A solid composition for emulsification and its preparation method and application

Abstract

The present invention discloses an emulsified solid composition and a preparation method and application thereof, belonging to the technical field of skin care. The emulsified solid composition comprises the following raw materials in parts by weight: 0.1-5.0 parts of fermented rice, 0.7-3.0 parts of solid particles, wherein the specific surface area of ​​the solid particles is 150-190 m 2 / g, the solid particles are selected from at least one of dimethyl silylated silica, methyl silylated silica, silica, cellulose, polylactic acid, polyvinyl alcohol, silicon dioxide and aluminosilicate. The solid composition for emulsification can be used as emulsified solid particles of Pickering emulsion to prepare a stable emulsified emulsion, and is particularly suitable for oil-in-water emulsion.

Description

Technical Field

[0001] The present invention relates to the technical field of skin care, in particular to a solid composition for emulsification and a preparation method and application thereof. Background Art

[0002] Ultraviolet rays (UV) are an important cause of skin problems. UV can be divided into UV-A (320-400nm), UV-B (280-320nm) and UV-C (100-280nm) according to different wavelengths. Different wavelengths cause different damage to the skin. UV-A can penetrate the surface of the skin and act on the dermis. Therefore, UV-A can easily cause skin aging (wrinkles, sagging, etc.); UV-B acts on the surface of the skin and is the main cause of sunburn. In addition, long-term exposure to UV-B will increase the incidence of skin cancer. UV-C is used for sterilization and disinfection. Due to the effect of the ozone layer, UV-C is not common in the natural environment.

[0003] In daily life, sunscreen cosmetics are a common means of sun protection. With the deepening of skin science research, there are reports that sunscreens have the risk of transdermal absorption, which may cause damage to the skin. Therefore, for people with sensitive skin, there are very few sunscreen cosmetics to choose from.

[0004] Pickering emulsion is an emulsion stabilized by solid particles rather than traditional surfactants. Pickering emulsions have attracted attention for their excellent stability and diverse applications, including cosmetics, pharmaceuticals, and food. In a Pickering emulsion, solid particles are dispersed in the oil phase or the water phase. When the two phases are mixed, the particles migrate to the oil-water interface and adsorb on the interface to form a barrier, which can be physical (a layer of particles) or chemical (interaction between particles and the liquid phase), thereby helping to stabilize the emulsion. Unlike the surfactants used in traditional emulsions, Pickering emulsions rely on solid particles to stabilize the oil-water mixture. These particles adsorb at the oil-water interface to form a protective layer, thereby stabilizing the emulsion. The principle is as follows Figure 1 shown.

[0005] In a Pickering emulsion, the solid particles used to stabilize the emulsion can be inorganic (such as silica gel, clay or metal oxides) or organic (such as cellulose or polymers). The size, shape and surface characteristics of these particles will affect the stability and properties of the emulsion.

[0006] At present, people have used the emulsification properties of solid particles to develop water-in-oil Pickering emulsions for use as sunscreen emulsions, reducing the risk of traditional emulsifiers causing damage to the skin. However, water-in-oil sunscreen emulsions have the problem of being thick and greasy on the skin. In oil-in-water emulsions, it is difficult to achieve a stable emulsification effect by using solid particles alone, and there is currently no stable water-in-oil Pickering emulsion. Summary of the invention

[0007] In order to solve the above technical problems, the present invention provides a solid emulsified composition, which can be used as an emulsifier in an oil-in-water emulsion, and because it does not use traditional surfactants and other characteristics, it will not cause harm to the skin and has high safety.

[0008] In one aspect, the present invention provides a solid composition for emulsification, comprising the following raw materials in parts by weight:

[0009] 0.1-5.0 parts of fermented rice

[0010] Solid particles 0.7-3.0 parts

[0011] Wherein, the specific surface area of ​​the solid particles is 150-190m 2 / g, the solid particles are selected from at least one of dimethyl silylated silica, methyl silylated silica, silica, cellulose, polylactic acid, polyvinyl alcohol, silicon dioxide and aluminosilicate.

[0012] In some embodiments, the weight ratio of the fermented rice to the solid particles is 8:2-2:8, preferably 3:1-1:3, preferably 1:1.

[0013] In some embodiments, the rice fermentation product is selected from at least one of starch, cellulose, and plant protein obtained by fermenting rice as raw material. Preferably, the rice fermentation product is a rice fermentation product obtained by fermentation with lactic acid bacteria, for example: a rice fermentation product obtained by fermentation with lactic acid bacteria under the trade name of Plant Lactic Acid Bacteria Fermented Rice-SR produced by Teconobo Company.

[0014] In some embodiments, the shape of the fermented rice product is round-shaped, for example, oval, elliptical and / or circular.

[0015] In some embodiments, the solid particles are spherical in shape, such as oval, elliptical and / or circular.

[0016] In some embodiments, the solid particles are silica dimethyl silylate.

[0017] On the other hand, the present invention discloses a method for preparing the above-mentioned solid composition for emulsification, comprising the following steps: taking the rice fermentation product and solid particles, and mixing them evenly to obtain the solid composition.

[0018] On the other hand, the present invention discloses the use of the above-mentioned solid emulsification composition in the preparation of an emulsion, preferably, the emulsion is an oil-in-water emulsion. It can be understood that this oil-in-water emulsion can be used as a skin care product, cosmetic, medical emulsion, etc. for trial application on the skin surface.

[0019] In another aspect, the present invention discloses a sunscreen cream comprising the following ingredients in percentage by weight:

[0020]

[0021] The sunscreen cream is an oil-in-water emulsion;

[0022] The sunscreen is selected from: one or two of chemical sunscreens and physical sunscreens;

[0023] The regulator is selected from: one or more of a skin feel regulator, a pH regulator, a rheology modifier, a moisturizing emollient and a preservative;

[0024] The oil is selected from: one or both of liquid oil and solid oil ester.

[0025] It is understandable that the specific types of the above-mentioned regulators can be adjusted and screened according to the type and requirements of the preparation.

[0026] In some embodiments, the sunscreen cream does not contain surfactants, PEGs, polyglycerols, phospholipids, or ionic emulsifiers.

[0027] In some embodiments, the chemical sunscreen is selected from: diethylhexyl butyramido triazone, bis-ethylhexyloxyphenol methoxyphenyl triazine, ethylhexyl triazone, ethylhexyl salicylate, octocrylene, butyl methoxydibenzoylmethane, and terephthalylidene dicamphor sulfonic acid, preferably at least one of ethylhexyl salicylate, octocrylene, butyl methoxydibenzoylmethane, diethylhexyl butyramido triazone and terephthalylidene dicamphor sulfonic acid.

[0028] In some embodiments, the physical sunscreen is selected from: titanium dioxide.

[0029] In some embodiments, the amount of the sunscreen agent is 10-25%, preferably 22%.

[0030] In some embodiments, the amount of the chemical sunscreen is 10-20%, preferably 18.5%.

[0031] In some embodiments, the amount of the solid composition for emulsification is 0.8-1.5%, preferably 1.0%.

[0032] In some embodiments, the skin feel adjusting agent is selected from at least one of silica, cyclopentasiloxane and cyclohexasiloxane.

[0033] In some embodiments, the amount of the skin feel adjuster is 10-15%, preferably 12%.

[0034] In some embodiments, the pH adjuster is selected from: arginine and / or sodium hydroxide.

[0035] In some embodiments, the pH adjuster is used in an amount of 0.05-0.5%, preferably 0.35%.

[0036] In some embodiments, the rheology modifier is selected from at least one of xanthan gum, microcrystalline cellulose and cellulose gum, preferably xanthan gum.

[0037] In some embodiments, the rheology modifier is used in an amount of 0.01-0.15%, preferably 0.08%.

[0038] In some embodiments, the moisturizing emollient is selected from at least one of polyols, preferably, the moisturizing emollient is selected from at least one of glycerol, diglycerol, butylene glycol and pentylene glycol, for example, at least one of glycerol, butylene glycol and pentylene glycol.

[0039] In some embodiments, the moisturizing emollient is used in an amount of 5-15%, preferably 9%.

[0040] In some embodiments, the preservative is selected from: phenoxyethanol.

[0041] In some embodiments, the amount of the preservative is 0.01-0.5%, preferably 0.3%.

[0042] In some embodiments, the liquid oil is selected from at least one of diisopropyl sebacate, C12-15 alcohol benzoate, and phenethyl alcohol benzoate, preferably diisopropyl sebacate and / or C12-15 alcohol benzoate.

[0043] In some embodiments, the amount of the liquid oil is 5-15%, preferably 10%.

[0044] In some embodiments, the solid oil ester is selected from: behenyl alcohol.

[0045] In some embodiments, the amount of the solid oil ester is 0-5%, preferably 0%.

[0046] In some embodiments, the sunscreen cream consists of a sunscreen, a solid composition for emulsification, a skin feel regulator, a pH regulator, a rheology modifier, a moisturizing emollient, a preservative, a liquid oil, a solid oil ester, and water;

[0047] The sunscreen includes chemical sunscreen and physical sunscreen. The chemical sunscreen is ethylhexyl salicylate, octocrylene, butyl methoxydibenzoylmethane, diethylhexyl butyramido triazone and terephthalylidene dicamphor sulfonic acid, and the amount is 15-20%, preferably 18.5%. The physical sunscreen is titanium dioxide, and the amount is 1-5%, preferably 3.5%;

[0048] The solid emulsification composition is a lactic acid bacteria / rice fermentation product and silica dimethyl silylate in a weight ratio of 1:1, and the dosage is 0.5-1.5%, preferably 1.0%;

[0049] The skin feel regulator is silica, cyclopentasiloxane and cyclohexasiloxane, and the amount used is 10-15%, preferably 12%;

[0050] The pH regulator is sodium hydroxide and arginine, and the dosage is 0.05-0.5%, preferably 0.35%;

[0051] The rheology modifier is xanthan gum, and the dosage is 0.01-0.15%, preferably 0.08%;

[0052] The moisturizing emollients are glycerin, butylene glycol and pentylene glycol, and the amount used is 5-15%, preferably 9%;

[0053] The preservative is phenoxyethanol, and the dosage is 0.01-0.5%, preferably 0.3%;

[0054] The liquid oil is diisopropyl sebacate and C12-15 alcohol benzoate, and the amount is 5-15%, preferably 10%;

[0055] The solid oil ester is behenyl alcohol, and the dosage is 0.5-5%, preferably 0%.

[0056] On the other hand, the present invention also discloses a method for preparing the above-mentioned sunscreen cream, comprising the following steps: according to the water-soluble or oil-soluble properties of each component, mixing them respectively and evenly to obtain an aqueous phase and an oil phase, adding the aqueous phase to the oil phase and a pre-dispersed solid composition for emulsification, and homogenizing until the emulsification is complete.

[0057] In some embodiments, the preparation method includes the following steps: dividing each component into an aqueous phase, an oil phase and a room temperature phase according to its water-soluble or oil-soluble properties and thermal stability, heating the aqueous phase components and the oil phase components separately according to predetermined requirements, and after complete dispersion, adding the aqueous phase into the oil phase and the pre-dispersed solid composition for emulsification, homogenizing until complete emulsification, cooling, adding the pre-mixed room temperature phase, continuing to homogenize until the texture is uniform, and degassing to obtain the product.

[0058] In some embodiments, the sunscreen cream comprises the following steps:

[0059] (1) Ethylhexyl salicylate, octocrylene, butyl methoxydibenzoylmethane, diethylhexyl butyramido triazone, liquid oil and solid oil ester are divided into phase A, silica, cyclopentasiloxane, cyclohexasiloxane, moisturizing emollient, rheology modifier and physical sunscreen are divided into phase B, polydimethylsiloxane and emulsified solid composition are divided into phase C, terephthalylidene dicamphor sulfonic acid aqueous solution containing sodium hydroxide is divided into phase D, arginine and preservative are divided into phase E for standby use;

[0060] (2) Phase A is mixed at room temperature, and phase B is completely dispersed at room temperature. Phase A and phase C are homogenized at 60-80°C for 3 minutes to obtain phase A. Phase B is added to phase A and homogenized for 3 minutes. After being completely uniform, it is cooled to 45°C to obtain phase B. Phase D is dispersed at room temperature and then added to phase B and homogenized for 3 minutes to obtain phase C. Finally, phase E is slowly added to phase C and homogenized for 5 minutes.

[0061] On the other hand, the present invention also discloses a skin lotion, comprising the above-mentioned solid emulsification composition, skin oil and water. It can be understood that the solid emulsification composition of the present invention can be widely used in the preparation of Pickering emulsion to play a role in stabilizing emulsification.

[0062] In some embodiments, the skin lotion is an oil-in-water emulsion.

[0063] In some embodiments, the skin lotion further comprises a conditioning agent, wherein the conditioning agent is selected from one or more of a moisturizing emollient, a skin feel conditioning agent, a rheology modifier, a pH adjusting agent, and a preservative.

[0064] In some embodiments, the moisturizing lotion is composed of the following raw materials in percentage by mass: 0.5-1.5% of a solid emulsifying composition, 10-25% of a liquid moisturizing oil, 0-5% of a solid moisturizing oil, 1-15% of a moisturizing emollient, 5-20% of a skin feel regulator, 0.01-0.5% of a rheology modifier, 0.01-0.5% of a pH regulator, 0.01-0.5% of a preservative, and the balance is water.

[0065] On the basis of being in accordance with the common sense in the art, the above-mentioned preferred conditions can be arbitrarily combined to obtain the preferred embodiments of the present invention.

[0066] The reagents and raw materials used in the present invention are commercially available.

[0067] The positive and progressive effects of the present invention are:

[0068] The present invention discloses an emulsifying solid composition, which is obtained by combining rice fermentation product and solid particles, and has an excellent emulsifying effect. The emulsifying solid composition is used to prepare an emulsion by Pickering emulsification method, which reduces the use of emulsifiers and greatly reduces the permeability of the obtained emulsion.

[0069] The sunscreen cream of the present invention reduces the use of emulsifiers by using a solid emulsifying composition, greatly reduces the permeability of chemical sunscreens in the obtained sunscreen, and improves the safety to the skin. In addition, the sunscreen cream is proved to be a high sunscreen product suitable for people with sensitive skin through PFA, SPF tests and skin function improvement tests. BRIEF DESCRIPTION OF THE DRAWINGS

[0070] Figure 1 Schematic diagram of the formation principle of Pickering emulsion.

[0071] Figure 2 This is a schematic diagram of the lactic acid bacteria / rice fermentation product in Example 1.

[0072] Figure 3 The following are photos of the product properties of recipes 2 and 3 in Example 2.

[0073] Figure 4 The following are photos of the product properties of recipes 4 and 5 in Example 2.

[0074] Figure 5 The following are photos of the product properties of formulations 6 and 7 in Example 2.

[0075] Figure 6 This is a flat plate rotation test diagram for formulations 2, 4 and 6 in Example 2.

[0076] Figure 7 This is a microscope photograph of the sunscreen cream of Formula 2 in Example 3.

[0077] Figure 8 These are the Raman spectra of the subjects in Example 3 before and after using the sunscreen cream of Formula 1 or 2.

[0078] Fig. 9 It is the relative content of organic sunscreen agent penetration in the skin at 0-20 μm of the sunscreen creams of Formula 2 and Formula 1 in Example 3.

[0079] Fig.10This is a heat map visualization of the penetration of sunscreen creams of Formula 2 and Formula 1 in Example 3.

[0080] Fig.11 This is a schematic diagram of the erythema index a* value in Example 5.

[0081] Fig.12 This is a schematic diagram of the transepidermal water loss TEWL value in Example 5.

[0082] Fig.13 This is a schematic diagram of the moisture content of the stratum corneum in Example 5.

[0083] Fig.14 This is a photograph of the properties of the skin lotion in Example 6 after being left at room temperature for one week. DETAILED DESCRIPTION

[0084] The present invention is further described below by way of examples, but the present invention is not limited to the scope of the examples. The experimental methods in the following examples without specifying specific conditions are carried out according to conventional methods and conditions, or selected according to the product specifications.

[0085] Example 1

[0086] According to the formulations and preparation methods in Table 1 below, a variety of sunscreen creams were obtained.

[0087] Table 1. Sunscreen cream formula (wt%)

[0088]

[0089]

[0090]

[0091] The above lactic acid bacteria / rice fermentation product is a rice fermentation product obtained by lactic acid bacteria fermentation (Teco Nova Company, trade name Plant Lactobacillus Fermented Rice-SR), which is quasi-circular in shape under a microscope, such as Figure 2 Silica dimethyl silylate is from Evonik Industries AG, product model R974, and its specific surface area is 150-190m 2 / g.

[0092] Preparation method:

[0093] Phase A (oil phase) was mixed at room temperature, phase B (water phase) was completely dissolved at room temperature, phase A and phase C1 or phase C2 were homogenized at 60-80°C for 3 minutes to obtain phase A, phase B was added to phase A and homogenized for 3 minutes, and after being completely uniform, it was cooled to 45°C to obtain phase B, phase D was dispersed at room temperature and added to phase B and homogenized for 3 minutes to obtain phase C, and finally phase E was slowly added to phase C and homogenized for 5 minutes to obtain experimental samples, i.e. sunscreen creams with different formulas.

[0094] Example 2

[0095] This example verifies the performance of the experimental samples with different formulations obtained in Example 1.

[0096] 1. Methods

[0097] The experimental samples prepared according to formulations 2-7 of Example 1 were placed in containers of the same specifications and left at room temperature for one week before performance observation and comparison were performed.

[0098] 2. Results

[0099] The results are as follows Figure 3-6 As shown. Among them, Figure 3 The product properties of Formulas 2 and 3 are shown in the figure. Compared with Formula 2, Formula 3 does not add a solid composition for emulsification. It can be seen that Formula 3 is obviously unable to emulsify and exhibits severe stratification.

[0100] Figure 4 These are photos of the product properties of Formulas 4 and 5. Compared with Formula 2, Formula 4 does not add silica dimethyl silylate, Formula 5 does not add silica dimethyl silylate, and starch is used instead of "lactic acid bacteria / rice fermentation product". It can be seen that formulas using only starch powder (such as lactic acid bacteria / rice fermentation product or starch alone) will also have serious instability problems.

[0101] Figure 5 The product properties of Formulas 6 and 7 are shown in the figure. Compared with Formula 2, Formula 6 does not add lactic acid bacteria / rice fermentation products, and Formula 7 replaces silica dimethyl silylate with silica. It can be seen that the formula using only silica powder (such as silica dimethyl silylate or silica alone) will also have serious instability problems.

[0102] Figure 6 This is a flat plate rotation test diagram for formulas 2, 4 and 6. The test method is: take an appropriate amount of cream and place it on a horizontally placed flat plate, then gradually increase the rotation angle of the flat plate relative to the horizontal plane, observe the sliding of the cream of each formula, and thus determine its viscosity and stability.

[0103] As can be seen from the figure, formula 4 begins to fall rapidly at 30° ( Figure 6), while Formula 2 still does not fall at 60° (30° photo not shown), and Formula 6 is obviously not uniform. It can be intuitively found that the degree of emulsion uniformity is that Formula 2 is better than Formula 4, and Formula 4 is better than Formula 6.

[0104] Example 3

[0105] In this example, the sunscreen creams of Formula 1 and Formula 2 were examined for their effects on human body application.

[0106] 1. Structural verification

[0107] Take the sunscreen cream of formula 2 and observe the sample under optical microscope under bright field light source and polarized light source at room temperature. The results are as follows: Figure 7 shown.

[0108] Figure 7 2 are microscope photos of the sunscreen cream of formula 2, wherein A is a bright field photo (magnified 50 times) and B is a polarized field photo (magnified 50 times). As can be seen from the figure, solid particles are gathered on the interface of the emulsion, and it can be determined that the embodiment is a Pickering emulsified sunscreen lotion.

[0109] 2. Determine the difference in penetration of sunscreen agents in different sunscreen products into human skin by confocal Raman spectroscopy

[0110] (1) Sample

[0111] Samples: The sunscreen creams of Formula 1 and Formula 2 were used as experimental samples, both of which were in the form of white liquid.

[0112] (2) Experimental methods

[0113] All volunteers signed informed consent forms before the test, in accordance with the Declaration of Helsinki. Considering that the melanin in the skin of some volunteers will produce strong fluorescence interference, the volunteers whose melanin content exceeds the standard were excluded through pre-testing in accordance with the operating standards of the SPF test before the test. Volunteers (n = 10) were prohibited from using sunscreen products and other cosmetics or medicines in the test area 48 hours before the test. During the test, the volunteers will wash the skin on the inside of their arms and keep it in a constant temperature and humidity environment with a temperature of 21±1℃ and a humidity of 50±10% for 30 minutes. Find 3 test areas with a diameter of 18mm on the inside of the volunteer's arm, with each area at least 3cm apart. Each product is evenly applied at a dosage of 2mg / cm2, and the test time nodes are before use (T0) and 120min after use (T120). One test area is tested before use, and the remaining two areas are tested after applying the product. After using the product, the product on the skin surface needs to be wiped off with filter paper before collecting the spectrum.

[0114] (3) Data processing

[0115] Horiba Miacro HR (Horiba Jobin Yvon SSA, Lille, France) confocal Raman spectroscopy (CRM) analysis was performed with a laser wavelength of 660 nm and a laser power of 13 mW at the sample. Raman spectra were collected in the range of 800–3800 cm -1 The acquisition depth is -6-20μm, the step is 2μm, the exposure time for each depth is 2s, the total is 2 times, and each area is collected 4 times in parallel.

[0116] According to the standard method of Raman testing, the skin surface is composed of keratin AUC2910-2965cm -1 (Area under the curve) is determined by half of the maximum value. Raman acquisition and data processing use Raman commercial analysis software Labspec 6 (HoribaScientific, France). All spectra are processed in the same way, and cosmic rays have been removed before processing. A Savitzky-Golay filter is used for smoothing, a 9th-order polynomial is used to remove the fluorescence baseline, and singular value decomposition (SVD) is used to reduce spectral noise. The classical least squares model is used to determine the penetration content of sunscreen. The Raman spectrum of the sunscreen is measured on a calcium fluoride window. The collection is 2s in the range of 800-3800cm-1, accumulated 10 times, and cosmic rays and fluorescence baselines are removed. The processed data is analyzed for significance and graphed using Origin Pro2022.

[0117] (4) Result determination method

[0118] In order to determine the difference in penetration of sunscreens in different depths of the skin, the sunscreen content was expressed as mean plus standard deviation (SD). The penetration of sunscreens at different depths of the skin was expressed as Score, which indicates the strength of the Raman signal directly analyzed by Labspec 6 software (Horiba Scientific, France). The sunscreen content of the experimental group and the control group was subjected to an independent sample T test (two independent-sample t-test) (p < 0.05).

[0119] (5)Results.

[0120] The thickness of the stratum corneum of human arm skin is about 15.3±2.8μm. The 20μm set in the experiment includes the stratum corneum of the skin. Whether the organic sunscreen can penetrate the stratum corneum is the focus of this experiment.

[0121] Figure 8The Raman spectra of the subjects before and after using the sunscreen cream of formula 1 or 2, where No. 1 black is the sunscreen cream of formula 1, No. 2 red is the sunscreen cream of formula 2, No. 3 blue is the skin without sunscreen cream, and No. 4 green is the Raman spectrum curve of the skin with sunscreen cream of formula 1. The above results show that when the sunscreen cream is present, if there are peaks in the three regions of 1200, 1300 and 1600, it can be judged that the changes are caused by the addition of sunscreen. The permeability of the sample can be judged by observing the strength of the signal at different skin depths. In this experiment, 1600cm is preferred. -1 .

[0122] Fig. 9 The relative penetration content of organic sunscreens in formula 2 and formula 1 at 0-20 μm in the skin, where the red circle is the sunscreen of formula 1 and the black square is the sunscreen of formula 2. The above results show that at all depths of the skin, the Score, an indicator representing the intensity of the sunscreen signal in formula 2, is lower than that in formula 1, indicating that the penetration ability of formula 2 into the skin is much lower than that of formula 1.

[0123] Fig.10 This is a visualization heat map of the penetration of sunscreen creams with formula 2 and formula 1. Red represents a high content of organic sunscreen, and blue represents a low content of organic sunscreen. The left picture is the sunscreen cream with formula 2, and the right picture is the sunscreen cream with formula 1. The visualization heat map can more intuitively observe the penetration of the two sunscreen products in ten volunteers. The visualization heat map of each product consists of ten columns, and each column represents the penetration of a subject. The above results show that different volunteers have great differences in the penetration of organic sunscreens. After using the sunscreen product for 2 hours, the penetration of organic sunscreens will break through the stratum corneum of some volunteers. The probability of this happening in the sunscreen cream with formula 1 is greater than that in the sunscreen cream with formula 2.

[0124] The above experimental results show that the penetration of the sunscreen cream emulsified with Pickering using Formula 2 is much smaller than that of the sunscreen cream using Formula 1 with a common emulsifier.

[0125] Example 4

[0126] In this embodiment, the sunscreen cream of Formula 2 is used for population efficacy testing, and the SPF and PFA values ​​of the sunscreen cream product of Formula 2 are tested through human body efficacy tests.

[0127] 1. Methods

[0128] According to the conventional test methods in this field (Chapter 8, Item 2 of the 2015 edition of the "Safety Technical Specifications for Cosmetics", "Determination Method of Sun Protection Index (SPF) of Sunscreen Cosmetics"; Chapter 8, Item 4 of the 2015 edition of the "Safety Technical Specifications for Cosmetics", "Determination Method of Long-wave Ultraviolet Protection Index (PFA) of Sunscreen Cosmetics"), the subjects lie prone and their backs are irradiated. The minimum erythema dose (MED value) of the subjects' skin to ultraviolet irradiation is predicted 24 hours before the test, and the ultraviolet irradiation dose is adjusted according to the predicted results for the test samples.

[0129] On the day of the test, a spot no smaller than 30 cm was selected on the back of the subject. 2 Normal skin area, (2.00±0.05)mg / cm 2 Apply the sample to be tested or the standard reference substance (S1 with PFA=4.4 and P2 with SPF=16.1) evenly on the above-mentioned area, wait for 15 minutes or proceed as required by the label instructions.

[0130] Then choose the appropriate ultraviolet radiation dose and perform the irradiation in three situations: ① No sample is applied to the subject's skin; ② A standard control sample is applied; ③ The sample to be tested is applied.

[0131] The experimental results were observed after 16-24 hours, and the MED values ​​(the time required for the minimum erythema dose MED to appear on the skin) were recorded under the three conditions respectively.

[0132] 2. Test result analysis method

[0133] Sun protection factor (SPF): The ratio of the MED required to cause erythema on the skin protected by the sunscreen cosmetic to the MED required to cause erythema on the unprotected skin is the SPF of the sunscreen cosmetic. It can be expressed as follows:

[0134]

[0135] The PFA value of a sample for a single subject was calculated using the following formula:

[0136] MPPDp: Minimum sustained darkening dose (MPPD) of the skin protected by the test product;

[0137]

[0138] MPPDu: Minimum persistent tanning dose (MPPD) for unprotected skin;

[0139] The above minimum sustained black dyeing dose (MPPD) is obtained by pre-standard control test.

[0140] 3. Results

[0141] The test results are shown in the following table.

[0142] Table 2. SPF and PFA values ​​of sunscreen cream of formula 2 (mean ± SD)

[0143] average value SD SPF 58.93 2.81 PFA 14.1 1.9

[0144] The above results show that the sunscreen cream of Formula 2 has an SPF greater than 50 and a PA greater than 12, and is a sunscreen lotion product with excellent sun protection effect.

[0145] Example 5

[0146] This example evaluates the efficacy of the sunscreen cream of Formula 2 in terms of repair, moisturizing, and soothing through a human efficacy test.

[0147] 1. Methods

[0148] (1) Efficacy determination index

[0149] Soothing: the skin erythema index a* value of the subjects before and after using the sample;

[0150] Repair: The average transepidermal water loss (TEWL) of the subjects before and after using the samples;

[0151] Moisturizing: The moisture content of the stratum corneum of the subjects' skin before and after using the samples.

[0152] (2) Test principle

[0153] Soothing: Test the skin erythema index a* value. The higher the a* value, the higher the skin hemoglobin content, which means the skin redness is more obvious.

[0154] Repair: The TEWL value reflects the barrier function of the stratum corneum and can be used to evaluate the repair ability of cosmetics for the skin barrier function. Under the test conditions, the higher the TEWL value obtained, the more transepidermal water loss per unit time and unit cross-sectional area; the lower the TEWL value, the less transepidermal water loss per unit time and unit cross-sectional area.

[0155] Moisturizing: The capacitance method is used to measure the moisture content of the stratum corneum of human skin. According to the different moisture content of the stratum corneum of the skin, the measured skin capacitance value is different, and its parameters can represent the moisture content of the skin.

[0156] (3) Test method

[0157] Before the test: The subjects washed their faces with facial cleanser and rested in a constant temperature and humidity room for 15 minutes.

[0158] A. Before using the product, use SkinColorimeter CL400 to measure the erythema index a* value; use Tewameter to test the transepidermal water loss of the face; use Corneometer to measure the moisture content of the stratum corneum.

[0159] B. Apply the product every morning and evening according to the product usage instructions.

[0160] C. Repeat step 1 after 1W and 2W of product use.

[0161] (4) Test result analysis method

[0162] Soothing: Analyze and record the average a* value of the erythema index of the subjects before and after using the sample. The more the a value decreases before and after use, the better the soothing effect of the product.

[0163] Repair: The lower the TEWL value, the less transepidermal water loss per unit time and unit cross-sectional area.

[0164] Moisturizing: The higher the moisture content of the stratum corneum, the higher the moisturizing level of the skin.

[0165] (5) Test results

[0166] The test results are as follows Figure 11-13 As shown, Fig.11 is the erythema index a* value, Fig.12 TEWL value (g / hm 2 ), Fig.13 is the stratum corneum water content (CU).

[0167] The results showed that after using the sunscreen cream with formula 2 for two weeks, the subjects' skin redness (a* value) was significantly reduced, the skin barrier function was improved (TEWL), and the water content of the stratum corneum was also increased, that is, the condition of the subjects' sensitive skin was improved, indicating that this sunscreen cream is suitable for people with sensitive skin.

[0168] Example 6

[0169] A skin lotion is prepared according to the following formula.

[0170] Table 3. Body lotion formula (wt%)

[0171]

[0172] Preparation method: Mix phase A (oil phase) at room temperature, dissolve phase B (water phase) completely at room temperature, homogenize phase A and phase C at 60-80°C for 3 minutes to obtain phase A, add phase B into phase A and homogenize for 3 minutes, cool to 45°C after complete homogenization to obtain phase B, finally slowly add phase D into phase B and homogenize for 5 minutes to obtain the experimental sample, which is the moisturizing lotion.

[0173] Performance verification: Place the above lotion at room temperature for one week and observe its properties. Fig.14 As shown in the figure, it can be seen that the skin lotion is in good condition and has not changed, indicating that the solid composition for emulsification can play a good emulsification role.

Claims

1. A solid composition for emulsification, characterized in that: Contains the following raw materials in parts by weight: 0.1-5.0 parts of fermented rice Solid particles 0.7-3.0 parts Wherein, the specific surface area of ​​the solid particles is 150-190m 2 / g, the solid particles are selected from at least one of dimethyl silylated silica, methyl silylated silica, silica, cellulose, polylactic acid, polyvinyl alcohol, silicon dioxide and aluminosilicate.

2. The solid composition for emulsification according to claim 1, characterized in that At least one of the following conditions is met: (1) The weight ratio of the fermented rice to the solid particles is 8:2-2:8, preferably 3:1-1:3, preferably 1:1; (2) the rice fermentation product is selected from at least one of starch, cellulose and plant protein obtained by fermenting rice as a raw material, and preferably, the rice fermentation product is a rice fermentation product obtained by fermenting with lactic acid bacteria; (3) The shape of the fermented rice product is quasi-circular, for example, oval, elliptical and / or circular; (4) The solid particles are quasi-circular in shape, for example, oval, elliptical and / or circular; (5) The solid particles are silica dimethyl silylate.

3. The method for preparing the solid composition for emulsification according to claim 1 or 2, characterized in that: The following steps are involved: The fermented rice product and the solid particles are mixed evenly to obtain the product.

4. Use of the solid emulsified composition according to claim 1 or 2 in preparing an emulsion, preferably, the emulsion is an oil-in-water emulsion.

5. A sunscreen cream, characterized in that: The composition includes the following weight percentages: The sunscreen cream is an oil-in-water emulsion; The sunscreen is selected from: one or two of chemical sunscreens and physical sunscreens; The regulator is selected from: one or more of a skin feel regulator, a pH regulator, a rheology modifier, a moisturizing emollient and a preservative; The oil is selected from: one or both of liquid oil and solid oil ester.

6. The sunscreen cream according to claim 5, characterized in that Meet at least one of the following conditions: (1) The sunscreen cream does not contain surfactants, PEGs, polyglycerols, phospholipids, or ionic emulsifiers; (2) The chemical sunscreen is selected from: diethylhexyl butyramido triazone, bis-ethylhexyloxyphenol methoxyphenyl triazine, ethylhexyl triazone, ethylhexyl salicylate, octocrylene, butyl methoxydibenzoylmethane, terephthalylidene dicamphor sulfonic acid, preferably at least one of ethylhexyl salicylate, octocrylene, butyl methoxydibenzoylmethane, diethylhexyl butyramido triazone and terephthalylidene dicamphor sulfonic acid; (3) The physical sunscreen is selected from: titanium dioxide; (4) The amount of the sunscreen is 10-25%, preferably 22%; (5) The amount of the chemical sunscreen is 10-20%, preferably 18.5%; (6) The amount of the solid composition for emulsification is 0.8-1.5%, preferably 1.0%; (7) The skin feel adjuster is selected from at least one of silica, cyclopentasiloxane and cyclohexasiloxane; (8) The amount of the skin feel adjuster is 10-15%, preferably 12%; (9) The pH regulator is selected from: arginine and / or sodium hydroxide; (10) The pH regulator is used in an amount of 0.05-0.5%, preferably 0.35%; (11) The rheology modifier is selected from at least one of xanthan gum, microcrystalline cellulose and cellulose gum, preferably xanthan gum; (12) The amount of the rheology modifier is 0.01-0.15%, preferably 0.08%; (13) The moisturizing emollient is selected from at least one of polyols. Preferably, the moisturizing emollient is selected from at least one of glycerol, diglycerol, butylene glycol and pentylene glycol, for example, at least one of glycerol, butylene glycol and pentylene glycol; (14) The amount of the moisturizing emollient is 5-15%, preferably 9%; (15) The preservative is selected from: phenoxyethanol; (16) The amount of the preservative is 0.01-0.5%, preferably 0.3%; (17) The liquid oil is selected from at least one of diisopropyl sebacate, C12-15 alcohol benzoate, and phenethyl alcohol benzoate, preferably diisopropyl sebacate and / or C12-15 alcohol benzoate; (18) The amount of the liquid oil is 5-15%, preferably 10%; (19) The solid oil ester is selected from: behenyl alcohol; (20) The amount of the solid oil ester is 0-5%, preferably 0%.

7. The sunscreen cream according to claim 5, characterized in that: It consists of a sunscreen, a solid composition for emulsification, a skin feel regulator, a pH regulator, a rheology modifier, a moisturizing emollient, a preservative, liquid oil, a solid oil ester and water; The sunscreen includes chemical sunscreen and physical sunscreen. The chemical sunscreen is ethylhexyl salicylate, octocrylene, butyl methoxydibenzoylmethane, diethylhexyl butyramido triazone and terephthalylidene dicamphor sulfonic acid, and the amount is 15-20%, preferably 18.5%. The physical sunscreen is titanium dioxide, and the amount is 1-5%, preferably 3.5%; The solid emulsification composition is a lactic acid bacteria / rice fermentation product and silica dimethyl silylate in a weight ratio of 1:1, and the dosage is 0.5-1.5%, preferably 1.0%; The skin feel regulator is silica, cyclopentasiloxane and cyclohexasiloxane, and the amount used is 10-15%, preferably 12%; The pH regulator is sodium hydroxide and arginine, and the dosage is 0.05-0.5%, preferably 0.35%; The rheology modifier is xanthan gum, and the dosage is 0.01-0.15%, preferably 0.08%; The moisturizing emollients are glycerin, butylene glycol and pentylene glycol, and the amount used is 5-15%, preferably 9%; The preservative is phenoxyethanol, and the dosage is 0.01-0.5%, preferably 0.3%; The liquid oil is diisopropyl sebacate and C12-15 alcohol benzoate, and the amount is 5-15%, preferably 10%; The solid oil ester is behenyl alcohol, and the dosage is 0.5-5%, preferably 0%.

8. The method for preparing the sunscreen cream according to any one of claims 5 to 7, characterized in that: The following steps are involved: According to the water-soluble or oil-soluble properties of each component, mix them evenly to obtain a water phase and an oil phase, put the water phase into the oil phase and the pre-dispersed solid composition for emulsification, and homogenize until the emulsification is complete; Furthermore, the method comprises the following steps: according to the water-solubility or oil-solubility and thermal stability of each component, the components are divided into a water phase, an oil phase and a room temperature phase, the water phase components and the oil phase components are heated separately according to predetermined requirements, after complete dispersion, the water phase is added into the oil phase and the pre-dispersed solid composition for emulsification, homogenized until complete emulsification, cooled, the pre-mixed room temperature phase is added, the homogenization is continued until the texture is uniform, and degassing is performed to obtain the product.

9. The preparation method according to claim 8, characterized in that: The sunscreen cream is the sunscreen cream according to claim 7, comprising the following steps: (1) Ethylhexyl salicylate, octocrylene, butyl methoxydibenzoylmethane, diethylhexyl butyramido triazone, liquid oil and solid oil ester are divided into phase A, silica, cyclopentasiloxane, cyclohexasiloxane, moisturizing emollient, rheology modifier and physical sunscreen are divided into phase B, polydimethylsiloxane and emulsified solid composition are divided into phase C, terephthalylidene dicamphor sulfonic acid aqueous solution containing sodium hydroxide is divided into phase D, arginine and preservative are divided into phase E for standby use; (2) Phase A is mixed at room temperature, and phase B is completely dispersed at room temperature. Phase A and phase C are homogenized at 60-80°C for 3 minutes to obtain phase A. Phase B is added to phase A and homogenized for 3 minutes. After being completely uniform, it is cooled to 45°C to obtain phase B. Phase D is dispersed at room temperature and then added to phase B and homogenized for 3 minutes to obtain phase C. Finally, phase E is slowly added to phase C and homogenized for 5 minutes.

10. A skin lotion, characterized in that: Comprising the solid composition for emulsification according to claim 1 or 2, emollient oil and water; Preferably, the skin lotion further comprises a regulator, and the regulator is selected from: one or more of a moisturizing emollient, a skin feel regulator, a rheology modifier, a pH regulator and a preservative; For example, the skin lotion is composed of the following raw materials in percentage by mass: 0.5-1.5% of a solid emulsifying composition, 10-25% of a liquid skin oil, 0-5% of a solid skin oil, 1-15% of a moisturizing emollient, 5-20% of a skin feel regulator, 0.01-0.5% of a rheology modifier, 0.01-0.5% of a pH regulator, 0.01-0.5% of a preservative, and the balance is water.

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