CN113952250B - Stable photo-aging resistant composition and preparation method thereof - Google Patents
Stable photo-aging resistant composition and preparation method thereof Download PDFInfo
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- CN113952250B CN113952250B CN202111288253.XA CN202111288253A CN113952250B CN 113952250 B CN113952250 B CN 113952250B CN 202111288253 A CN202111288253 A CN 202111288253A CN 113952250 B CN113952250 B CN 113952250B
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Abstract
The invention discloses a stable anti-photoaging composition and a preparation method thereof, belonging to the technical field of cosmetic preparation, and the invention provides a stable anti-photoaging composition and a preparation method thereof, wherein the composition comprises the following components: according to the mass ratio (1-10): (1-5): 3:1:2: (4-16): (1-4): 1: (10-20): (30-50) ascorbic acid, superoxide dismutase, triolein, squalol, begonia seed oil, poloxamer 407, PPG-12/SMDI copolymer, hexylene glycol, glycerol, and deionized water; the composition has the advantages of synergistic effect, synergistic stability, multiple ways and omnibearing photo-aging resistance, the high-content photo-aging resistance composition is wrapped in a gel system, and the gel slow-release system enables the effective components to be released slowly, so that the mildness of the product and the skin tolerance are improved, and meanwhile, the long-acting photo-aging resistance effect can be exerted.
Description
Technical Field
The invention relates to a stable anti-photoaging composition and a preparation method thereof, belonging to the technical field of cosmetic preparation.
Background
Aging is an irresistible natural law that often manifests itself visually in a unique morphology, the skin being the first organ. Skin aging causes can be divided into endogenous and exogenous factors. Endogenous factors are mainly natural aging. Exogenous aging is related to our living environment (ultraviolet rays, air pollution, etc.) and living habit (smoking, staying up at night, etc.). Of these, aging of exogenous factors is currently the most hot topic, the "photoaging" monad. Skin photoaging refers to the process of premature aging of skin by damage caused by sunlight or artificially derived ultraviolet radiation in nature. The nature of ultraviolet damaged cells is that photon energy of ultraviolet rays is absorbed by atoms or molecules of the cells, causing a change in the electron energy level state of the atoms, generating a large amount of secondary electrons and free radicals, and thus causing various damage events in the cells. In addition, visible light has a certain pushing effect on the occurrence of skin photoaging. Heat stress generated by IR in sunlight may be involved in the expression of MMPS (matrix metalloproteinases) in the skin and the progression of photoaging of the skin, including disruption of the extracellular matrix proteins inherent to the skin, affecting the formation of elastic fibers in the skin, inducing inflammatory cell infiltration of the skin and oxidative DNA damage of the skin.
Sun protection is one of the simplest and most necessary methods for preventing photoaging of skin. The removal of conventional physical sunscreens, sun protection products and post-sun repair are also important means. In order to achieve higher protection effect, the sun-screening product used in daily life often needs to be added with more physical and chemical sun-screening agents, and the high-content physical sun-screening agents have the problems of whitening, thick skin feel, difficult cleaning and easy pore blocking, and the high-content chemical sun-screening agents have certain irritation to sensitive skin groups. Furthermore, sun protection products are generally directed to blocking or absorbing only the ultraviolet portion, without preventing or repairing ultraviolet and visible light induced skin photoaging.
Vitamins, trace elements, thymine dinucleotide, polyphenols, flavonoids and the like are all the current research data to prove that the essential research results on skin photoaging are achieved, but the stability of the components is often caused in the use process, the phenomena of losing activity and changing color are easy to occur in the use and storage processes, and meanwhile, part of active components have the problems of odor, solubility, irritation and the like, so that the application of the active components in products and the maximization of the effect are limited. The gel slow release technology is one of carrier technologies, and can load various functional components to obtain innovative raw materials which have good transdermal absorbability, high bioavailability, good stability, good compatibility, mildness, no stimulation and benefit for application. How to obtain an anti-aging product with high stability and remarkable effect becomes a hot spot and a difficult point of research.
Disclosure of Invention
In order to solve the problems of poor stability, single action mechanism, inconvenient use, insignificant effect and the like of anti-aging products in the prior art, the invention provides a stable anti-photoaging composition and a preparation method thereof. The problems of poor stability, single action mechanism, inconvenient use, insignificant effect and the like of anti-aging products in the prior art are solved. In addition, the anti-photoaging composition can be conveniently added into various dosage forms of products such as water aqua, essence, cream, facial mask and the like.
The present invention provides a cosmetic composition comprising: 1 to 10 weight parts of ascorbic acid, 1 to 5 weight parts of superoxide dismutase and 2 weight parts of crab seed oil.
In one embodiment of the invention, the cosmetic composition further comprises a stabilizer; the stabilizer comprises one or more of triolein, squalol, stearic acid and p-hydroxyacetophenone.
In one embodiment of the invention, the cosmetic composition further comprises an emulsifier; the emulsifier comprises one or more of poloxamer 407, glyceryl stearate, lecithin and sorbitan stearate.
In one embodiment of the present invention, the cosmetic composition further comprises a humectant comprising one or more of glycerin, hyaluronic acid, squalane.
In one embodiment of the present invention, the cosmetic composition further comprises a bacteriostatic agent and a thickening agent; the bacteriostat comprises one or more of hexanediol, glycerol, p-hydroxyacetophenone and chlorphenicol glycolether; the thickener comprises one or more of PPG-12/SMDI copolymer, xanthan gum, sodium polyacrylate and carbomer.
In one embodiment of the invention, the composition is: mass ratio (1-10): (1-5): 3:1:2: (4-16): (1-4): 1: (10-20): (30-50) ascorbic acid, superoxide dismutase, triolein, squalol, crab apple seed oil, poloxamer 407, PPG-12/SMDI copolymer, hexylene glycol, glycerol and deionized water.
In one embodiment of the invention, the composition is, in mass ratio 6:3:3:1:2:16:4:1:10:50, ascorbic acid, superoxide dismutase, triolein, squalol, begonia seed oil, poloxamer 407, PPG-12/SMDI copolymer, hexanediol, glycerol and deionized water are weighed.
The invention also provides a preparation method of the anti-aging gel, which comprises the following steps:
(1) According to the mass ratio (1-10): (1-5): 3:1:2: (4-16): (1-4): 1: (10-20): (30-50) weighing ascorbic acid, superoxide dismutase, triolein, squalene, crab apple seed oil, poloxamer 407, PPG-12/SMDI copolymer, hexanediol, glycerol and deionized water;
(2) Mixing poloxamer 407, PPG-12/SMDI copolymer, glycerin, hexanediol and 70% deionized water weighed in the step (1) at 500-1000rpm, stirring uniformly, heating to 75-85 ℃, and continuously stirring until completely dissolved;
(3) Adding the triolein, the squalene and the crab seed oil weighed in the step (1) into the gel solution in the step B, uniformly stirring at the rotating speed of 500-1000rpm, and then cooling to 30-40 ℃ to obtain semitransparent viscous gel;
(4) Dissolving the ascorbic acid and the superoxide dismutase weighed in the step (1) in the rest 30% of deionized water, and stirring at a rotating speed of 500-1000rpm until the ascorbic acid and the superoxide dismutase are completely dissolved;
(5) And (3) adding the active substance solution obtained in the step (4) into the gel obtained in the step (3), uniformly stirring at the rotating speed of 1000-1500 rpm, and cooling to room temperature to obtain semitransparent viscous high-content anti-photoaging gel.
In one embodiment of the present invention, the step (1) is that, in mass ratio 7:3:3:1:2:13:3:1:17:50, ascorbic acid, superoxide dismutase, triolein, squalol, begonia seed oil, poloxamer 407, PPG-12/SMDI copolymer, hexylene glycol, glycerol and deionized water.
In one embodiment of the present invention, the step (1) is that, in mass ratio of 6:2:3:1:2:15:2:1:20:48, ascorbic acid, superoxide dismutase, triolein, squalol, begonia seed oil, poloxamer 407, PPG-12/SMDI copolymer, hexylene glycol, glycerol and deionized water.
In one embodiment of the present invention, the step (1) is that, in mass ratio of 6:3:3:1:2:16:4:1:14:50, ascorbic acid, superoxide dismutase, triolein, squalol, begonia seed oil, poloxamer 407, PPG-12/SMDI copolymer, hexylene glycol, glycerol and deionized water.
In one embodiment of the present invention, the step (1) is that, in mass ratio 5:2:3:1:2:16:3:1:18:49, ascorbic acid, superoxide dismutase, triolein, squalol, begonia seed oil, poloxamer 407, PPG-12/SMDI copolymer, hexylene glycol, glycerol, and deionized water.
In one embodiment of the present invention, the step (1) is that, in mass ratio of 10:5:3:1:2:14:2:1:20:42, ascorbic acid, superoxide dismutase, triolein, squalol, begonia seed oil, poloxamer 407, PPG-12/SMDI copolymer, hexylene glycol, glycerol and deionized water.
The invention also provides the anti-aging gel prepared by the method.
The invention also provides the application of the cosmetic composition, the method or the anti-photoaging gel in the preparation of anti-aging products.
In one embodiment of the invention, the application of the anti-photoaging gel in cosmetics can be used as an anti-photoaging active substance to be added into cosmetics to play roles in resisting oxidation, inflammation, whitening, repairing, wrinkle resistance and the like.
In one embodiment of the present invention, the anti-aging product comprises any one of a lotion, an essence, an emulsion, a cream, a spray, a mask, a cream, and a gel.
In one embodiment of the invention, the high-content anti-photoaging gel is applied to various dosage forms of products such as cosmetic water, essence, cream, spray, mask and the like, and the addition amount is preferably 0.1-10% by mass.
Advantageous effects
(1) The method has the advantages that the unstable and highly-irritating ascorbic acid is wrapped in a gel slow-release system consisting of the triolein, the superoxide dismutase, the batyl alcohol and the crab seed oil, and the substances act together to improve the stability of the ascorbic acid, so that the ascorbic acid is slowly released, the mildness of the product and the skin tolerance are improved, and meanwhile, the ascorbic acid can better play a role under the protection.
(2) The non-enzymatic system of ascorbic acid and the enzymatic system of superoxide dismutase cooperate to resist oxygen, inhibit ROS production by UV irradiation and scavenge excessive ROS.
(3) The ascorbic acid can inhibit the activity of tyrosinase and regulate the synthesis of collagen, so that the effects of whitening and resisting wrinkles are achieved, the superoxide dismutase has good affinity as endogenous enzyme, cells can be protected from damage, in addition, the anti-inflammatory effect of the squalol can inhibit erythema caused by UV, the crab seed oil can protect DNA and promote cell repair, and various active components in the composition are synergistic, so that the effect of omnibearing anti-photoaging is achieved.
(4) The prepared anti-photoaging gel can be simply and conveniently directly applied to cosmetics in various dosage forms such as water, essence, emulsion, face cream, facial mask and the like.
Detailed Description
The following examples further illustrate the technical aspects of the present invention, but the scope of the present invention is not limited thereto.
The ascorbic acid (vitamin C) of the present invention is numbered 04092 in China, catalog of used cosmetic raw Material names (2015 edition), and the ascorbic acid referred to in the examples below is ASCOBIC ACID FINE POWDER available from DSM company. Ascorbic acid is a vitamin and natural antioxidant essential to the human body. VC has strong antioxidant activity, can eliminate oxygen free radicals, inhibit lipid peroxidation, and protect skin from free radical damage caused by ultraviolet rays; simultaneously, VC can inhibit the activity of tyrosinase, prevent melanin from generating, and achieve the whitening effect; in addition, VC can regulate the synthesis of collagen, and the collagen is more stable through hydroxylation, so that the support of the epidermis layer is improved, wrinkles are reduced, and the skin is rich in elasticity. However, VC has the problems of unstable property and large irritation while being powerful and comprehensive in efficacy. VC can react with various substances chemically, is easily damaged by oxidants, light, heat, trace heavy metals, fluorescent substances and the like to lose reducing power, and limits the effective utilization rate of VC.
The superoxide dismutase (SOD) disclosed by the invention has the serial number of 01622 in the name catalog of used cosmetics raw materials (2015 edition) in China, and the superoxide dismutase (SOD) related in the following examples is purchased from the Zhongkexin-containing SOD yeast powder, and has the enzyme activity of 50 ten thousand IU/g, good high-temperature stability and acid and alkali resistance. Superoxide dismutase is an antioxidant metalloenzyme widely existing in organisms, and can catalyze superoxide to be converted into oxygen and hydrogen peroxide through disproportionation reaction, so that the purposes of scavenging oxygen free radicals in cells and protecting cells are achieved, and the superoxide dismutase plays an important role in the oxidation and antioxidant balance of organisms. Most of SOD circulating in the market at present has low activity, needs to be stored in a refrigerating way and is easy to inactivate, so that the normal exertion of functions and the application in products are greatly limited. The Chinese kexin technology team creatively solves the problems, prepares the SOD which is safe and mild, stable in property, resistant to high temperature and acid and alkali through the microbial fermentation technology, and can be easily applied to various products.
The TRIOLEIN (TRILEIN) of the present invention has a serial number of 05838 in China (catalog of used cosmetic raw Material names (2015 edition)), and the TRIOLEIN in the following examples is Algapur HSHO microalgae oil purchased from Lubo Co. Triolein is a natural oil with stable properties and silky skin feel, is not easy to oxidize, and is also beneficial to stabilizing other unstable active ingredients such as ascorbic acid.
The invention discloses a shark liver ALCOHOL (BATYL ALCOHOOL), which has the serial number of 05876 in the name catalog of used cosmetic raw materials (2015 edition) in China; the scyllitol referred to in the examples below is Batyl Alcohol 100, available from solar chemistry. The scyllitol is high-carbon alcohol with anti-inflammatory effect, has remarkable inhibiting effect on erythema caused by UV, can improve SPF value of sun-screening product, improve skin feel and increase stability.
The malus spectabilis (CALOPHYLLUM INOPHYLLUM) seed oil (CALOPHYLLUM INOPHYLLUM SEED OIL) of the invention has the serial number of 02736 in the "used cosmetics raw materials name catalog (2015 edition)" of China, and the malus spectabilis seed oil referred to in the following examples is nyanmplung oil malus spectabilis oil purchased from qi Hua Du. The crab seed oil is an organic active oil for preventing photoaging, has the effects of SPF synergy, free radical removal, DNA protection from UVB injury and cell repair promotion, and provides a comprehensive protection and treatment solution from natural sources.
The POLOXAMER 407 (POLOXAMER 407) of the invention has the serial number of 01541 in China 'used cosmetic raw materials name catalog (2015 edition), the PPG-12/SMDI COPOLYMER (PPG-12/SMDI copoler) has the serial number of 00843 in China' used cosmetic raw materials name catalog (2015 edition), and the compound of the POLOXAMER 407 and the PPG-12/SMDI COPOLYMER related in the following examples is purchased from French Polymer experert.
The hexanediol has the serial number of 00004 in the name catalog of used cosmetics raw materials (2015 edition) in China, can be used as an antibacterial agent and provides anti-corrosion and antibacterial effects for a slow-release system; the glycerin has the serial number of 02421 in the name catalog of used cosmetics raw materials (2015 edition) in China, has good moisture absorption and preservation effects, and can be used as a structure improver of poloxamer 407 and PPG-12/SMDI copolymer to improve the viscosity and the moisture preservation performance of a gel system. The hexanediol and glycerin referred to in the examples below were purchased from microphone.
The detection method involved in the following examples is as follows:
detection of ascorbic acid content:
the ascorbic acid content of the samples was tested by high performance liquid chromatography. The liquid phase conditions are as follows: c18 chromatographic column, mobile phase methanol: distilled water (3:7 volume ratio), flow rate 1ML/MIN, detection wavelength 260NM
Calculation of ascorbic acid retention:
and (3) placing the sample at 25 ℃ and 40 ℃ for stability experiments under the illumination condition, testing the ascorbic acid content at 1, 2, 3 and 4 weeks by using high performance liquid chromatography, and obtaining the ascorbic acid retention rate according to the ratio of the content measurement result to the initial ascorbic acid content.
Detection of skin moisture:
the subject needs to sit for 20min under the environment of constant temperature and humidity (room temperature 22+/-2 ℃ and relative humidity 45+/-5%) before testing, and skin moisture is measured and analyzed by using a CM825 skin moisture tester before and after the use of the left and right faces for 3 weeks and 6 weeks.
Detection of skin elasticity:
the subject needs to sit for 20min under the environment of constant temperature and humidity (room temperature 22+/-2 ℃ and relative humidity 45+/-5%) before testing, and skin elasticity is measured and analyzed before using the MPA580 skin elasticity tester for the left face and the right face, after 3 weeks and after 6 weeks.
Mildness test method and evaluation criteria:
the following tests were performed according to the requirements related to the human skin patch test in cosmetic safety Specification (2015 edition): selecting 30 volunteers 18-60 years old meeting test requirements as subjects, and selecting a range of no more than 50mm 2 A plaque test apparatus of about 1mm depth. The samples were placed in plaque test chambers, and plaque test was applied to the back of the subject with hypoallergenic tape, gently pressed with the palm to apply uniformly to the skin for 24 hours. Skin reactions were observed 30min after removal of the subject plaque tester (after disappearance of the indentations), 24h and 48h, respectively, and the skin reactions were observed according to the criteria of table 1, and the observations were recorded. More than 5 subjects with grade 1 skin adverse reaction, or more than 2 subjects with grade 2 skin adverse reaction, or any of grade 1, grade 3 or more than grade 3 epithelium in 30 subjectsAnd when the skin is in adverse reaction, judging that the test object has adverse reaction on the skin of a human body.
TABLE 1 skin response grading Standard for skin seal Patch test
Example 1: anti-photoaging composition and preparation method thereof
The method comprises the following specific steps:
(1) According to the mass ratio of 7:3:3:1:2:13:3:1:17:50, weighing ascorbic acid, superoxide dismutase, triolein, squalol, crab apple seed oil, poloxamer 407, PPG-12/SMDI copolymer, hexanediol, glycerol and deionized water;
(2) Mixing poloxamer 407, PPG-12/SMDI copolymer, glycerin, hexanediol and 70% volume deionized water weighed in the step (1) at a rotating speed of 1000rpm, uniformly stirring, heating to 80 ℃, and continuously stirring until the mixture is completely dissolved to prepare a gel solution;
(3) Adding the triolein, the squalene and the crab apple seed oil weighed in the step (1) into the gel solution obtained in the step (2), uniformly stirring at a rotating speed of 1000rpm, and then cooling to 30 ℃ to obtain semitransparent viscous gel;
(4) Dissolving the ascorbic acid and the superoxide dismutase weighed in the step (1) in the rest 30% of deionized water, and stirring at a rotation speed of 500rpm until the ascorbic acid and the superoxide dismutase are completely dissolved to obtain an active substance solution;
(5) And (3) adding the active substance solution obtained in the step (4) into the semitransparent viscous gel obtained in the step (3), uniformly stirring at a rotating speed of 1500rpm, and cooling to room temperature to obtain semitransparent viscous high-content photoaging-resistant gel 1.
Example 2: anti-photoaging composition and preparation method thereof
The method comprises the following specific steps:
(1) According to the mass ratio of 6:2:3:1:2:15:2:1:20:48, ascorbic acid, superoxide dismutase, triolein, squalol, crab apple seed oil, poloxamer 407, PPG-12/SMDI copolymer, hexanediol, glycerol and deionized water;
(2) Mixing poloxamer 407, PPG-12/SMDI copolymer, glycerin, hexanediol and 70% deionized water weighed in the step (1) at 800rpm, stirring uniformly, heating to 85 ℃, and continuously stirring until the mixture is completely dissolved to prepare a gel solution;
(3) Adding the triolein, the squalene and the crab apple seed oil weighed in the step (1) into the gel solution obtained in the step (2), uniformly stirring at the rotating speed of 800rpm, and then cooling to 40 ℃ to obtain semitransparent viscous gel;
(4) Dissolving the ascorbic acid and the superoxide dismutase weighed in the step (1) in the rest 30% of deionized water, and stirring at a rotation speed of 500rpm until the ascorbic acid and the superoxide dismutase are completely dissolved to obtain an active substance solution;
(5) And (3) adding the active substance solution obtained in the step (4) into the semitransparent viscous gel obtained in the step (3), uniformly stirring at the speed of 1200rpm, and cooling to room temperature to obtain semitransparent viscous high-content photoaging-resistant gel 2.
Example 3: anti-photoaging composition and preparation method thereof
The method comprises the following specific steps:
(1) According to the mass ratio of 6:3:3:1:2:16:4:1:14:50, weighing ascorbic acid, superoxide dismutase, triolein, squalol, crab apple seed oil, poloxamer 407, PPG-12/SMDI copolymer, hexanediol, glycerol and deionized water;
(2) Mixing poloxamer 407, PPG-12/SMDI copolymer, glycerin, hexanediol and 70% volume deionized water weighed in the step (1) at a rotating speed of 1000rpm, uniformly stirring, heating to 75 ℃, and continuously stirring until the mixture is completely dissolved to prepare a gel solution;
(3) Adding the triolein, the squalene and the crab apple seed oil weighed in the step (1) into the gel solution obtained in the step (2), uniformly stirring at a rotating speed of 1000rpm, and then cooling to 35 ℃ to obtain semitransparent viscous gel;
(4) Dissolving the ascorbic acid and the superoxide dismutase weighed in the step (1) in the rest 30% of deionized water, and stirring at 600rpm until the ascorbic acid and the superoxide dismutase are completely dissolved to obtain an active substance solution;
(5) And (3) adding the active substance solution obtained in the step (4) into the semitransparent viscous gel obtained in the step (3), uniformly stirring at the rotating speed of 1400rpm, and cooling to room temperature to obtain semitransparent viscous high-content photoaging-resistant gel 3.
Example 4: anti-photoaging composition and preparation method thereof
The method comprises the following specific steps:
(1) According to the mass ratio of 5:2:3:1:2:16:3:1:18:49, ascorbic acid, superoxide dismutase, triolein, squalol, crab apple seed oil, poloxamer 407, PPG-12/SMDI copolymer, hexanediol, glycerol and deionized water;
(2) Mixing poloxamer 407, PPG-12/SMDI copolymer, glycerin, hexanediol and 70% deionized water weighed in the step (1) at 900rpm, stirring uniformly, heating to 80 ℃, and continuously stirring until the mixture is completely dissolved to prepare a gel solution;
(3) Adding the triolein, the squalene and the crab apple seed oil weighed in the step (1) into the gel solution obtained in the step (2), uniformly stirring at a rotating speed of 700rpm, and then cooling to 40 ℃ to obtain semitransparent viscous gel;
(4) Dissolving the ascorbic acid and the superoxide dismutase weighed in the step (1) in the rest 30% of deionized water, and stirring at 1000rpm until the ascorbic acid and the superoxide dismutase are completely dissolved to obtain an active substance solution;
(5) And (3) adding the active substance solution obtained in the step (4) into the semitransparent viscous gel obtained in the step (3), uniformly stirring at a rotating speed of 1500rpm, and cooling to room temperature to obtain semitransparent viscous high-content photoaging-resistant gel 4.
Example 5: anti-photoaging composition and preparation method thereof
The method comprises the following specific steps:
(1) The mass ratio is 10:5:3:1:2:14:2:1:20:42, weighing ascorbic acid, superoxide dismutase, triolein, squalol, crab apple seed oil, poloxamer 407, PPG-12/SMDI copolymer, hexanediol, glycerol and deionized water;
(2) Mixing poloxamer 407, PPG-12/SMDI copolymer, glycerin, hexanediol and 70% volume deionized water weighed in the step (1) at 900rpm, uniformly stirring, heating to 75 ℃, and continuously stirring until the mixture is completely dissolved to prepare a gel solution;
(3) Adding the triolein, the squalene and the crab apple seed oil weighed in the step (1) into the gel solution obtained in the step (2), uniformly stirring at a rotating speed of 1000rpm, and then cooling to 30 ℃ to obtain semitransparent viscous gel;
(4) Dissolving the ascorbic acid and the superoxide dismutase weighed in the step (1) in the rest 30% of deionized water, and stirring at a rotation speed of 500rpm until the ascorbic acid and the superoxide dismutase are completely dissolved to obtain an active substance solution;
(5) And (3) adding the active substance solution obtained in the step (4) into the semitransparent viscous gel obtained in the step (3), uniformly stirring at the speed of 1300rpm, and cooling to room temperature to obtain semitransparent viscous high-content photoaging-resistant gel 5.
Comparative example:
1. an aqueous solution of 5.32% by mass of ascorbic acid (in terms of the content of ascorbic acid in example 1) was prepared as a control group a.
2. The specific embodiment is the same as example 1, except that the raw materials are adjusted as follows: ascorbic acid, poloxamer 407, PPG-12/SMDI copolymer, hexanediol, glycerol and deionized water, and the specific steps are as follows:
(1) According to 7:13:3:1:17:50, ascorbic acid, poloxamer 407, PPG-12/SMDI copolymer, hexanediol, glycerol and deionized water;
(2) Mixing poloxamer 407, PPG-12/SMDI copolymer, glycerin, hexanediol and 70% volume deionized water weighed in the step (1) at a rotating speed of 1000rpm, uniformly stirring, heating to 80 ℃, and continuously stirring until the mixture is completely dissolved to prepare a gel solution;
(3) Dissolving the ascorbic acid weighed in the step (1) in the rest 30% of deionized water by volume, and stirring at a rotation speed of 500rpm until the ascorbic acid is completely dissolved to obtain an active substance solution;
(4) And (3) adding the active substance solution obtained in the step (3) into the gel solution obtained in the step (2), uniformly stirring at a rotating speed of 1500rpm, and cooling to room temperature to obtain a control group B.
3. The specific embodiment is the same as example 1, except that superoxide dismutase is not added, i.e. according to 7:3:1:2:13:3:1:17:50, ascorbic acid, triolein, squalene, crab apple seed oil, poloxamer 407, PPG-12/SMDI copolymer, hexanediol, glycerol and deionized water are weighed out as a control group C. The method comprises the following specific steps:
(1) According to 7:3:1:2:13:3:1:17:50, weighing ascorbic acid, triolein, squalene, crab apple seed oil, poloxamer 407, PPG-12/SMDI copolymer, hexanediol, glycerol and deionized water;
(2) Mixing poloxamer 407, PPG-12/SMDI copolymer, glycerin, hexanediol and 70% volume deionized water weighed in the step (1) at a rotating speed of 1000rpm, uniformly stirring, heating to 80 ℃, and continuously stirring until the mixture is completely dissolved to prepare a gel solution;
(3) Adding the triolein, the squalene and the crab apple seed oil weighed in the step (1) into the gel solution obtained in the step (2), uniformly stirring at a rotating speed of 1000rpm, and then cooling to 30 ℃ to obtain semitransparent viscous gel;
(4) Dissolving the ascorbic acid weighed in the step (1) in the rest 30% of deionized water by volume, and stirring at a rotation speed of 500rpm until the ascorbic acid is completely dissolved to obtain an active substance solution;
(5) And (3) adding the active substance solution obtained in the step (4) into the semitransparent viscous gel obtained in the step (3), uniformly stirring at a rotating speed of 1500rpm, and cooling to room temperature to obtain a control group C.
4. The specific embodiment is the same as example 1, except that no crab seed oil is added, namely according to 7:3:3:1:13:3:1:17:50, ascorbic acid, superoxide dismutase, triolein, squalol, poloxamer 407, PPG-12/SMDI copolymer, hexylene glycol, glycerol and deionized water were weighed and the prepared gel was used as control group D.
(1) According to 7:3:3:1:13:3:1:17:50, ascorbic acid, superoxide dismutase, triolein, squalol, poloxamer 407, PPG-12/SMDI copolymer, hexanediol, glycerol and deionized water;
(2) Mixing poloxamer 407, PPG-12/SMDI copolymer, glycerin, hexanediol and 70% volume deionized water weighed in the step (1) at a rotating speed of 1000rpm, uniformly stirring, heating to 80 ℃, and continuously stirring until the mixture is completely dissolved to prepare a gel solution;
(3) Adding the triolein, the squalene and the crab apple seed oil weighed in the step (1) into the gel solution obtained in the step (2), uniformly stirring at a rotating speed of 1000rpm, and then cooling to 30 ℃ to obtain semitransparent viscous gel;
(4) Dissolving the ascorbic acid and the superoxide dismutase weighed in the step (1) in the rest 30% of deionized water, and stirring at a rotation speed of 500rpm until the ascorbic acid and the superoxide dismutase are completely dissolved to obtain an active substance solution;
(5) And (3) adding the active substance solution obtained in the step (4) into the semitransparent viscous gel obtained in the step (3), uniformly stirring at a rotating speed of 1500rpm, and cooling to room temperature to obtain a control group D.
Example 6: characterization of anti-photoaging gel Properties
(1) Stability test of anti-aging gels 1 to 5 and gels in comparative examples
The samples prepared in examples 1 to 5 and comparative example were subjected to stability tests at 25℃and 40℃under light conditions, and the ascorbic acid contents were measured by high performance liquid chromatography for 1, 2, 3 and 4 weeks, and the ascorbic acid retention was calculated from the results of the content measurement, and the results are shown in Table 2.
TABLE 2 stability test results
As can be seen from the data in Table 2, the stability test for 4 weeks shows that the aqueous solution of ascorbic acid in the control group A has poor photo and thermal stability, the retention rate of ascorbic acid in the control group A is only about 60% under high temperature and light conditions, the photo and thermal stability of the ascorbic acid gel in the control group B, C, D is obviously improved compared with that in the control group A, the retention rate of ascorbic acid in the control group A is more than 80%, the retention rate of ascorbic acid in the photo-aging resistant gel 1-5 is higher than that in the control group, and the retention rate of ascorbic acid in the control group A is higher than 90% under the conditions of 25 ℃ and 40 ℃. Wherein the ascorbic acid retention of the anti-photoaging gel 1 is highest in several groups, and the ascorbic acid retention is higher than 95% at 25 ℃ and 40 ℃ under the illumination condition.
Experimental results show that after the ascorbic acid is coated by poloxamer 407 and PPG-12/SMDI copolymer in a specific ratio, the light stability and the heat stability are improved, and meanwhile, the stability of the ascorbic acid can be further improved by adding superoxide dismutase, triolein, squalol and crab seed oil. Therefore, the composition and the gelation treatment technology provided by the invention can coordinate and enhance the efficacy, have the function of stabilizing and protecting the ascorbic acid, and can improve the light stability and the heat stability of the ascorbic acid.
(2) Mild test of photo-aging resistant gels 1 to 5 and gels in comparative examples
Detecting according to the mildness method of the anti-photoaging gel, respectively taking 0.02g of control group A, B, C, D and 0.02g of anti-photoaging gel 1-5 into a patch tester cell, applying the patch tester to the back of a subject by using a hypoallergenic adhesive tape, and uniformly applying the patch tester to the skin by using palm light pressure for 24 hours. Skin reactions were observed 30min after removal of the subject plaque tester (after disappearance of the indentations), 24h and 48h, respectively, and the skin reactions were observed according to the criteria of table 1, and the observations were recorded. And when the number of the patients with the skin untoward effect of level 1 is more than 5, or the number of the patients with the skin untoward effect of level 2 is more than 2, or any skin untoward effect of level 1, level 3 or more than level 3 occurs in 30 subjects, judging that the tested object has skin untoward effect on human bodies.
The test results are shown in Table 3.
TABLE 3 results of the irritation test
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Note that: 1 (7) The number of adverse reactions was 1, corresponding to subject number 7
As shown in Table 3, the aqueous solution of the ascorbic acid with the mass fraction of 5.32% has a certain irritation to human skin, and the ascorbic acid is coated by poloxamer 407 and PPG-12/SMDI copolymer to prepare gel with the same concentration, so that the release of the ascorbic acid can be controlled, the irritation of the ascorbic acid can be obviously reduced, and in addition, the addition of superoxide dismutase, triolein, squalol and crab apple seed oil can further improve the mildness of the ascorbic acid. The ascorbic acid is combined with superoxide dismutase, triolein, squalol and crab seed oil according to a specific proportion and subjected to gelation treatment, so that the direct contact of high-concentration ascorbic acid with skin can be avoided, the irritation of the ascorbic acid is obviously reduced, and discomfort such as stinging and the like possibly caused by the ascorbic acid can be effectively avoided.
Example 7: preparation of face cream containing anti-photoaging gel
Examples 1 to 6 show that the photo-aging resistant gel prepared by the formulation of the invention can obtain better effects, and the cream is prepared by taking the photo-aging resistant gel prepared by example 1 as an example, so that the creams prepared by other formulations have the same beneficial effects.
The method comprises the following specific steps:
(1) The mass ratio is 10:5:5:70:10, weighing glycerol, cetyl alcohol, microcrystalline wax, deionized water and photo-aging resistant gel 1;
(2) Mixing and stirring the glycerol, the microcrystalline wax and the deionized water weighed in the step (1) at a rotating speed of 1000rpm, heating to 80 ℃, and continuously stirring until the glycerol, the microcrystalline wax and the deionized water are completely dissolved;
(3) Adding the cetyl alcohol weighed in the step (1) into the solution obtained in the step (2), uniformly stirring at a rotating speed of 1000rpm, and then cooling to 30 ℃;
(4) Adding the anti-photoaging gel 1 weighed in the step (1) into the solution obtained in the step (3), and stirring at 500rpm until the gel is completely dissolved to obtain the cream containing 10% of the mass fraction of the anti-photoaging gel prepared in the example 1.
Detecting the effect of the prepared face cream:
skin photoaging is clinically characterized by rough skin texture, dryness, increased wrinkles, sagging, lack of elasticity, irregular pigmentation, and the like, so the invention comprehensively evaluates the efficacy of the photoaging-resistant gel by measuring skin moisture and elasticity. 40 female volunteers were selected, aged between 25 and 45 years, and the subjects were asked to use a face cream containing 10% by mass of the anti-photoaging gel prepared in example 1 on the left face, to use a blank control without the anti-photoaging gel cream added on the right face, and to follow up once a day before and 3 and 6 weeks before and 3 times in total, the follow up being the same time during the day.
Before the test, the subject needs to sit for 20min under the environment of constant temperature and humidity (room temperature 22+/-2 ℃ and relative humidity 45+/-5%), and then the skin moisture and elasticity of the left and right faces before use, after 3 weeks and after 6 weeks are measured and analyzed by using a CM825 skin moisture tester and an MPA580 skin elasticity tester. The results are shown in tables 4 and 5, wherein table 4 shows the moisturizing effect data after different time periods of the left and right faces using different samples, and table 5 shows the skin elasticity data after different time periods of the left and right faces using different samples.
Table 4 moisture test data for left and right faces at different times
TABLE 5 different time elasticity test data for left and right faces
As shown in Table 4, the water content of the skin of the left and right faces gradually increased with the increase of the use time, and the water content of the skin of the left face was higher than that of the right face of the sample containing the photo-aging resistant gel prepared in example 1, which indicates that the photo-aging resistant composition gel prepared in the invention can increase the water content of the horny layer of the skin, and sufficient water can make the skin show a full and smooth healthy state.
As shown in Table 5, as the service time increases, the R2 and R5 values of the left and right faces increase, and the R2 and R5 values of the left face are higher than those of the right face using the blank control sample after the left face uses example 1, and are closer to 1, which indicates that the photo-aging resistant composition gel prepared by the invention can effectively improve skin elasticity. The skin moisture and elasticity test data are combined, so that the skin care composition has the beneficial effect of remarkable photo-aging resistance.
Experiments prove that the cream containing at least 10% of the mass fraction of the anti-photoaging gel prepared by the embodiment 1 can have beneficial effects.
In conclusion, the photoaging resistant composition gel has the advantages of good stability, low irritation, high bioavailability, remarkable effect, convenience in application and the like.
While the invention has been described with reference to the preferred embodiments, it is not limited thereto, and various changes and modifications can be made therein by those skilled in the art without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (3)
1. A cosmetic composition, characterized in that it comprises: 1-10 parts by weight of ascorbic acid, 1-5 parts by weight of superoxide dismutase, 2 parts by weight of crab apple seed oil, 3 parts by weight of triolein, 1 part by weight of squalene, 13 parts by weight of poloxamer 407, 3 parts by weight of PPG-12/SMDI copolymer, 1 part by weight of hexanediol, 10-20 parts by weight of glycerol and 30-50 parts by weight of deionized water; the preparation method of the cosmetic composition comprises the following steps:
(1) According to the mass ratio (1-10): (1-5): 3:1:2:13:3:1: (10-20): (30-50) weighing ascorbic acid, superoxide dismutase, triolein, squalene, crab apple seed oil, poloxamer 407, PPG-12/SMDI copolymer, hexanediol, glycerol and deionized water;
(2) Mixing poloxamer 407, PPG-12/SMDI copolymer, glycerin, hexanediol and 70% deionized water weighed in the step (1) at a rotating speed of 500-1000rpm, uniformly stirring, heating to 75-85 ℃, and continuously stirring until the mixture is completely dissolved to prepare a gel solution;
(3) Adding the triolein, the squalene and the crab apple seed oil weighed in the step (1) into the gel solution obtained in the step (2), uniformly stirring at a rotating speed of 500-1000rpm, and then cooling to 30-40 ℃ to obtain semitransparent viscous gel;
(4) Dissolving the ascorbic acid and the superoxide dismutase weighed in the step (1) in the rest 30% of deionized water, and stirring at a rotating speed of 500-1000rpm until the ascorbic acid and the superoxide dismutase are completely dissolved to obtain an active substance solution;
(5) And (3) adding the active substance solution obtained in the step (4) into the semitransparent viscous gel obtained in the step (3), uniformly stirring at a rotating speed of 1000-1500 rpm, and cooling to room temperature to obtain the cosmetic composition.
2. Use of the cosmetic composition of claim 1 for the preparation of an anti-aging product.
3. The use according to claim 2, wherein said anti-aging product comprises any one of lotions, essences, emulsions, creams, sprays, masks, ointments, gels.
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