CN114983841A - Water-in-oil peony sun block without silicone oil and preparation method thereof - Google Patents
Water-in-oil peony sun block without silicone oil and preparation method thereof Download PDFInfo
- Publication number
- CN114983841A CN114983841A CN202210677575.1A CN202210677575A CN114983841A CN 114983841 A CN114983841 A CN 114983841A CN 202210677575 A CN202210677575 A CN 202210677575A CN 114983841 A CN114983841 A CN 114983841A
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- sunscreen
- carbonate
- sun
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- A61K8/922—Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof of vegetable origin
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Abstract
The invention discloses a water-in-oil peony sun block emulsion without silicone oil and a preparation method thereof, belonging to the technical field of cosmetics; the sunscreen emulsion comprises the following components in parts by mass: 18.02-23.2 parts of sun-screening agent, 1-2.2 parts of emulsifier, 0.01-0.45 part of thickening agent, 0.01-1 part of film-forming agent, 0.1-2 parts of silica, 20-80 parts of solvent and 0.04-22 parts of ester-alkane mixture, wherein the ester-alkane mixture consists of diethylhexyl carbonate, dioctyl carbonate, C12-15 alcohol benzoate and C9-12 alkane; the sunscreen milk provided by the invention does not contain silicone oil, and can avoid the damage effect of the silicone oil on human skin and the environment; meanwhile, the sunscreen cream provided by the invention has fresh skin feeling and extremely low anaphylactic reaction rate, can effectively inhibit grease secretion and reduce water loss on the skin, and has a high SPF value; in addition, the preparation method of the sunscreen emulsion provided by the invention is simple and convenient to operate.
Description
Technical Field
The invention belongs to the technical field of cosmetics, and particularly relates to water-in-oil peony sun block emulsion without silicone oil and a preparation method thereof.
Background
In recent years, domestic and foreign researches find that the skin is mainly damaged by various external environment pressure factors: dry air, drastic changes in air temperature, bacteria, viruses, air pollution and light pollution and damage, etc., wherein the result of light damage will be sunburn, color-sinking and photoaging of the skin. When the skin is excessively exposed to ultraviolet rays, epidermal cells are damaged, tyrosinase is activated, pigment synthesis is accelerated, the moisturizing function of the skin is damaged, the skin becomes dry, elastic fibers in the dermis are damaged, and fine wrinkles are generated. Under strong irradiation, skin inflammation and burning can be caused, and severe people can cause skin cancer, so that sun protection is an essential part for protecting the skin of a human body, and the selection of sun protection products is particularly important.
The sunscreen products are generally divided into oil-in-water sunscreen and water-in-oil sunscreen, the water-in-oil sunscreen is poor in water resistance and is not suitable for people working outdoors for a long time, the water-in-oil sunscreen is strong in water resistance and has a high-efficiency sunscreen effect both indoors and outdoors, but most of the water-in-oil sunscreen products on the market are mainly silicone oil systems in order to achieve a thin skin feeling, and certain harm to human bodies is caused by neglecting the silicone oil. The silicone oil belongs to nonpolar oil, has strong permeation, and some skin-sensitive people can have the symptoms of skin redness and itching when using the sunscreen product of the silicone oil system, thereby not only not protecting the skin, but also damaging the skin. And advocate environmental protection now, some commonly used sun-screening agents on the market have certain harmful effects on their nature too, according to the research, there are about 6-14000 tons of sun-screening agents to wash and enter coral reef area each year, thousands of sun-screening products contain two most threatening chemical substances, namely ethylhexyl methoxycinnamate, benzophenone-3, these two sun-screening factors, absorb the ultraviolet ray, make the coral reef take place the whitening reaction, benzophenone-3 will prevent the growth of baby coral, to several different coral species are poisonous in the laboratory test, cause the coral to bleach at lower temperature, and reduce their adaptability to climate change.
At present, no research is made on a direction of creating a water-in-oil peony sun block which is friendly to human skin and environment and is beautiful and green and does not contain silicone oil in cosmetics.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide the sun block which does not contain silicone oil, is environment-friendly and is friendly to human skin and the preparation method thereof.
In order to achieve the purpose, the invention adopts the technical scheme that: the water-in-oil peony sun block emulsion free of silicone oil comprises the following components in parts by mass: 18.02-23.2 parts of sun-screening agent, 1-2.2 parts of emulsifier, 0.01-0.45 part of thickening agent, 0.01-1 part of film-forming agent, 0.1-2 parts of silica, 20-80 parts of solvent and 0.04-22 parts of ester-alkane mixture; the mixture of esters and alkanes consists of diethylhexyl carbonate, dioctyl carbonate, C12-15 alcohol benzoate and C9-12 alkane.
The esterane mixture is adopted to replace the conventional silicone oil in the water-in-oil peony sunscreen milk without the silicone oil, so that the damage of the silicone oil to human skin and the environment can be avoided, the effect of the obtained sunscreen agent can be better than that of the conventional silicone oil by combining the four components, and the sunscreen agent can achieve lower anaphylactic reaction rate, higher oil secretion inhibition rate and less percutaneous water loss. Specifically, diethylhexyl carbonate has extremely low viscosity and high spreadability, has good solubilization on crystal active substances, and can well disperse the sunscreen agent, so that the prepared sunscreen lotion has fresh and cool skin feel; the dicaprylyl carbonate is a novel emollient, has extremely dry and comfortable skin feel and good spreadability, has an effect comparable to that of volatile silicone oil, has good solubility to a sunscreen agent, and can reduce the greasy feel of the prepared sunscreen cream; the C12-15 alcohol benzoate has excellent solubility to the sunscreen agent, so that the prepared sunscreen cream has fresh and cool skin feeling and is not sticky; the C9-12 alkane is derived from high-purity alkane of plant raw materials, belongs to nonpolar oil, has fresh and cool skin feel, obvious smooth feel and extremely strong spreadability, has skin feel similar to silicone oil, and can reduce the greasy feel of the sunscreen cream; the invention can achieve the effect which can not be obtained by single use by combining and using the four components.
As a preferred embodiment of the sun-blocking emulsion, the mass ratio of the diethylhexyl carbonate, the dioctyl carbonate, the C12-15 alcohol benzoate and the C9-12 alkane is diethylhexyl carbonate: dioctyl carbonate: c12-15 alcohol benzoates: c9-12 alkyl ═ 0.01 to 4: (0.01-6): (0.01-6): (0.01-6).
As a preferred embodiment of the sun-blocking emulsion, the mass ratio of the diethylhexyl carbonate, the dioctyl carbonate, the C12-15 alcohol benzoate and the C9-12 alkane is diethylhexyl carbonate: dioctyl carbonate: c12-15 alcohol benzoates: c9-12 alkyl ═ 1.8-2.2: (1.8-2.2): (1.8-2.2): (2.6-3.4).
When the mass ratio of the diethyl hexyl carbonate, the dioctyl carbonate, the C12-15 alcohol benzoate and the C9-12 alkane is diethyl hexyl carbonate: dioctyl carbonate: c12-15 alcohol benzoates: c9-12 alkyl ═ 1.8-2.2: (1.8-2.2): (1.8-2.2): (2.6-3.4), the obtained sunscreen lotion had the best refreshing skin feeling, and the proportion of volunteers who felt refreshing was 99%.
As a preferred embodiment of the sun-screening cream, the sun-screening cream further comprises the following components in parts by mass: 0.12 to 0.6 portion of antioxidant, 0.1 to 1.83 portions of skin conditioner, 0.1 to 0.5 portion of preservative and 0.01 to 0.05 portion of chelating agent.
As a preferred embodiment of the sunscreen of the present invention, the sunscreen agent includes a plant sunscreen agent and a non-plant sunscreen agent; the plant sunscreen agent comprises peony seed oil and peony fermentation liquor, and the non-plant sunscreen agent comprises at least one of titanium dioxide, isoamyl p-methoxycinnamate, bis-ethylhexyloxyphenol methoxyphenyl triazine, ethylhexyl salicylate and phenyl benzimidazole sulfonic acid.
As a preferred embodiment of the sunscreen emulsion of the present invention, the mass ratio of the plant sunscreen agent to the non-plant sunscreen agent is (0.02-1.2): (18-22).
According to the invention, the plant sunscreen agent and the non-plant sunscreen agent are selected for compounding, and the existence of the plant sunscreen agent can assist the non-plant sunscreen agent to increase the sun protection index; meanwhile, the selected sunscreen agents are all green, green and environment-friendly sunscreen agents which are friendly to skin, mild and non-irritant and beautiful. Wherein the titanium dioxide is treated by stearic acid and aluminum hydroxide and replaces the conventional titanium dioxide treated by silicon; isoamyl p-methoxycinnamate, the molecular weight of which is 192.21 and the use amount of the regulatory limit is 10 percent, is a substitute of ethylhexyl methoxycinnamate; the bis-ethylhexyloxyphenol methoxyphenyl triazine is a novel broad-spectrum ultraviolet absorbent, has the molecular weight of 627.8, mainly absorbs the ultraviolet with the wavelength of 343nm and 310-; ethylhexyl salicylate with molecular weight of 250.34 belongs to UVB sunscreen agent, mainly absorbs ultraviolet ray with wavelength of 280-340nm, and the limit amount is 5%; phenylbenzimidazole sulfonic acid, a water-soluble UVB sunscreen, has a molecular weight of 274.3, absorbs primarily ultraviolet light at a wavelength of 280-320nm, in a regulated amount of 8% (based on the acid). Through the combined action of the plant sunscreen agent and different types of non-plant sunscreen agents, medium-long wave ultraviolet rays can be effectively absorbed, and a remarkable sunscreen effect is achieved.
As a preferred embodiment of the sunscreen emulsion of the present invention, the emulsifier comprises at least one of polyglycerol emulsifier, span, tween and liquid crystal emulsifier; the thickener comprises disteardimonium hectorite; the film forming agent comprises at least one of VP/VA copolymer, acrylic acid (ester)/ethylhexyl acrylate copolymer, acrylic acid (ester)/dimethylaminoethyl methacrylate copolymer and polyamide-8; the solvent comprises at least one of water and ethanol.
As a preferred embodiment of the sunscreen emulsion of the present invention, the emulsifier includes polyglycerin-3 diisostearate and sorbitan isostearate; the thickener comprises disteardimonium hectorite; the film former comprises a VP hexadecene copolymer; the solvent includes water and ethanol.
As a preferred embodiment of the sunscreen emulsion of the present invention, the antioxidant comprises at least one of tocopherol acetate, carnosine, and tetrahydro-methyl-pyrimidine carboxylic acid; the skin conditioner comprises at least one of arginine, epigallocatechin gallate glucoside (EGCD); the preservative comprises at least one of sodium chloride and p-hydroxyacetophenone; the chelating agent comprises at least one of EDTA-2Na, sodium citrate and sodium gluconate.
As a preferred embodiment of the sunscreen emulsion of the present invention, the antioxidant comprises tocopherol acetate, carnosine and tetrahydro-methyl-pyrimidine-carboxylic acid; the skin conditioner comprises arginine and epigallocatechin gallate glucoside; the preservative comprises sodium chloride and p-hydroxyacetophenone; the chelating agent comprises sodium gluconate.
In addition, the invention provides a preparation method of the sunscreen emulsion, which comprises the following steps:
(1) grinding the raw material of the phase B until the granularity is 30-60 meshes, adding the phase A which is heated and dissolved in advance, grinding and mixing uniformly;
(2) adding a C phase which is stirred and activated into a gel state in advance into the system which is ground and uniformly mixed in the step (1), adding a D phase after homogenizing, heating and stirring, adding a small amount of E phase aqueous solution for multiple times while stirring, homogenizing and cooling after the addition is finished;
(3) adding the F phase and the G phase which are dissolved in advance into the system cooled in the step (2), uniformly stirring, then adding the H phase, homogenizing and filtering to obtain the sun-block emulsion;
the phase A is isoamyl p-methoxycinnamate, bis-ethylhexyloxyphenol methoxyphenyl triazine, ethylhexyl salicylate and phenylbenzimidazole sulfonic acid; the phase B is diethyl hexyl carbonate, dioctyl carbonate, C12-15 alcohol benzoate, C9-12 alkyl tocopheryl acetate, peony seed oil, titanium dioxide, silica, polyglycerol-3 diisostearate and sorbitan isostearate; the phase C is disteardimonium hectorite; the phase D is a VP/hexadecene copolymer; the phase E is water, glycerol, butanediol, sodium chloride, p-hydroxyacetophenone and sodium gluconate; the F phase is water, peony fermentation liquor, tetrahydro-methyl pyrimidine carboxylic acid, epigallocatechin gallate glucoside and carnosine; the G phase is arginine; the H phase is ethanol.
As a preferred embodiment of the production method of the present invention, the mass part of water in the F phase in the sunscreen milk is 1.8 to 2.2 mass parts.
As a preferable embodiment of the preparation method of the present invention, the temperature of the phase A dissolved by raising the temperature in the step (1) is 60 to 70 ℃, the temperature of the phase A dissolved by raising the temperature in the step (2) is 70 to 80 ℃, and the temperature after lowering the temperature is 40 to 45 ℃.
As a preferred embodiment of the preparation method of the present invention, in the step (2), the homogenization time for adding into the D phase after homogenization is 2-5 minutes, the homogenization speed is 600-800r/min, and the homogenization for homogenization and temperature reduction is medium-high speed homogenization 3-5 minutes, wherein the homogenization speed is 800-1000 r/min; the homogenization time in the step (3) is 0.5-1.5 minutes, and the homogenization speed is 400-600 r/min.
As a preferable embodiment of the preparation method of the present invention, in the step (3), the mesh number of the filter cloth for filtration is 200 mesh.
Compared with the prior art, the invention has the beneficial effects that:
firstly: the sunscreen milk provided by the invention does not contain silicone oil, and can avoid the damage effect of the silicone oil on human skin and the environment;
secondly, the method comprises the following steps: the sunscreen cream provided by the invention has fresh and cool skin feeling and extremely low anaphylactic reaction rate, can effectively inhibit grease secretion and reduce water loss through skin, and has a higher SPF value;
thirdly, the steps of: the preparation method of the sunscreen emulsion provided by the invention is simple and convenient to operate.
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to specific examples.
Examples 1 to 7
Examples 1-7 provide a sunscreen having the composition shown in table 1, with the parts by mass of the components being filled in table 1, but the total parts by mass of the overall formulation being 100 parts, so that the balance in the table represents the supplemental formulation to 100 parts; the emulsifier is polyglycerol-3 diisostearate and sorbitan isostearate which are compounded according to the mass ratio of 2.5:1, the thickener is disteardimonium hectorite, the film forming agent is VP/hexadecene copolymer, the humectant is glycerol and butanediol which are compounded according to the mass ratio of 1:1.5, and the chelating agent is sodium gluconate.
Table 1: formulation tables for sunscreen emulsions of examples 1-7
The preparation method of examples 1 to 7 is as follows:
(1) grinding the raw material of the phase B until the granularity is 30-60 meshes, adding the phase A which is preheated to 65 ℃ for dissolution, grinding and mixing uniformly;
(2) adding a C phase which is stirred and activated in advance to form a gel state into the system which is ground and mixed uniformly in the step (1), homogenizing for 3.5 minutes at the speed of 700r/min, adding a D phase raw material, heating to 75 ℃, stirring, adding a small amount of E phase aqueous solution for multiple times, stirring while emulsifying uniformly, homogenizing for 4 minutes at the speed of 900r/min after the addition is finished, and cooling to 42 ℃ while stirring at the speed of 45r/min after the uniform stirring;
(3) adding a pre-dissolved F phase and a pre-dissolved G phase into the system cooled in the step (2), uniformly stirring, adding an H phase, homogenizing at the speed of 500r/min for 1 minute, and filtering with a 200-mesh filter cloth after each index is qualified to obtain the sun-block emulsion;
the phase A is isoamyl p-methoxycinnamate, bis-ethylhexyloxyphenol methoxyphenyl triazine, ethylhexyl salicylate and phenylbenzimidazole sulfonic acid; the phase B is diethyl hexyl carbonate, dioctyl carbonate, C12-15 alcohol benzoate, C9-12 alkyl, tocopherol acetate, peony seed oil, titanium dioxide, silica and an emulsifier; the phase C is a thickening agent; the phase D is a film forming agent; the phase E is water, glycerol, butanediol, sodium chloride, p-hydroxyacetophenone and sodium gluconate; the phase F is water, peony fermentation liquor, tetrahydro-methyl pyrimidine carboxylic acid, EGCG and carnosine; the G phase is arginine; the H phase is ethanol; wherein the amount of water in the F phase is 2 parts by mass.
Comparative examples 1 to 11
Comparative examples 1 to 11 of the present invention provide a sunscreen having the composition shown in table 2, in which the components are filled in parts by mass in table 2, but the total parts by mass of the entire formulation is 100 parts, so that the balance in the table represents a supplementary formulation up to 100 parts; the components other than the silicone oil were completely the same as in examples 1 to 7, and the preparation process was also completely the same as in examples 1 to 7 except that the silicone oil was used as a part of the B phase instead of the corresponding mixture of the esteranes.
Table 2: formulation of sunscreen emulsions of comparative examples 1-11
Effect example 1
Effect example of the invention the refreshing degree of the sunscreen emulsions obtained in examples 1 to 7 and comparative examples 1 to 11 was investigated;
the test method comprises the following steps: recruiting 200 volunteers of different ages, cleaning the two arms with clear water, sucking excessive water with a non-scrap water-absorbing dry paper towel, sitting for 5 minutes under the conditions that the ambient temperature is 20-22 ℃ and the humidity is 40-60%, smearing 0.5g of a test sample on the corresponding position on the arm, evaluating the skin feeling, and calculating the percentage of the corresponding selected number of people, wherein the percentage of the cleaness is 100 percent (the number of the selected test sample/the total number of people); the test results are shown in table 3;
table 3: test Table for the cleanability of sunscreen emulsions obtained in examples 1 to 7 and comparative examples 1 to 11
As can be seen from Table 3, when the sunscreen emulsion obtained by the technical scheme of the invention has excellent cleanability, the percent of cleanability is more than 82%, even can reach 99%, and compared with the results of comparative example 1, the ester alkane mixture in the invention can effectively replace the conventional silicone oil, and the percent of cleanability is equivalent to or even higher; as can be seen from examples 1-4, when the mass ratio of the four components in the mixture of ester and alkane is not changed, but the mass parts in the sunscreen milk are changed, the obtained freshness is different; it can be seen from examples 1 and 5-6 that when the total amount of the mixture of the esterases is the same, the mass ratio of the four components is changed, and the effect on the percentage of freshness is also exerted, wherein the percentage of freshness is most preferable when the mass ratio of diethylhexyl carbonate, dioctyl carbonate, C12-15 alcohol benzoate and C9-12 alkane is 2:2:2: 3; as can be seen from example 1 and comparative examples 1 to 8, when one or more of the components of the mixture of esteranes is/are reduced and replaced by the corresponding silicone oil, the refreshing effect of the resulting product is markedly reduced, in a range of 17.17 to 60.61%; as can be seen from example 1 and comparative example 9, when the total parts by mass of the mixture of the ester alkanes is not changed, but the compounding ratio of the components in the mixture of the ester alkanes is not within the range given in the present invention, the freshness of the obtained product is also significantly reduced; as can be seen from example 1 and comparative example 10, when the addition amount of the ester-alkane mixture is further increased, the refreshing feeling of the product is not improved, but rather, the refreshing feeling is deteriorated; as can be seen from example 1 and comparative example 11, when the components in the mixture of esteranes were replaced with similar components, no comparable effect could be achieved.
Effect example 2
According to the effect example of the invention, a patch test is adopted to explore the potential possibility of adverse reaction of human skin caused by the sun-screening milk obtained in examples 1-7 and comparative examples 1-11;
1. subject selection:
1) selecting 18-60 years volunteers meeting experimental requirements as subjects
2) The subject was not selected as the one having the following condition
(1) Those taking antihistamines for nearly one week or immunosuppressive agents within nearly one month
(2) In the last two months, the part to be tested is applied with any anti-inflammatory drug
(3) The subject suffering from inflammatory dermatosis is not cured clinically
(4) Insulin-dependent diabetic patients
(5) Patients suffering from asthma or other chronic respiratory diseases undergoing therapy
(6) Patients receiving anticancer chemotherapy within 6 months
(7) Patients with immunodeficiency or autoimmune disease
(8) Lactating or pregnant women
(9) Bilateral mastectomy and bilateral underarm lymph node resection
(10) The judgment of the test result is influenced by scar, pigment, atrophy, nevus flammeus or other flaws on the skin to be tested
(11) Participating in other clinical trial researchers
(12) Those with high constitutional sensitivity
2. The test method comprises the following steps:
1) selecting at least 30 persons to participate in the test according to the inclusion criteria of the subject;
2) the selected area is not more than 50mm 2 And qualified spot test equipment with the depth of about 1 mm. The test substance is placed in the chamber of the plaque tester in an amount of about 0.020g to about 0.025g (solid or semi-solid) or about 0.020mL to about 0.025mL (liquid). The test substances were the products prepared in examples 1 to 7 and comparative examples 1 to 11, and the control group was a blank control (without any substance). Applying the spot test device with the test substance on the back of the subject with hypoallergenic tapeThe curved part of the forearm is gently pressed with the palm to apply it on the skin for 24 h.
3) The skin reactions were observed according to the standard of table 4 30min (after disappearance of the indentation), 24h and 48h after removal of the test article plaque test device, respectively, and the observation results were recorded.
Table 4: skin reaction grading standard of skin closed patch test
3. And (3) testing results:
record patch test results as shown in table 5;
table 5: patch test result table (the total number of people in the test is 30)
As can be seen from Table 5, 30 people have no obvious stimulation in the sun-screening and breast spot-blocking patch test result prepared by the technical scheme of the invention, in the comparative example, the higher the content of the contained silicone oil is, the stronger the stimulation is, wherein the patch test result of a pure silicone oil system (comparative example 1) is the most serious, 10 reaction grades 1 appear in 0.5h, and 4 reaction grades 2 appear; it can also be seen from the data of example 1 and comparative examples 10 and 11 that further addition of the mixture of ester alkanes or replacement of components in the mixture of ester alkanes with other similar components can cause some irritation to the product.
Effect example 3
The effect examples of the present invention explore the oil control ability of the sunscreen emulsions obtained in examples 1 to 7 and comparative examples 1 to 11; measuring the transparency of the oil absorption adhesive tape after absorbing sebum to obtain the skin surface grease amount; the specific test method comprises the following steps: 190 volunteers with oily or mixed skin are selected and aged 20-Between 35 years of age, they were randomly divided into 19 groups of 10 people each, each group being individually coated with a different test sample, one of which served as a blank and was not coated with any product. Cleaning forehead with alkaline soap-based facial cleanser, cleaning forehead with clear water, sucking water with non-scrap water-absorbing dry paper towel, sitting at 20-22 deg.C and 40-60% humidity for 30min to prevent drinking water and beverage, keeping relaxed and not touching forehead, testing oil secretion at different positions on forehead with oil probe SM815 of CK tester, measuring for 3 times, taking average value as initial value, and taking (2.0 + -0.1) mg/m 3 Uniformly coating a used sample on a designated area of the forehead by using a silica gel finger stall, respectively measuring the sebum secretion amount within 1 hour and 6 hours after the sample is coated and statically seated, measuring for 3 times by taking different positions, averaging, calculating the inhibition rate of the skin surface grease secretion, and evaluating the test result. The CK tester oil content probe SM815 is used for detecting the skin oil content, and the smaller the measured value is, the lower the skin oil content is; inhibition rate [ (after use-before use)/before use]100% of the total weight; the test results are shown in table 6;
table 6: oil control test result table
As can be seen from table 6, the sunscreen lotion obtained by the technical scheme of the present invention has an effective oil control effect, the inhibition rate on oil is above 27.84% at 1 hour, and the inhibition rate on oil is above 24.19% at 6 hours, that is, the oil control effect equivalent to that of the silicone oil system in comparative example 1 can be achieved under the condition that the addition amount of the ester-alkane mixture in the silicone oil-free system adopted by the present invention is very small (example 4); it can be seen from example 1 and comparative example 1 that when the amount of the ester-alkane mixture is the same as that of the silicone oil, the oil control effect of the product obtained in example 1 is significantly better than that of the product obtained in comparative example 1, wherein the oil inhibition rate of example 1 is increased by 13.00% and 28.70% respectively compared with that of comparative example 1 at 1 hour and 6 hours, and the data also shows that the durability of the oil control effect of the invention is better than that of the silicone oil system.
Effect example 4
Effect example of the present invention, the skin barrier repair effect of the sunscreen emulsions obtained in examples 1 to 7 and comparative examples 1 to 11 was studied, and the skin barrier repair effect of the test sample was evaluated by continuously using the test product for 28 days by volunteers under normal conditions, and measuring the TEWL value of the skin water loss through the surface by probe analysis of the CK apparatus, and the specific test method: selecting 30 volunteers, washing with clear water to remove oil and dust on arms in an environment with a temperature of 20-22 deg.C and a humidity of 40-60%, sitting still for 30min, no drinking water or beverage, relaxing the mood of the volunteers, exposing the arms, and avoiding touching the arms, measuring with a CK test instrument probe 3 times at different positions in the measurement areas of the sample application side and the blank control side before the test samples are used, respectively taking the average value as the initial value of the sample application side and the control side, recording as D0, then applying the corresponding test samples in the designated area, completely covering each measurement area, applying once in the morning, continuously applying for 28 days, measuring 3 times at different positions in the measurement areas of the sample application side and the blank control side, respectively taking the average value as the measurement values of the sample application side and the control side, recording as D28, and comparing the percutaneous moisture loss TEWL values of each test group, calculating the change rate, wherein the change rate is [ (after use-before use)/before use ]. 100%; the test results are shown in table 7;
table 7: percutaneous water loss test data table
From the experimental data in table 7, the sunscreen lotion obtained by the technical scheme of the present invention can significantly reduce the moisture loss through skin, while the higher the silicone oil content in comparative examples 1 to 8, the poorer the effect of reducing the moisture loss through skin, which fully indicates that silicone oil has certain irritation to human skin.
Effect example 5
Effect examples of the present invention study SPF values of sun-screening milks obtained in examples 1 to 7 and comparative examples 1 to 11; coating the sunscreen cosmetic on a special adhesive tape according to the property that the ultraviolet absorbent and the screening agent in the sunscreen cosmetic can block ultraviolet rays, irradiating the special adhesive tape with ultraviolet rays with different wavelengths, measuring the absorbance value of a sample, and directly evaluating the sunscreen effect according to the measured value; the specific test method comprises the following steps: and repeatedly coating the sun-proof sample on a quartz plate with accurate thickness by using a full-automatic coating platform and a coater to obtain a plurality of sun-proof sample coatings with good reproducibility and accurate coating film thickness. The comparative thickness of the coating film is 5 microns; measuring the absorption curve of the coating sample by using an ultraviolet-visible spectrophotometer, and recording the absorption value between 290 nanometers and 400 nanometers; simulating sunlight irradiation by using an HPA skin beautifying lamp to coat a sample, wherein the lamp source energy is 6.7 milliwatts per square centimeter, and the irradiation dose is equivalent to the sunlight irradiation dose of 31 degrees of north latitude at summer noon for 1 hour; measuring a sample coating absorption curve by using an ultraviolet-visible spectrophotometer after the irradiation is finished, substituting the measured value into an ISO2443 calculation formula, and calculating the SPF value and the PA value of the sample; the test results are shown in table 8;
table 8: sunscreen capability test result table of sunscreen emulsion
From table 8, it can be found that the sunscreen emulsion prepared by the technical scheme of the invention has excellent sunscreen performance, the SPF value is greater than 41.6, and PA + + +.
Finally, it should be noted that the above embodiments are intended to illustrate the technical solutions of the present invention and not to limit the scope of the present invention, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications and equivalent substitutions can be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (10)
1. The water-in-oil peony sun block free of silicone oil is characterized by comprising the following components in parts by mass: 18.02-23.2 parts of sun-screening agent, 1-2.2 parts of emulsifier, 0.01-0.45 part of thickening agent, 0.01-1 part of film-forming agent, 0.1-2 parts of silica, 20-80 parts of solvent and 0.04-22 parts of ester-alkane mixture;
the mixture of ester and alkyl is composed of diethylhexyl carbonate, dioctyl carbonate, C12-15 alcohol benzoate and C9-12 alkyl.
2. The suncare cream of claim 1, wherein the mass ratio of diethylhexyl carbonate, dioctyl carbonate, C12-15 alcohol benzoate, and C9-12 alkane is diethylhexyl carbonate: dioctyl carbonate: c12-15 alcohol benzoates: c9-12 ═ c.01-4: (0.01-6): (0.01-6): (0.01-6).
3. The sunscreen according to claim 2 wherein the mass ratio of diethylhexyl carbonate, dioctyl carbonate, C12-15 alcohol benzoate and C9-12 alkane is diethylhexyl carbonate: dioctyl carbonate: c12-15 alcohol benzoate: c9-12 alkyl ═ 1.8-2.2: (1.8-2.2): (1.8-2.2): (2.6-3.4).
4. The suncare milk of claim 1, further comprising the following components in parts by mass: 0.12 to 0.6 portion of antioxidant, 0.1 to 1.83 portions of skin conditioner, 0.1 to 0.5 portion of preservative and 0.01 to 0.05 portion of chelating agent.
5. The suntan emulsion of claim 1, wherein the sunscreens include plant sunscreens and non-plant sunscreens; the plant sunscreen agent comprises peony seed oil and peony fermentation liquor, and the non-plant sunscreen agent comprises at least one of titanium dioxide, isoamyl p-methoxycinnamate, bis-ethylhexyloxyphenol methoxyphenyl triazine, ethylhexyl salicylate and phenyl benzimidazole sulfonic acid.
6. The suntan lotion of claim 5, wherein the mass ratio of plant sunscreens to non-plant sunscreens is (0.02-1.2): (18-22).
7. The sun-block emulsion according to claim 1, wherein the emulsifier comprises at least one of polyglycerol emulsifier, span, tween, liquid crystal emulsifier; the thickener comprises disteardimonium hectorite; the film forming agent comprises at least one of VP/VA copolymer, acrylic acid (ester)/ethylhexyl acrylate copolymer, acrylic acid (ester)/dimethylaminoethyl methacrylate copolymer and polyamide-8; the solvent comprises at least one of water and ethanol.
8. The suncare milk of claim 4, wherein the antioxidant comprises at least one of tocopherol acetate, carnosine, and tetrahydromethylpyrimidine carboxylic acid; the skin conditioner comprises at least one of arginine, epigallocatechin gallate glucoside; the preservative comprises at least one of sodium chloride and p-hydroxyacetophenone; the chelating agent comprises at least one of EDTA-2Na, sodium citrate and sodium gluconate.
9. A process for the preparation of a sun-screen according to any of claims 1 to 8, comprising the steps of:
(1) grinding the raw material of the phase B until the granularity is 30-60 meshes, adding the phase A which is heated and dissolved in advance, grinding and mixing uniformly;
(2) adding a C phase which is stirred and activated into a gel state in advance into the system which is ground and uniformly mixed in the step (1), adding a D phase after homogenizing, heating and stirring, adding a small amount of E phase aqueous solution for multiple times while stirring, homogenizing and cooling after the addition is finished;
(3) adding the F phase and the G phase which are dissolved in advance into the system cooled in the step (2), uniformly stirring, then adding the H phase, homogenizing and filtering to obtain the sun-block emulsion;
the phase A is isoamyl p-methoxycinnamate, bis-ethylhexyloxyphenol methoxyphenyl triazine, ethylhexyl salicylate and phenylbenzimidazole sulfonic acid; the phase B is diethyl hexyl carbonate, dioctyl carbonate, C12-15 alcohol benzoate, C9-12 alkyl tocopheryl acetate, peony seed oil, titanium dioxide, silica, polyglycerol-3 diisostearate and sorbitan isostearate; the phase C is disteardimonium hectorite; the phase D is a VP/hexadecene copolymer; the phase E is water, glycerol, butanediol, sodium chloride, p-hydroxyacetophenone and sodium gluconate; the F phase is water, peony fermentation liquor, tetrahydro-methyl pyrimidine carboxylic acid, epigallocatechin gallate glucoside and carnosine; the G phase is arginine; the H phase is ethanol.
10. The method according to claim 9, wherein the temperature of the phase A dissolved by heating in the step (1) is 60 to 70 ℃, the temperature of the phase A dissolved by heating in the step (2) is 70 to 80 ℃, and the temperature after cooling is 40 to 45 ℃.
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| CN116211720A (en) * | 2023-02-08 | 2023-06-06 | 广州海龟爸爸生物科技有限公司 | Child sun cream containing transparent zinc oxide and preparation method thereof |
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Denomination of invention: A silicone oil free water in oil peony sunscreen and its preparation method Effective date of registration: 20231008 Granted publication date: 20230627 Pledgee: Guotou Taikang Trust Co.,Ltd. Pledgor: Meichulai (Hangzhou) Cosmetics Co.,Ltd. Registration number: Y2023980060101 |
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