Disclosure of Invention
The invention aims to provide a water-oil biphase smoothing toner added with blue copper peptide and a preparation method thereof.
The technical scheme of the invention is as follows: the water-oil biphase smoothing toner added with the blue copper peptide comprises the following components in percentage by weight: 5 to 30 percent of humectant, 0.1 to 5 percent of preservative, 0.01 to 1.0 percent of tripeptide-1 copper, 1 to 30 percent of skin conditioning agent, 0.001 to 2 percent of penetration enhancer, 0.01 to 5 percent of pH buffering agent, 1 to 20 percent of oil phase and the balance of water.
The water-oil biphase skin softening water added with the blue copper peptide comprises the following components in percentage by weight: 8 to 20 percent of humectant, 0.5 to 3 percent of preservative, 0.05 to 0.5 percent of tripeptide-1 copper, 3 to 20 percent of skin conditioning agent, 0.1 to 1 percent of penetration enhancer, 0.05 to 3 percent of pH buffering agent, 5 to 15 percent of oil phase and the balance of water.
In the water-oil biphase skin softening water added with the blue copper peptide, the humectant comprises the following components in percentage by weight: 1 to 10 percent of 1,3 butanediol, 0.1 to 2 percent of 1,3 propanediol, 0.5 to 5 percent of glycerin, 0.001 to 1 percent of sodium hyaluronate and 0.01 to 2 percent of panthenol.
In the water-oil biphase skin softening water added with the blue copper peptide, the preservative comprises the following components in percentage by weight: 2.0 to 4.0 percent of 1, 2-pentanediol, 0.30 to 1.2 percent of 1, 2-hexanediol and 0.02 to 0.15 percent of ethylhexyl glycerol.
In the water-oil biphase skin softening water added with the blue copper peptide, the skin conditioner comprises the following components in percentage by weight: 0.05 to 5 percent of malto-oligosaccharin, 0.01 to 2 percent of tetrahydropalmatine carboxylic acid, 20.001 to 2 percent of biological gum, 0.05 to 3 percent of tetrandra root extract, 0.001 to 2 percent of calcium pantetheine sulfonate, 0.01 to 2 percent of glyceroglycoside, 50.0001 to 1 percent of palmitoyl tripeptide, 20.0001 to 1 percent of hexapeptide and 80.0001 to 1 percent of acetyl hexapeptide.
In the water-oil biphase smoothing toner added with the blue copper peptide, the pH buffering agent comprises the following components in percentage by weight: citric acid 0.001-1% and sodium citrate 0.001-1%.
In the water-oil biphase skin softening water added with the blue copper peptide, the penetration enhancer comprises the following components in percentage by weight: 0.001-1% of inositol and 0.001-1% of bis-diethoxydiglycol cyclohexane 1, 4-dicarboxylic acid ester.
In the water-oil biphase skin softening water added with the blue copper peptide, the oil phase comprises the following components in percentage by weight: isononyl isononanoate 0.5-3.0%, methyl trimethicone 0.2-2.0%, hydrogenated poly (C6-14 olefin) 0.5-5%, squalane 0.1-2%, hexyldecanol 0.01-1%, bisabolol 0.01-1%, N-palmitoyl hydroxyproline cetyl ester 0.01-1%, stearic acid 0.01-1%, brassinosteroids 0.001-1% and phytosterol/octyldodecanol lauroyl glutamate 0.01-1%.
A preparation method of water-oil biphase smoothing toner added with blue copper peptide comprises the following steps:
a. uniformly mixing water, 1,3 butanediol, 1,3 propylene glycol, glycerol and sodium hyaluronate, heating to 70-80 ℃, stirring and cooling to 50-60 ℃, and adding preservative and panthenol while stirring until cooling to 40-45 ℃ to obtain a product A;
b. sequentially adding maltooligosaccharide glucoside, tetrahydropyrimidine carboxylic acid, biological gum-2, tetrandra root extract, tripeptide-1 copper and pH buffer into the product A, regulating the pH to 5.5-6.5, uniformly stirring, and cooling to 30-35 ℃ to obtain a product B;
c. sequentially adding pantetheine calcium sulfonate, glyceroglycosides, palmitoyl tripeptide-5, hexapeptide-2, acetyl hexapeptide-8 and penetration enhancer into the product B, stirring uniformly, standing, cooling to room temperature to obtain a water phase, wherein the pH value of the water phase is 5.5-6.5;
d. taking an oil phase which is uniformly mixed, wherein the mass ratio of the water phase to the oil phase is 80-99: 1 to 20, and obtaining the finished product.
In the preparation method, in the step a, the cooling speed is 0.5-0.8 ℃/min, and the stirring speed is 150-250 r/min.
Compared with the prior art, the invention has the beneficial effects that:
the invention provides a water-oil biphase skin softening water added with blue copper peptide, which adopts a water-oil biphase form, wherein a water phase and an oil phase are mixed according to a specific proportion, the water phase is immediately supplemented with water, the oil phase is permanently locked, and the water phase and the oil phase are preferably composed of components, wherein the oil phase ratio can reach 20%, the water-oil phase layering speed is high, and the limit is clear.
The specific oil phase component selected by the invention adopts synthetic esters, low viscosity silicone oil and direct-linked alkane as main components, and the preferable proportion is 0.5-3.0% isononyl isononanoate, 0.2-2.0% methyl trimethyl silicone and 0.5-5% hydrogenated poly (C6-14 olefin). The composition and the proportion of the grease with three different structures provide balanced oily feel and excellent stability. The specific grease structure and proportion have small interfacial tension, are easy to spread out on the water surface, have large difference between the water and oil coefficients of the water phase, are quick to layer, have less foam and have clear oil-water interface.
According to the invention, the long carbon chain alkyl glycol composition is adopted as an antiseptic system, and is added in a specific proportion, and three alkyl glycols with different carbon chain lengths are preferably combined, so that the dosage of the whole antiseptic can be further reduced, an excellent antiseptic effect is achieved, the irritation of the conventional antiseptic to the skin is reduced to the greatest extent, and the antiseptic is suitable for skin sensitive people. The optimized preservative system has good compatibility with a pH buffering agent in the skin softening water, does not influence the pH of the system, can ensure the content of the blue copper peptide to the greatest extent, prevents copper ions from degrading, and effectively improves the bioactivity of the blue copper peptide. Through high temperature and light acceleration experiment investigation, the stability of the appearance, smell and blue copper peptide content of the skin softening water is good. Meanwhile, the optimal antiseptic system has large difference of water-oil distribution coefficients with oil phase components, is applied to the double-phase smoothing toner, so that the water-oil double-phase interface of the smoothing toner is clear, and the oil-water layer can be rapidly layered after shaking, and has good long-term storage stability.
In addition, the skin-friendly lipid component squalane and plant sterol grease are added into the oil phase, so that the skin adhesion of the blue copper peptide skin softening water can be improved, the brick wall structure of a skin barrier is supplemented, the skin-friendly lipid component squalane and plant sterol grease can be used for repairing a sebum membrane and a cuticle barrier under the combined action of the skin conditioner, such as tetramethyl pyrimidine carboxylic acid, pantetheine calcium sulfonate and the like, skin water and oil double-supplementing, and a myo-base water supplementing channel is opened, the penetration of the myo-ethanol and bis-diethoxydiglycol cyclohexane 1, 4-dicarboxylic ester penetration enhancer in the water phase to the deep skin is facilitated, meanwhile, the grease sealing effect can be further improved, the action time of the blue copper peptide in the water phase is prolonged, the blue copper peptide penetration promoting performance is improved, and the water-oil double-phase system can cooperate with the biological efficacy of the blue copper peptide; the blue copper peptide can play better roles of repairing, anti-wrinkle, tightening, relieving and the like in a skin softening water system.
The invention also provides a preparation method of the skin softening water, which has the advantages of simple operation and easy production, and is beneficial to the stability and efficacy exertion of the blue copper peptide; and the uniformity of the effective components is ensured by controlling the temperature and the stirring time.
Detailed Description
The invention is further illustrated by the following examples, which are not intended to be limiting.
The water-oil biphase smoothing toner added with the blue copper peptide comprises the following components in percentage by weight: 5 to 30 percent of humectant, 0.1 to 5 percent of preservative, 0.01 to 1.0 percent of tripeptide-1 copper, 1 to 30 percent of skin conditioning agent, 0.001 to 2 percent of penetration enhancer, 0.01 to 5 percent of pH buffering agent, 1 to 20 percent of oil phase and the balance of water.
The humectant comprises the following components in percentage by weight: 1 to 10 percent of 1,3 butanediol, 0.1 to 2 percent of 1,3 propanediol, 0.5 to 5 percent of glycerin, 0.001 to 1 percent of sodium hyaluronate and 0.01 to 2 percent of panthenol.
The preservative comprises the following components in percentage by weight: 2.0 to 4.0 percent of 1, 2-pentanediol, 0.30 to 1.2 percent of 1, 2-hexanediol and 0.02 to 0.15 percent of ethylhexyl glycerol.
The skin conditioning agent comprises the following components in percentage by weight: 0.05 to 5 percent of malto-oligosaccharin, 0.01 to 2 percent of tetrahydropalmatine carboxylic acid, 20.001 to 2 percent of biological gum, 0.05 to 3 percent of tetrandra root extract, 0.001 to 2 percent of calcium pantetheine sulfonate, 0.01 to 2 percent of glyceroglycoside, 50.0001 to 1 percent of palmitoyl tripeptide, 20.0001 to 1 percent of hexapeptide and 80.0001 to 1 percent of acetyl hexapeptide.
The pH buffering agent comprises the following components in percentage by weight: citric acid 0.001-1% and sodium citrate 0.001-1%.
The penetration enhancer comprises the following components in percentage by weight: 0.001-1% of inositol and 0.001-1% of bis-diethoxydiglycol cyclohexane 1, 4-dicarboxylic acid ester.
The oil phase comprises the following components in percentage by weight: isononyl isononanoate 0.5-3.0%, methyl trimethicone 0.2-2.0%, hydrogenated poly (C6-14 olefin) 0.5-5%, squalane 0.1-2%, hexyldecanol 0.01-1%, bisabolol 0.01-1%, N-palmitoyl hydroxyproline cetyl ester 0.01-1%, stearic acid 0.01-1%, brassinosteroids 0.001-1% and phytosterol/octyldodecanol lauroyl glutamate 0.01-1%.
The preparation method of the skin softening lotion comprises the following steps:
a. uniformly mixing water, 1,3 butanediol, 1,3 propylene glycol, glycerol and sodium hyaluronate, heating to 70-80 ℃, stirring and cooling to 50-60 ℃, and adding preservative and panthenol while stirring until cooling to 40-45 ℃ to obtain a product A; the cooling speed is 0.5-0.8 ℃/min, and the stirring speed is 150-250 r/min.
b. Sequentially adding maltooligosaccharide glucoside, tetrahydropyrimidine carboxylic acid, biological gum-2, tetrandra root extract, tripeptide-1 copper and pH buffer into the product A, regulating the pH to 5.5-6.5, uniformly stirring, and cooling to 30-35 ℃ to obtain a product B;
c. sequentially adding pantetheine calcium sulfonate, glyceroglycosides, palmitoyl tripeptide-5, hexapeptide-2, acetyl hexapeptide-8 and penetration enhancer into the product B, stirring uniformly, standing, cooling to room temperature to obtain a water phase, wherein the pH value of the water phase is 5.5-6.5;
d. taking an oil phase which is uniformly mixed, wherein the mass ratio of the water phase to the oil phase is 80-99: 1 to 20, and obtaining the finished product.
Example 1:
the water-oil biphase smoothing toner added with the blue copper peptide comprises the following components in percentage by weight: humectant, preservative, tripeptide-1 copper 0.2%, skin conditioner, penetration enhancer, pH buffer, oil phase, and water.
The humectant comprises the following components in percentage by weight: 5% of 1, 3-butanediol, 0.5% of 1, 3-propanediol, 1% of glycerol, 0.05% of sodium hyaluronate and 1% of panthenol.
The preservative comprises the following components in percentage by weight: 3% of 1, 2-pentanediol, 1% of 1, 2-hexanediol and 1% of ethylhexyl glycerol.
The skin conditioning agent comprises the following components in percentage by weight: 2% of maltooligosaccharide glucoside, 0.5% of tetrahydropyrimidine carboxylic acid, 0.8% of biological gum-2, 2% of tetrandra extract, 1.2% of calcium pantetheine sulfonate, 1.5% of glyceroglycoside, 50.05% of palmitoyl tripeptide, 20.02% of hexapeptide and 0.07% of acetyl hexapeptide-8.
The pH buffering agent comprises the following components in percentage by weight: citric acid 0.01% and sodium citrate 0.07%.
The penetration enhancer comprises the following components in percentage by weight: 0.1% inositol and 0.15% bis-diethoxydiglycol cyclohexane 1, 4-dicarboxylate.
The oil phase comprises the following components in percentage by weight: isononyl isononanoate 3%, methyl trimethicone 1%, hydrogenated poly (C6-14 olefins) 1%, squalane 1%, hexyldecanol 0.01%, bisabolol 0.02%, N-palmitoyl hydroxyproline cetyl ester 0.02%, stearic acid 0.02%, brassinosteroids 0.02%, phytosterol/octyldodecanol lauroyl glutamate 0.01%
The preparation method of the skin softening lotion comprises the following steps:
the method comprises the following steps:
a. uniformly mixing water, 1,3 butanediol, 1,3 propylene glycol, glycerol and sodium hyaluronate, heating to 75 ℃, stirring and cooling to 55 ℃, wherein the cooling speed is 0.6 ℃/min, adding preservative and panthenol while stirring, and the stirring speed is 200r/min until the temperature is reduced to 43 ℃, thus obtaining a product A;
b. sequentially adding maltooligosaccharide glucoside, tetrahydropyrimidine carboxylic acid, biological gum-2, radix stephaniae tetrandrae extract, tripeptide-1 copper and pH buffer into the product A, adjusting the pH to 6, uniformly stirring, and cooling to 33 ℃ to obtain a product B;
c. sequentially adding pantetheine calcium sulfonate, glyceroglycosides, palmitoyl tripeptide-5, hexapeptide-2, acetyl hexapeptide-8, bis-diethoxy diglycol cyclohexane 1, 4-dicarboxylic acid ester and inositol into the product B, uniformly stirring, standing, and cooling to room temperature to obtain a water phase;
d. taking an oil phase which is uniformly mixed, wherein the mass ratio of the water phase to the oil phase is 95:5, mixing to obtain a finished product.
According to the formulations in table 1, the skin softening water of example 1 and comparative examples 1 to 5 was prepared as a test sample according to the method of example 1, and performance test was performed.
Table 1 raw materials table for different test samples
1. Stability test:
the stability was measured by placing example 1 and comparative examples 1 to 5 at 45℃and 25℃and storing under the same light conditions and observing the initial state, the color at 2 weeks and the pH at 4 weeks of each test sample, and the test results are shown in Table 2.
TABLE 2 stability test results for different test samples
As is clear from the results of the above table, the color and pH of example 1 were stable under different conditions, whereas the effect of example 1 was not achieved in comparative examples 1 to 5.
2. Water-oil separation layer comparison
Samples prepared in example 1 and comparative examples 1 to 5 were placed in a 100mL measuring cylinder with a stopper and shaken up and down at the same speed for 30 times, and left to stand for observing the delamination speed of the water-oil phase, recording the time of complete delamination of the water-oil phase, recording the interface definition after 5 minutes, and whether there was a phenomenon of oil droplet wall built-up or not, to evaluate the water-oil phase, and the results are shown in table 3.
TABLE 3 comparison of the Water-oil separation of different test samples
It can be seen that the water-oil dual-phase smoothing toner prepared in example 1 has high water-oil layer layering speed after shaking, clear oil-water interface and no wall hanging phenomenon. While comparative examples 1 to 5 did not achieve the effect of example 1.
2. Human efficacy test:
a total of 60 female volunteers 35-45 years old were enrolled, and the skin status of 30 volunteers in each group was similar.
Volunteer screening criteria: the volunteer's face was required to be sensitive skin (passing lactic acid stinging test), and exhibited symptoms of skin lack of water, redness, local fever, etc., and the skin on one side of the face was dehydrated rate of trans-epidermal water loss TEWL in the cheek region>12g/h/m 2 The skin barrier is damaged and the eyes have macroscopic wrinkles.
The blue copper peptide skin softening lotion of example 1 and comparative example 5 was used twice daily for four weeks after each morning and evening face wash, respectively, with no other functional skin care product used. Skin test was performed on volunteers before use, 14 days, and 42 days, and the test values were averaged. The detection indexes comprise: skin moisture content, skin moisture loss, skin elasticity, skin thickness, skin wrinkles and skin color.
Skin moisture content skin stratum corneum moisture content was measured using a skin moisture meter corneometer cm 825;
skin moisture loss the skin transepidermal water loss rate was measured using a skin moisture loss meter TewameterTM 300;
skin elasticity the skin elasticity tester cutmeterdutamp a580 was used to measure skin elasticity;
skin thickness was measured by using an EUB-4 wig ultrasonic scanner produced by HITACHI, with a 7.5MHz linear probe, and focusing at an adjustable depth of 4-5 mm.
The detection results are shown in Table 4.
TABLE 4 human body test conditions of different test samples
(. Times. Shows significant differences (p < 0.05) in measured values compared to the product before use)
From the results, the skin softening water of comparative example 5 has certain effects of moisturizing and increasing skin elasticity, but the effect is relatively weak compared with the oil phase added in example 1, so that the oil phase of the skin softening water of the invention is helpful for the efficacy exertion of blue copper peptide, and has remarkable effects of moisturizing and moisturizing, delaying aging and increasing skin elasticity.
The skin softening water containing the blue copper peptide has the advantages that compared with the oil phase added in the comparative example 5, the skin thickness increasing effect of the example 1 is stronger than that of the comparative example 5, the oil phase and the water phase have synergistic effect, and the skin softening water has remarkable effects of slowing down skin sensitivity and repairing skin damage barriers and reducing skin redness.
Skin color and skin wrinkles were tested on the volunteer population using example 1.
The skin color adopts VISIA-CR to collect facial images and analyze skin color;
skin wrinkles facial image acquisition and skin wrinkles analysis were performed using Primos-CR.
The results of the test of red Pi Fufan (VISIA-CR) are shown in FIG. 1.
The greater the skin color a value, the redder the skin color (indicating a significant difference in measured values, p <0.05, compared to before sample use).
As can be seen from fig. 1, compared to before the sample was used:
the skin color a values of the test areas were significantly reduced by 2.86% after 14 days using the sample of example 1;
after 42 days using the sample of this example 1, the skin color a value of the test area was significantly reduced by 8.85%;
the results of the skin wrinkles (Primos-CR) -canthus wrinkles are shown in fig. 2.
The smaller the Ra value of the wrinkles, the more improved the skin wrinkles (x means a significant difference in measured values compared to before sample use, p < 0.05).
As can be seen from fig. 2, compared to before the sample was used:
after 14 days using the sample of this example 1, the Ra value of skin wrinkles in the corner of the eye was significantly reduced by 9.38%;
after 42 days using the sample of this example 1, the Ra value of skin wrinkles in the corner of the eye was significantly reduced by 11.17%;
in conclusion, the skin softening water containing the blue copper peptide has remarkable effects on skin redness and skin wrinkles, and the effects of repairing skin barriers and resisting wrinkles are shown.