oxygen barrier layer, forming an O / W / SI multiple emulsion, which greatly reduces the irritation of the product and improves the mildness of the eye serum cream, making it suitable for delicate eye skin. At the same time, the stability of the active ingredients is effectively improved, so that the active ingredients are not easily inactivated and discolored under high temperature and light conditions.
[0023] 2. Vitamin K2 is easily soluble and has high oxidative stability.
[0024] 3. The molecular structure of the organosilicon cross-linked polymer does not contain polyether chains or polyglycerol chains, and can form high-viscosity silicone gel in silicone oil, which can stabilize the oil phase through a three-dimensional network structure.
[0025] 4. The cross-linked organosilicon polymer modified by polyether / polyglycerol has hydrophilicity, lipophilicity and thickening property, and its molecular structure does not contain alkyl chains, which can prevent the migration of vitamin K2 and non-silicone oil in the O / W primary emulsion to the outer layer. BRIEF DESCRIPTION OF DRAWINGS
[0026] Figure 1 is a comparison chart of the appearance of the eye serum creams prepared in Examples 1-3 and Comparative Example 1 after stability testing at 50°C under natural light for 4 weeks; Figure 2 is a comparison chart of the change in the water content of the stratum corneum of the eye skin of the subjects before using the eye serum creams prepared in Example 2, Comparative Example 1, Comparative Example 3, Comparative Example 4 and Comparative Example 5, after using the eye serum creams for 14 days, and after using the eye serum creams for 28 days; Figure 3 is a comparison chart of the change in the amount of transdermal water loss of the eye skin of the subjects before using the eye serum creams prepared in Example 2, Comparative Example 1, Comparative Example 3, Comparative Example 4 and Comparative Example 5, after using the eye serum creams for 14 days, and after using the eye serum creams for 28 days; Figure 4is a comparison chart of changes in the elasticity of the eye skin of the subject before and after using the eye serum cream of Example 2, Comparative Example 1, Comparative Example 3, Comparative Example 4 and Comparative Example 5 for 14 days and 28 days. Figure 5 is a comparison chart of changes in the ITA° value of the eye skin of the subject before and after using the eye serum cream of Example 2, Comparative Example 1, Comparative Example 3, Comparative Example 4 and Comparative Example 5 for 14 days and 28 days. DETAILED DESCRIPTION
[0027] It should be noted that vitamin K2, as an important fat-soluble vitamin in the human body, is extremely sensitive to light and heat, and is prone to discoloration and inactivation. Edible bird's nest acid, also known as sialic acid, is a naturally occurring acidic amino sugar that exists widely in living organisms, especially in edible bird's nest. Edible bird's nest acid is also extremely prone to discoloration and inactivation under high temperature and light conditions, affecting the efficacy and appearance uniformity of the cosmetic product. Fibronectin, as a multifunctional extracellular matrix glycoprotein, is prone to conformational changes and loss of activity due to the influence of temperature, pH value and mechanical stress.
[0028] The embodiment of the present application discloses an eye serum cream, which comprises a D-phase component, an oil-phase component, an aqueous-phase component and a cross-linked silicone gel. The D-phase component comprises a biological emulsifier and a first polyol. The oil-phase component comprises vitamin K2 and a non-silicone oil. The aqueous-phase component comprises edible bird's nest acid, fibronectin, a second polyol, a water-soluble polymer, a preservative, a pH regulator and deionized water. The cross-linked silicone gel comprises an organosilicon cross-linked polymer, a polyether / polyglycerol modified cross-linked organosilicon polymer and an organosilicon oil. Vitamin K2 has good affinity with human skin, has soothing, antioxidant and skin barrier functions, and can repair and improve skin aging problems. In particular, it can inhibit abnormal angiogenesis and promote blood circulation, and has a significant effect on improving blood vessel type dark circles. Edible bird's nest acid has excellent moisturizing, antioxidant, soothing, anti-aging and skin lightening effects. Fibronectin can promote cell adhesion and migration and accelerate skin repair. The synergistic effect of vitamin K2, edible bird's nest acid and fibronectin enables the eye serum cream to have good repair, anti-wrinkle, moisturizing and dark circle lightening effects. The biological emulsifier is used to replace the traditional emulsifier, and the D-phase emulsification method is used to prepare an O / W primary emulsion, the vitamin K2 is encapsulated in the non-silicone oil of the O / W primary emulsion, the edible bird's nest acid and the fibronectin are dissolved in the aqueous phase of the O / W primary emulsion, and the outermost layer uses the cross-linked silicone gel to form an oxygen barrier layer, thereby forming an O / W / SI multiple emulsion, greatly reducing the irritation of the product and improving the mildness of the eye serum cream, so that it is suitable for delicate eye skin. At the same time, the stability of the active ingredients (vitamin K2, edible bird's nest acid and fibronectin) is effectively improved, so that the active ingredients are not prone to inactivation and discoloration under high temperature and light conditions.
[0029] It should be noted that the cross-linked silicone gel does not contain linear or branched silicone emulsifiers.
[0030] In one embodiment, the D-phase component includes 0.05-5wt% of the biological emulsifier and 1-10wt% of the first polyol, the oil-phase component includes 0.01-0.1wt% of vitamin K2 and 2-15wt% of the non-silicone oil, the water-phase component includes 0.1-2wt% of the bird's nest acid, 0.005-0.05wt% of the fibronectin, 1-5wt% of the second polyol, 0.1-1wt% of the water-soluble polymer, 0.1-1wt% of the preservative, 0.5-1.5wt% of the pH regulator, and 20-70wt% of the deionized water, and the cross-linked silicone gel includes 0.5-5wt% of the silicone cross-linked polymer, 0.5-5wt% of the polyether / polyglycerol modified cross-linked silicone polymer, and 25-65wt% of the silicone oil.
[0031] In one embodiment, the biological emulsifier is at least one of the Bacillus fermentation product and the glycolipid prepared by microbial fermentation. The first polyol is at least one of glycerol, butylene glycol, and 1,3-propanediol. The second polyol is at least one of glycerol, butylene glycol, and 1,3-propanediol.
[0032] Preferably, the biological emulsifier is at least one of the Bacillus fermentation product and the glycolipid prepared by microbial fermentation of Bacillus subtilis, Pseudomonas aeruginosa, or Myriococcum.
[0033] In one embodiment, the non-silicone oil is at least one of caprylic / capric triglyceride and dioctyl carbonate. The non-silicone oil is easy to dissolve vitamin K2 and has high oxidation stability. The silicone oil is at least one of dimethicone and cyclopentadimethylsiloxane.
[0034] In one embodiment, the water-soluble polymer is at least one of acryloyldimethyltauramide / VP copolymer, xanthan gum, and hydroxyethyl cellulose. The preservative is at least one of phenoxyethanol, ethylhexylglycerin, chlorphenesin, and p-hydroxyacetophenone; and the pH regulator is at least one of arginine, triethanolamine, aminomethylpropanol, and sodium hydroxide.
[0035] In one embodiment, the silicone cross-linked polymer has a three-dimensional network structure, is at least one of polydimethylsiloxane / vinyl polydimethylsiloxane cross-linked polymer, divinyl polydimethylsiloxane / polydimethylsiloxane cross-linked polymer, and diphenyl polydimethylsiloxane cross-linked polymer, and does not contain a polyether chain or a polyglycerol chain in the molecular structure, so that a high-viscosity silicone gel can be formed in the silicone oil and the oil phase can be stabilized by the three-dimensional network structure.
[0036] In one embodiment, the polyether / polyglycerin modified cross-linked silicone polymer is at least one of dimethicone PEG-10 / 15 crosspolymer, dimethicone PEG-15 crosspolymer, and dimethicone / polyglycerin-3 crosspolymer. The polyether / polyglycerin modified cross-linked silicone polymer has hydrophilicity, lipophilicity, and thickening property, and does not contain an alkyl chain in the molecular structure, which can prevent the migration of vitamin K2 and non-silicone oil in the O / W initial cream to the outer layer.
[0037] It should be noted that the following mass percentages are based on the mass percentage of the eye essence cream.
[0038] The application also discloses a preparation method of the eye essence cream. S1. Preparing an oil phase component, a water phase component, a cross-linked silicone gel, and a D phase component.
[0039] In the embodiment of the application, under the condition of normal temperature and low-speed stirring, 0.01-0.1wt% of vitamin K2 is added to 2-15wt% of non-silicone oil until the vitamin K2 is completely dissolved, forming the oil phase component.
[0040] In the embodiment of the application, under the condition of normal temperature and low-speed stirring, 0.1-1wt% of water-soluble polymer is added to 1-5wt% of the second polyol to form a water-soluble polymer dispersion liquid. Then, 0.1-2wt% of bird's nest acid is added to 20-70wt% of deionized water to form a bird's nest acid solution. Subsequently, the pH of the bird's nest acid solution is adjusted to 6-7 by using 0.5-1.5wt% of a pH adjuster, and then 0.005-0.05wt% of fibronectin, 0.1-1wt% of a preservative, and the water-soluble polymer dispersion liquid are added to the bird's nest acid solution until the water-soluble polymer is completely swelled, forming the water phase component.
[0041] In the embodiment of the application, under the condition of normal temperature and stirring speed of 800-1200r / min, 0.5-5wt% of silicone cross-linked polymer and 0.5-5wt% of polyether / polyglycerin modified cross-linked silicone polymer are added to 25-65wt% of silicone oil to form the cross-linked silicone gel.
[0042] In the embodiment of the application, under the condition of normal temperature and low-speed stirring, 0.05-5wt% of biological emulsifier is added to 1-10wt% of the first polyol to form the D phase component.
[0043] S2. Add the oil phase component to the D phase component and mix well to form the D phase oleogel.
[0044] In this embodiment, under the conditions of room temperature and a stirring speed of 800-1200 r / min, the oil phase component is slowly added to the D phase component and mixed to form a D phase oleogel.
[0045] S3. Add the aqueous phase component to the D phase oleogel and mix well to form an O / W primary emulsion.
[0046] In this embodiment, at room temperature and with a stirring speed of 800-1200 r / min, the aqueous phase component is slowly added to the D-phase oleogel and mixed to form an O / W primary emulsion.
[0047] S4. Add O / W colostrum to the cross-linked silicone gel and mix well to form an eye serum.
[0048] In this embodiment, under the conditions of room temperature and a stirring speed of 800-1200 r / min, O / W pre-emulsion is slowly added to the cross-linked silicone gel and mixed to form an eye serum.
[0049] S5. Vacuum defoaming treatment is performed on the eye serum.
[0050] In this embodiment of the application, when the eye serum is subjected to vacuum defoaming treatment, the vacuum degree is between -0.08Mpa and -0.12Mpa to avoid the catalytic oxidation of active ingredients by oxygen-containing air entrained by rapid stirring.
[0051] Preparation Example Preparation Example 1 Under normal temperature and low-speed stirring conditions, vitamin K2 (0.02 wt%) was added to 7 wt% caprylic / capric triglyceride until the vitamin K2 was completely dissolved, forming an oil phase component.
[0052] Under ambient temperature and low-speed stirring conditions, 0.5 wt% hydroxyethyl cellulose was added to 5 wt% butanediol and mixed thoroughly to form a water-soluble polymer dispersion. Then, 2 wt% sialic acid was added to 40.365 wt% deionized water and mixed thoroughly to form a sialic acid solution. Subsequently, the pH of the sialic acid solution was adjusted to 6-7 using 1.1 wt% pH adjuster. Then, 0.015 wt% fibronectin, 0.54 wt% phenoxyethanol, 0.06 wt% ethylhexylglycerin, and the water-soluble polymer dispersion were added to the sialic acid solution until the hydroxyethyl cellulose completely swelled, forming the aqueous phase.
[0053] Under the condition of normal temperature and high-speed stirring, 0.5wt% of polydimethylsiloxane / vinyl polydimethylsiloxane cross-linking polymer and 1.2wt% of polydimethylsiloxane PEG-10 / 15 cross-linking polymer were added into 33.3wt% of cyclopentameric dimethylsiloxane, and then mixed to form a cross-linked silicone gel.
[0054] Under the condition of normal temperature and low-speed stirring, 0.4wt% of Bacillus fermentation product was added into 8wt% of glycerol, and then mixed to form the D-phase component.
[0055] Preparation Example 2 Under the condition of normal temperature and low-speed stirring, 0.05wt% of vitamin K2 was added into 9wt% of caprylic / capric triglyceride until the vitamin K2 was completely dissolved, to form the oil-phase component.
[0056] Under the condition of normal temperature and low-speed stirring, 0.6wt% of acryloyl dimethyl ammonium taurate / VP copolymer was added into 5wt% of butanediol, and then mixed to form a water-soluble polymer dispersion. Then, 1wt% of bird's nest acid was added into 29.4wt% of deionized water, and then mixed to form a bird's nest acid solution. Subsequently, the pH of the bird's nest acid solution was adjusted to 6-7 by using 0.55wt% of a pH adjuster, and then 0.01wt% of fibronectin, 0.54wt% of phenoxyethanol, 0.06wt% of ethylhexylglycerin and the water-soluble polymer dispersion were added into the bird's nest acid solution until the acryloyl dimethyl ammonium taurate / VP copolymer was completely swelled, to form the water-phase component.
[0057] Under the condition of normal temperature and high-speed stirring, 1.5wt% of polydimethylsiloxane / vinyl polydimethylsiloxane cross-linking polymer and 2.4wt% of polydimethylsiloxane PEG-10 / 15 cross-linking polymer were added into 46.1wt% of polydimethylsiloxane, and then mixed to form a cross-linked silicone gel.
[0058] Under the condition of normal temperature and low-speed stirring, 0.2wt% of Bacillus fermentation product was added into 3.5wt% of glycerol, and then mixed to form the D-phase component.
[0059] Preparation Example 3 Under the condition of normal temperature and low-speed stirring, 0.03wt% of vitamin K2 was added into 5wt% of dicaprylyl carbonate until the vitamin K2 was completely dissolved, to form the oil-phase component.
[0060] Under the condition of normal temperature and low speed stirring, 0.4wt% of hydroxyethyl cellulose was added into 4wt% of butanediol to form a water-soluble polymer dispersion liquid. Then, 1.5wt% of bird's nest acid was added into 37.632wt% of deionized water to form a bird's nest acid solution. After that, the pH of the bird's nest acid solution was adjusted to 6-7 by using 0.83wt% of a pH adjuster, and then 0.008wt% of fibronectin, 0.54wt% of phenoxyethanol, 0.06wt% of ethylhexylglycerin and the water-soluble polymer dispersion liquid were added into the bird's nest acid solution until the hydroxyethyl cellulose was completely swollen to form the water phase component.
[0061] Under the condition of normal temperature and high speed stirring, 0.5wt% of dimethicone / vinyl dimethicone crosspolymer and 1.5wt% of dimethicone / polyglycerin-3 crosspolymer were added into 37.5wt% of dimethicone to form a crosslinked silicone gel.
[0062] Under the condition of normal temperature and low speed stirring, 0.5wt% of glycolipid was added into 10wt% of glycerol to form the D phase component.
[0063] Preparation Example 4 Under the condition of normal temperature and low speed stirring, 0.01wt% of vitamin K2 was added into 2wt% of caprylic / capric triglyceride until the vitamin K2 was completely dissolved to form the oil phase component.
[0064] Under the condition of normal temperature and low speed stirring, 0.1wt% of acryloyldimethyltaurine ammonium / VP copolymer was added into 1wt% of butanediol to form a water-soluble polymer dispersion liquid. Then, 0.1wt% of bird's nest acid was added into 66.035wt% of deionized water to form a bird's nest acid solution. After that, the pH of the bird's nest acid solution was adjusted to 6-7 by using a suitable pH adjuster, and then 0.005wt% of fibronectin, 0.54wt% of phenoxyethanol, 0.06wt% of ethylhexylglycerin and the water-soluble polymer dispersion liquid were added into the bird's nest acid solution until the acryloyldimethyltaurine ammonium / VP copolymer was completely swollen to form the water phase component.
[0065] Under the condition of normal temperature and high-speed stirring, 2.5wt% of polydimethylsiloxane / vinyl polydimethylsiloxane cross-linked polymer and 0.5wt% of polydimethylsiloxane PEG-10 / 15 cross-linked polymer were added into 25wt% of polydimethylsiloxane, and then mixed to form a cross-linked silicone gel.
[0066] Under the condition of normal temperature and low-speed stirring, 5wt% of Bacillus fermentation product was added into 10wt% of glycerin, and then mixed to form the D-phase component.
[0067] Preparation Example 5 Under the condition of normal temperature and low-speed stirring, 0.1wt% of vitamin K2 was added into 15wt% of caprylic / capric triglyceride until the vitamin K2 was completely dissolved, and then the oil-phase component was formed.
[0068] Under the condition of normal temperature and low-speed stirring, 0.1wt% of acryloyl dimethyl ammonium taurate / VP copolymer was added into 1wt% of butanediol, and then mixed to form a water-soluble polymer dispersion. Then, 0.1wt% of bird's nest acid was added into 41.265wt% of deionized water, and then mixed to form a bird's nest acid solution. After that, the pH of the bird's nest acid solution was adjusted to 6-7 by using a suitable pH adjuster, and then 0.005wt% of fibronectin, 0.54wt% of phenoxyethanol, 0.06wt% of ethylhexylglycerin and the water-soluble polymer dispersion were added into the bird's nest acid solution until the acryloyl dimethyl ammonium taurate / VP copolymer was completely swelled, and then the water-phase component was formed.
[0069] Under the condition of normal temperature and high-speed stirring, 0.5wt% of polydimethylsiloxane / vinyl polydimethylsiloxane cross-linked polymer and 0.5wt% of polydimethylsiloxane PEG-10 / 15 cross-linked polymer were added into 25wt% of polydimethylsiloxane, and then mixed to form a cross-linked silicone gel.
[0070] Under the condition of normal temperature and low-speed stirring, 5wt% of Bacillus fermentation product was added into 10wt% of glycerin, and then mixed to form the D-phase component.
[0071] Preparation Example 6 The difference from Preparation Example 1 is that the bioemulsifier is a glycolipid, and the first polyol is butanediol. The second polyol is 1,3-propanediol, the non-silicone oil is dioctyl carbonate, the silicone oil is polydimethylsiloxane, the water-soluble polymer is acryloyldimethyltaurine ammonium / VP copolymer, the silicone cross-linked polymer is diphenyl polydimethylsiloxane cross-linked polymer, and the polyether / polyglycerin modified cross-linked silicone polymer is polydimethylsiloxane / polyglycerin-3 cross-linked polymer.
[0072] Preparation Example 7 The difference from Preparation Example 2 is that the bioemulsifier is a glycolipid, and the first polyol is butanediol. The second polyol is 1,3-propanediol, the non-silicone oil is dioctyl carbonate, the silicone oil is cyclopentadimethylsiloxane, the water-soluble polymer is xanthan gum, the silicone cross-linked polymer is diphenyl polydimethylsiloxane cross-linked polymer, and the polyether / polyglycerin modified cross-linked silicone polymer is polydimethylsiloxane / polyglycerin-3 cross-linked polymer.
[0073] Preparation Example 8 The difference from Preparation Example 3 is that the bioemulsifier is Bacillus fermentation product, and the first polyol is 1,3-propanediol. The second polyol is glycerol, the non-silicone oil is caprylic / capric acid triglyceride, the silicone oil is cyclopentadimethylsiloxane, the water-soluble polymer is xanthan gum, the silicone cross-linked polymer is polydimethylsiloxane / vinyl polydimethylsiloxane cross-linked polymer, and the polyether / polyglycerin modified cross-linked silicone polymer is polydimethylsiloxane PEG-15 cross-linked polymer.
[0074] Preparation Example 9 Under the condition of normal temperature and low-speed stirring, 0.05wt% of vitamin K2 was added into 9wt% of caprylic / capric acid triglyceride until vitamin K2 was completely dissolved to form the oil phase component.
[0075] Under the condition of normal temperature and low-speed stirring, 0.6wt% of acryloyldimethyltaurine ammonium / VP copolymer was added into 5wt% of butanediol to form the water-soluble polymer dispersion liquid.
[0076] Preparation Example 10 The difference from Preparation Example 2 is that when preparing the silicone gel, 0.25wt% of propylene glycol carbonate and 1.25wt% of lithium montmorillonite dimethyl stearate were slowly added into 45.5wt% of polydimethylsiloxane under the condition of normal temperature and continuous stirring, and then 3wt% of PEG-10 polydimethylsiloxane was slowly added into the mixture when a uniform gel was formed to form the silicone gel.
[0077] Preparation Example 11 The difference from Preparation Example 2 is that no bird's nest acid is added when preparing the water phase component.
[0078] Preparation Example 12 The difference from Preparation Example 2 is that no vitamin K2 is added when preparing the oil phase component.
[0079] Preparation Example 13 The difference from Preparation Example 2 is that no fibronectin is added when preparing the water phase component.
[0080] Example Example 1
[0081] Under the conditions of room temperature and stirring speed of 1000 r / min, the oil phase component in Preparation Example 1 is slowly added to the D phase component in Preparation Example 1, mixed to form a D phase oil gel, then the water phase component in Preparation Example 1 is slowly added to the D phase oil gel, mixed to form an O / W primary emulsion, and then the O / W primary emulsion is slowly added to the cross-linked silica gel in Preparation Example 1, mixed to form an eye area essence. Finally, the eye area essence is subjected to vacuum defoaming treatment, and the vacuum degree is -0.10 MPa. Example 2
[0082] Under the conditions of room temperature and stirring speed of 1000 r / min, the oil phase component in Preparation Example 2 is slowly added to the D phase component in Preparation Example 2, mixed to form a D phase oil gel, then the water phase component in Preparation Example 2 is slowly added to the D phase oil gel, mixed to form an O / W primary emulsion, and then the O / W primary emulsion is slowly added to the cross-linked silica gel in Preparation Example 2, mixed to form an eye area essence. Finally, the eye area essence is subjected to vacuum defoaming treatment, and the vacuum degree is -0.10 MPa. Example 3
[0083] Under the conditions of room temperature and stirring speed of 1000 r / min, the oil phase component in Preparation Example 3 is slowly added to the D phase component in Preparation Example 3, mixed to form a D phase oil gel, then the water phase component in Preparation Example 3 is slowly added to the D phase oil gel, mixed to form an O / W primary emulsion, and then the O / W primary emulsion is slowly added to the cross-linked silica gel in Preparation Example 3, mixed to form an eye area essence. Finally, the eye area essence is subjected to vacuum defoaming treatment, and the vacuum degree is -0.10 MPa. Example 4
[0084] Under the condition of normal temperature and stirring speed of 1000 r / min, the oil phase component in Preparation Example 4 was slowly added into the D phase component in Preparation Example 4 to form a D phase oil gel, and then the water phase component in Preparation Example 4 was slowly added into the D phase oil gel to form an O / W primary emulsion, and then the O / W primary emulsion was slowly added into the cross-linked silica gel in Preparation Example 4 to form an eye area essence. Finally, the eye area essence was subjected to vacuum defoaming treatment, and the vacuum degree was -0.10 MPa. Example 5
[0085] Under the condition of normal temperature and stirring speed of 1000 r / min, the oil phase component in Preparation Example 5 was slowly added into the D phase component in Preparation Example 5 to form a D phase oil gel, and then the water phase component in Preparation Example 5 was slowly added into the D phase oil gel to form an O / W primary emulsion, and then the O / W primary emulsion was slowly added into the cross-linked silica gel in Preparation Example 5 to form an eye area essence. Finally, the eye area essence was subjected to vacuum defoaming treatment, and the vacuum degree was -0.10 MPa. Example 6
[0086] Under the condition of normal temperature and stirring speed of 1000 r / min, the oil phase component in Preparation Example 6 was slowly added into the D phase component in Preparation Example 6 to form a D phase oil gel, and then the water phase component in Preparation Example 6 was slowly added into the D phase oil gel to form an O / W primary emulsion, and then the O / W primary emulsion was slowly added into the cross-linked silica gel in Preparation Example 6 to form an eye area essence. Finally, the eye area essence was subjected to vacuum defoaming treatment, and the vacuum degree was -0.10 MPa. Example 7
[0087] Under the condition of normal temperature and stirring speed of 1000 r / min, the oil phase component in Preparation Example 7 was slowly added into the D phase component in Preparation Example 7 to form a D phase oil gel, and then the water phase component in Preparation Example 7 was slowly added into the D phase oil gel to form an O / W primary emulsion, and then the O / W primary emulsion was slowly added into the cross-linked silica gel in Preparation Example 7 to form an eye area essence. Finally, the eye area essence was subjected to vacuum defoaming treatment, and the vacuum degree was -0.10 MPa. Example 8
[0088] Under the condition of normal temperature and stirring speed of 1000 r / min, the oil phase component in Preparation Example 8 was slowly added into the D phase component in Preparation Example 8 to form a D phase oil gel, and then the water phase component in Preparation Example 8 was slowly added into the D phase oil gel to form an O / W primary emulsion, and then the O / W primary emulsion was slowly added into the cross-linked silica gel in Preparation Example 8 to form an eye area essence. Finally, the eye area essence was subjected to vacuum defoaming treatment, and the vacuum degree was -0.10 MPa.
[0089] Comparative Example 1 Comparative Example 1 Glycerin (3.5wt%), polyglyceryl-10 myristate (1.5wt%), polysorbate (1wt%) and the water-soluble polymer dispersion in Preparation Example 9 were added into deionized water (77.19wt%) in turn, stirred and heated to 85°C. The oil phase components in Preparation Example 9 were added into the above solution, homogenized for 5 min and then cooled by stirring. When the temperature dropped to 45°C, the following were added in turn: bird's nest acid (1wt%), fibronectin (0.01wt%), phenoxyethanol (0.54wt%) and ethylhexylglycerin (0.06wt%). The pH of the emulsion was adjusted to 6-7 using arginine (0.55wt%), and the cooling was continued by stirring until the temperature dropped to 37°C.
[0090] Comparative Example 2 The oil phase components in Preparation Example 10 were slowly added into the D-phase components in Preparation Example 10 under the conditions of room temperature and stirring at 1000r / min, mixed to form a D-phase oil gel, and then the water phase components in Preparation Example 10 were slowly added into the D-phase oil gel, mixed to form an O / W primary emulsion. The O / W primary emulsion was slowly added into the silicone gel in Preparation Example 10, mixed to form an eye essence emulsion. Finally, the eye essence emulsion was subjected to vacuum degassing treatment at a vacuum degree of -0.10Mpa.
[0091] Comparative Example 3 The oil phase components in Preparation Example 11 were slowly added into the D-phase components in Preparation Example 11 under the conditions of room temperature and stirring at 1000r / min, mixed to form a D-phase oil gel, and then the water phase components in Preparation Example 11 were slowly added into the D-phase oil gel, mixed to form an O / W primary emulsion. The O / W primary emulsion was slowly added into the cross-linked silicone gel in Preparation Example 11, mixed to form an eye essence emulsion. Finally, the eye essence emulsion was subjected to vacuum degassing treatment at a vacuum degree of -0.10Mpa.
[0092] Comparative Example 4 The oil phase components in Preparation Example 12 were slowly added into the D-phase components in Preparation Example 12 under the conditions of room temperature and stirring at 1000r / min, mixed to form a D-phase oil gel, and then the water phase components in Preparation Example 12 were slowly added into the D-phase oil gel, mixed to form an O / W primary emulsion. The O / W primary emulsion was slowly added into the cross-linked silicone gel in Preparation Example 12, mixed to form an eye essence emulsion. Finally, the eye essence emulsion was subjected to vacuum degassing treatment at a vacuum degree of -0.10Mpa.
[0093] Comparative Example 5 Under the condition of room temperature and stirring speed of 1000 r / min, the oil phase component in Preparation Example 13 was slowly added into the D phase component in Preparation Example 13, mixed to form a D phase oil gel, and then the water phase component in Preparation Example 13 was slowly added into the D phase oil gel, mixed to form an O / W primary emulsion, and then the O / W primary emulsion was slowly added into the cross-linked silica gel in Preparation Example 13, mixed to form an eye area essence. Finally, when the eye area essence was subjected to vacuum defoaming treatment, the vacuum degree was -0.10 MPa.
[0094] Performance test Test one, the eye area essences prepared in Examples 1-8 and Comparative Examples 1-5 were subjected to stability test under the condition of 50℃ and natural light for 4 weeks, and the appearance was as shown in Table 1. Among them, the appearance photos of Examples 1-3 and Comparative Examples were as shown in Figure 1
[0095] Test two, the eye area essences prepared in Examples 1-8 and Comparative Examples 1-5 were subjected to human patch test according to the human skin patch test in the “Cosmetic Safety Technical Specifications” (2015). The number of test persons was 30. The safety test results were as shown in Table 2.
[0096] Test three, 75 volunteers aged 30-45 years old with dark circles but without allergic diseases were selected and randomly divided into five groups, 15 persons in each group. The five groups of volunteers corresponded to using the eye area essences prepared in Example 2, Comparative Example 1, Comparative Example 3, Comparative Example 4 and Comparative Example 5, respectively. The volunteers were required to apply the same amount of eye area essence around the eyes every day in the morning and evening, and gently massage until absorption, for 28 consecutive days. The control group was selected by self-control. The data tested before the volunteers used the product (0 days) were taken as the control group, and the data tested after 14 days of continuous use of the product and after 28 days of continuous use of the product were taken as the experimental group. Before each test, the testee needed to clean the face in a constant temperature (21±1℃) and constant humidity (50±10% RH) environment for more than 30 minutes. The water content in the keratin layer of the eye area skin was measured by using a skin keratin layer hydration measuring instrument (Moisture Meter SC), and the test results were as shown in Figure 2 and Table 3. The amount of trans-epidermal water loss (TEWL value) of the eye area skin was measured by using a trans-epidermal water measuring instrument (VapoMeter), and the test results were as shown in Figure 3 and Table 4. The elasticity of the eye area skin was measured by using a skin elasticity measuring instrument (ElastiMeter), and the test results were as shown in Figure 4 and Table 5. The L value and b value were measured by using a spectrophotometer (CM-700D), and the ITA° value of the eye area skin was calculated, and the test results were as shown in Figure 5 and Table 6. Each test was tested by the same tester using the same test instrument on each subject, and the measurement area before and after using the product remained consistent. Each test was tested three times on the same subject, and the average value was taken. The statistical analysis software SPSS 25.0 was used for statistical analysis of the data. The measurement data is expressed as mean ± standard deviation, and normal distribution test is performed. If it meets the requirements of normal distribution, the paired sample t test is used for calculation of P value for comparison before and after itself, otherwise the two related sample rank sum test is used for calculation of P value. The above statistical analysis is a two-tailed test, the significance level a is 0.05, and whether the skin parameters before and after using the product have significant difference is analyzed. It should be noted that, Figure 2 , Figure 3 , Figure 4 and Figure 5 The "*" indicates that there is a significant difference in the measured value compared with before use (P<0.05).
[0097] Table 1 Stability test results
[0098] Table 2 Safety test results
[0099] Table 3 Eye skin stratum corneum water content (A.U)
[0100] Table 4 Eye skin transepidermal water loss
[0101] Table 5 Eye skin elasticity (N / m)
[0102] Table 6 Eye skin ITA ° value (°)
[0103] Table 1 and Figure 1It can be seen that the eye essence cream prepared by Examples 1-8 and Comparative Examples 3-5 has high ingredient stability, and the color change is shallow under high temperature and natural light, which proves that the O / W / SI multiple emulsification preparation technology can effectively protect vitamin K2 and bird's nest acid, prevent the inactivation and discoloration of active ingredients under light and high temperature conditions. The eye essence cream prepared by Comparative Example 1 using conventional O / W emulsification technology has poor stability under high temperature and natural light conditions, especially under natural light conditions, the color changes to dark yellow, which not only reduces the bioavailability of vitamin K2 and bird's nest acid, but also affects the appearance of the product. In Comparative Example 2, due to the use of linear polyether modified silicone emulsifier (PEG-10 dimethicone) and hydrophobically modified thickener (lithium montmorillonite dimethyl ammonium), the stability of the eye essence cream is the worst, and a little oil or stratification appears on the surface after 2 weeks of investigation under 50℃, -18℃ and cycle conditions, which seriously affects the use of the product.
[0104] As can be seen from Table 2, when 30 people used the eye essence cream prepared by Comparative Example 1, 2 people had weak red spots within 30 minutes after the spot tester was removed, while no one had red spots when using the eye essence cream prepared by Examples 1-8 and Comparative Examples 2-5. It proves that the product prepared by O / W / SI multiple emulsification technology has better safety.
[0105] Combining Table 3 and Figure 2It can be seen that after 14 days of continuous use of the eye serum cream prepared in Example 2 and after 28 days of continuous use of the eye serum cream prepared in Example 2, the water content of the stratum corneum of the eye skin was increased by 11.76% and 19.80% respectively compared with before use, and the differences were statistically significant (P<0.05). After 14 days of continuous use of the eye serum cream prepared in Comparative Example 1 and after 28 days of continuous use of the eye serum cream prepared in Comparative Example 1, the water content of the stratum corneum of the eye skin was increased by 5.19% and 10.40% respectively compared with before use, therefore, the moisturizing effect of the product prepared by traditional O / W emulsification technology was obviously weaker than that of the product prepared by O / W / SI multiple emulsification technology. After 14 days of continuous use of the eye serum cream prepared in Comparative Example 3 and after 28 days of continuous use of the eye serum cream prepared in Comparative Example 3, the water content of the stratum corneum of the eye skin was increased by 4.04% and 5.33% respectively compared with before use, and the differences were not statistically significant (P>0.05). It is proved that when the eye serum cream does not contain bird's nest acid, the moisturizing effect will be greatly reduced. After 14 days of continuous use of the eye serum cream prepared in Comparative Example 4 and after 28 days of continuous use of the eye serum cream prepared in Comparative Example 4, the water content of the stratum corneum of the eye skin was increased by 9.92% and 19.47% respectively compared with before use. After 14 days of continuous use of the eye serum cream prepared in Comparative Example 5 and after 28 days of continuous use of the eye serum cream prepared in Comparative Example 5, the water content of the stratum corneum of the eye skin was increased by 8.40% and 15.08% respectively compared with before use. It is proved that when the eye serum cream does not contain vitamin K2 or fibronectin, the moisturizing effect is slightly worse than that of the eye serum cream prepared in Example 2. In summary, it can be seen that the use of O / W / SI multiple emulsification technology and the use of vitamin K2, bird's nest acid and fibronectin can significantly increase the water content of the eye skin and have good moisturizing effect.
[0106] In combination with Table 4 and Figure 3It can be seen that after 14 days of continuous use of the eye serum emulsion prepared in Example 2 and after 28 days of continuous use of the eye serum emulsion prepared in Example 2, the amount of transdermal water loss of the eye skin was reduced by 14.13% and 20.77% respectively compared with before use, and the differences were statistically significant (P<0.05). After 14 days of continuous use of the eye serum emulsion prepared in Comparative Example 1 and after 28 days of continuous use of the eye serum emulsion prepared in Comparative Example 1, the amount of transdermal water loss of the eye skin was reduced by 7.68% and 10.29% respectively compared with before use, and the skin barrier function of the eye serum emulsion prepared in Comparative Example 1 was weaker than that of the eye serum emulsion prepared in Example 2. After 14 days of continuous use of the eye serum emulsion prepared in Comparative Example 3 and after 28 days of continuous use of the eye serum emulsion prepared in Comparative Example 3, the amount of transdermal water loss of the eye skin was reduced by 10.30% and 15.23% respectively compared with before use. After 14 days of continuous use of the eye serum emulsion prepared in Comparative Example 4 and after 28 days of continuous use of the eye serum emulsion prepared in Comparative Example 4, the amount of transdermal water loss of the eye skin was reduced by 11.81% and 16.82% respectively compared with before use. After 14 days of continuous use of the eye serum emulsion prepared in Comparative Example 5 and after 28 days of continuous use of the eye serum emulsion prepared in Comparative Example 5, the amount of transdermal water loss of the eye skin was reduced by 7.36% and 8.77% respectively compared with before use, and the differences were not statistically significant (P>0.05). It is proved that when the eye serum emulsion does not contain bird's nest acid or vitamin K2, the skin barrier function decreases, but is still better than that of the eye serum emulsion prepared in Comparative Example 1. When the eye serum emulsion does not contain fibronectin, the skin barrier function decreases seriously, and is even weaker than that of the eye serum emulsion prepared in Comparative Example 1. It can be seen from the above that compared with the eye serum emulsion prepared by traditional O / W emulsification technology, the use of O / W / SI multiple emulsification technology and the use of vitamin K2, bird's nest acid and fibronectin can significantly enhance the skin barrier and have good water locking effect.
[0107] In combination with Table 5 and Figure 4It can be seen that after 14 days of continuous use of the eye serum emulsion prepared in Example 2 and after 28 days of continuous use of the eye serum emulsion prepared in Example 2, the elasticity of the eye skin increased by 12.59% and 23.38% respectively compared with before use, and the differences were statistically significant (P<0.05). After 14 days of continuous use of the eye serum emulsion prepared in Comparative Example 1 and after 28 days of continuous use of the eye serum emulsion prepared in Comparative Example 1, the elasticity of the eye skin increased by 8.04% and 13.43% respectively compared with before use. It is proved that the eye serum emulsion prepared by using traditional emulsifiers has a weaker effect on improving the elasticity of the eye skin than the eye serum emulsion prepared in Example 2. After 14 days of continuous use of the eye serum emulsion prepared in Comparative Example 4 and after 28 days of continuous use of the eye serum emulsion prepared in Comparative Example 4, the elasticity of the eye skin increased by 6.76% and 12.88% respectively compared with before use. After 14 days of continuous use of the eye serum emulsion prepared in Comparative Example 5 and after 28 days of continuous use of the eye serum emulsion prepared in Comparative Example 5, the elasticity of the eye skin increased by 7.99% and 17.30% respectively compared with before use. After 14 days of continuous use of the eye serum emulsion prepared in Comparative Example 3 and after 28 days of continuous use of the eye serum emulsion prepared in Comparative Example 3, the elasticity of the eye skin increased by 3.45% and 8.57% respectively compared with before use, and the differences were not statistically significant (P>0.05). It is proved that when the eye serum emulsion does not contain vitamin K2 or fibronectin, the effect on improving the elasticity of the eye skin decreases compared with the eye serum emulsion prepared in Example 2, but is better than the eye serum emulsion prepared in Comparative Example 1. When the eye serum emulsion does not contain bird's nest acid, the effect on improving the elasticity of the eye skin decreases seriously compared with the eye serum emulsion prepared in Example 2, and is even weaker than the eye serum emulsion prepared in Comparative Example 1. It can be concluded from the above that the O / W / SI multiple emulsification technology and the use of vitamin K2, bird's nest acid and fibronectin can significantly enhance skin elasticity and have good anti-wrinkle effect.
[0108] In combination with Table 6 and Figure 5It can be seen that after 14 days of continuous use of the eye area essence cream prepared in Example 2 and after 28 days of continuous use of the eye area essence cream prepared in Example 2, the ITA° value of the eye area skin increased by 2.80% and 10.93% respectively compared with before use, and the differences were statistically significant (P<0.05). After 14 days of continuous use of the eye area essence cream prepared in Comparative Example 1 and after 28 days of continuous use of the eye area essence cream prepared in Comparative Example 1, the ITA° value of the eye area skin increased by 2.46% and 3.71% respectively compared with before use, and the differences were not statistically significant (P>0.05). It is proved that the traditional emulsifier prepared eye area essence cream has weaker effect on darkening of dark circles than the eye area essence cream prepared in Example 2. After 14 days of continuous use of the eye area essence cream prepared in Comparative Example 3 and after 28 days of continuous use of the eye area essence cream prepared in Comparative Example 3, the ITA° value of the eye area skin increased by 4.28% and 8.81% respectively compared with before use. After 14 days of continuous use of the eye area essence cream prepared in Comparative Example 5 and after 28 days of continuous use of the eye area essence cream prepared in Comparative Example 5, the ITA° value of the eye area skin increased by 2.50% and 8.33% respectively compared with before use. It is proved that when the eye area essence cream does not contain bird's nest acid or fibronectin, the effect of darkening of dark circles is slightly weaker than the eye area essence cream prepared in Example 2, but the effect of darkening of dark circles is still stronger than the eye area essence cream prepared in Comparative Example 1. After 14 days of continuous use of the eye area essence cream prepared in Comparative Example 4 and after 28 days of continuous use of the eye area essence cream prepared in Comparative Example 4, the ITA° value of the eye area skin increased by 0.39% and 4.44% respectively compared with before use, and the differences were not statistically significant (P>0.05). It is proved that when the eye area essence cream does not contain vitamin K2, the effect of darkening of dark circles is greatly reduced. In summary, the use of O / W / SI multiple emulsification technology and the use of vitamin K2, bird's nest acid and fibronectin can significantly increase the ITA° value of the eye area skin, brighten the skin color, and have certain effect on improving dark circles.
[0109] In summary, the O / W / SI multiple emulsification technology, vitamin K2, cystosarcoma and fibronectin can significantly improve the moisture content of the eye skin, have good moisturizing effect, can significantly enhance the skin barrier, have good water locking effect, can significantly enhance the skin elasticity, have good anti-wrinkle effect, can significantly increase the ITA° value of the eye skin, brighten the skin color, have certain effect of improving the dark circles, have certain synergistic effect in improving the problems of the eye skin, have good moisturizing, repairing, anti-wrinkle and dark circle lightening effect. Compared with the eye serum cream prepared by the traditional O / W emulsification technology, the bioavailability of the active substances can be effectively improved, and there is certain advantage in increasing the water content of the skin horny layer and promoting the skin barrier repair. At the same time, the O / W / SI multiple emulsification technology can effectively solve the problems of easy discoloration and inactivation of the active ingredients under high temperature and light conditions, improve the stability of the active ingredients, improve the mildness of the eye serum cream, and make it suitable for the delicate eye skin, so the safety is higher.
[0110] The embodiments of the specific implementation are the preferred embodiments of the present application, not limited to the protection scope of the present application, so: any equivalent changes made according to the structure, shape, principle of the present application should be covered within the protection scope of the present application.
Claims
1. An eye serum, characterized in that, The eye serum comprises a D-phase component, an oil-phase component, an aqueous phase component, and a cross-linked silicone gel; The D-phase component includes: a bio-emulsifier and a first polyol; The oil phase components include: vitamin K2 and non-organosilicone oil; The aqueous phase components include: sialic acid, fibronectin, second polyol, water-soluble polymer, preservative, pH adjuster, and deionized water; The cross-linked silicone gel includes: organosilicon cross-linked polymers, polyether / polyglycerol modified cross-linked organosilicon polymers, and organosilicon oils.
2. The eye serum according to claim 1, characterized in that, Based on the mass percentage of the eye serum, the D-phase component comprises: 0.05-5 wt% bio-emulsifier and 1-10 wt% first polyol; the oil phase component comprises: 0.01-0.1 wt% vitamin K2 and 2-15 wt% non-organosilicone oil; the aqueous phase component comprises: 0.1-2 wt% sialic acid, 0.005-0.05 wt% fibronectin, 1-5 wt% second polyol, 0.1-1 wt% water-soluble polymer, 0.1-1 wt% preservative, 0.5-1.5 wt% pH adjuster and 20-70 wt% deionized water; the cross-linked silicone gel comprises: 0.5-5 wt% organosilicon cross-linked polymer, 0.5-5 wt% polyether / polyglycerol modified cross-linked organosilicon polymer and 25-65 wt% organosilicon oil.
3. The eye serum according to claim 1 or 2, characterized in that, The bio-emulsifier is at least one of Bacillus fermentation products prepared by microbial fermentation and glycolipids; the first polyol is at least one of glycerol, butanediol and 1,3-propanediol; the second polyol is at least one of glycerol, butanediol and 1,3-propanediol.
4. The eye serum according to claim 1 or 2, characterized in that, The non-organosilicone oil is at least one of caprylic / capric triglyceride and dioctyl carbonate; the organosilicone oil is at least one of polydimethylsiloxane and cyclopentadimethylsiloxane.
5. The eye serum according to claim 1 or 2, characterized in that, The water-soluble polymer is at least one of ammonium acryloyldimethyl taurate / VP copolymer, xanthan gum, and hydroxyethyl cellulose; the preservative is at least one of phenoxyethanol, ethylhexylglycerin, chlorphenesin, and p-hydroxyacetophenone; and the pH adjuster is at least one of arginine, triethanolamine, aminomethylpropanol, and sodium hydroxide.
6. The eye serum according to claim 1 or 2, characterized in that, The organosilicon crosslinked polymer has a three-dimensional network structure and is at least one of polydimethylsiloxane / vinyl polydimethylsiloxane crosslinked polymer, divinyl polydimethylsiloxane / polydimethylsiloxane crosslinked polymer, and diphenyl polydimethylsiloxane crosslinked polymer.
7. The eye serum according to claim 1 or 2, characterized in that, The polyether / polyglycerol modified crosslinked organosilicon polymer is at least one of polydimethylsiloxane PEG-10 / 15 crosslinked polymer, polydimethylsiloxane PEG-15 crosslinked polymer, and polydimethylsiloxane / polyglycerol-3 crosslinked polymer.
8. A method for preparing an eye serum as described in any one of claims 1 to 7, characterized in that, include: S1. Prepare the oil phase component, the aqueous phase component, the cross-linked silica gel, and the D phase component; S2. Add the oil phase component to the D phase component and mix well to form a D phase oleogel; S3. Add the aqueous phase component to the D-phase oleogel and mix well to form an O / W primary emulsion; S4. Add the O / W pre-emulsion to the cross-linked silicone gel and mix well to form the eye serum; S5. Perform vacuum defoaming treatment on the eye serum.
9. The method for preparing the eye serum according to claim 8, characterized in that, In step S1, the above-mentioned amount of vitamin K2 is added to the above-mentioned amount of the non-organosilicone oil and mixed to form the oil phase component; the above-mentioned amount of the water-soluble polymer is added to the above-mentioned amount of the second polyol and mixed to form a water-soluble polymer dispersion; the above-mentioned amount of sialic acid is added to the above-mentioned amount of deionized water and mixed to form a sialic acid solution; the pH of the sialic acid solution is adjusted to 6-7 using the above-mentioned amount of pH adjuster, and then the above-mentioned amount of fibronectin, the above-mentioned amount of preservative and the water-soluble polymer dispersion are added to the sialic acid solution and mixed to form the aqueous phase component; the above-mentioned amount of the organosilicon crosslinking polymer and the above-mentioned amount of the polyether / polyglycerol modified crosslinked organosilicon polymer are added to the above-mentioned amount of organosilicon oil and mixed to form the crosslinked silicone gel; the above-mentioned amount of the bio-emulsifier is added to the above-mentioned amount of the first polyol and mixed to form the D phase component.
10. The method for preparing the eye serum according to claim 8, characterized in that, In step S1, when preparing the cross-linked silica gel, the stirring speed is 800-1200 r / min; in step S2, the stirring speed is 800-1200 r / min; in step S3, the stirring speed is 800-1200 r / min; in step S4, the stirring speed is 800-1200 r / min; in step S5, the vacuum degree is between -0.08 MPa and -0.12 MPa. The oil phase component, the aqueous phase component, the cross-linked silicone gel, the D phase component, the D phase oleogel, the O / W colostrum, and the eye serum are prepared at room temperature.