An auto-emulsifying oil composition and its application in cosmetics

Abstract

The present invention discloses a self-emulsifying oil composition. The preparation raw materials and their addition amounts are as follows: the weight ratio of long-chain alkyl glycerol ether to oil emulsification stabilizer is (0.1 - 0.5):(0.1 - 2.0). The present invention can enable the oil to self-emulsify to form a stable micelle system, form creams with different textures, and reduce the use of externally added emulsifiers in cosmetics. Moreover, the system can maintain a stable state in high and low temperature environments of (-18 to 48 °C) without deterioration. At the same time, the emulsification stability of the product can be maintained. The particle size distribution of this preparation is uniform, with a particle size of 1 - 5 microns, and it is more friendly to sensitive skin when applied to cosmetics, has a delicate skin feel, and the ingredients are easy to absorb.

Description

Technical Field

[0001] The present invention relates to a self-emulsifying oil composition and its application in cosmetics, relates to A61K, and specifically relates to the field of preparations for dressing. Background Art

[0002] With the progress of technology, the aggravation of environmental pollution, and the acceleration of people's living rhythm, people pay more and more attention to skin care. However, due to the stimulation of the external environment, the sensitivity of people's skin increases year by year, and the skin barrier function declines. Therefore, choosing cosmetics with lower irritation is the new trend of future skin care. In traditional skin care preparations such as lotions and creams, emulsifiers are inevitably used. Common emulsifiers can form a uniform and stable system between immiscible water and oil phases, making it easy to apply and clean. However, emulsifiers have certain safety risks to the skin. High-concentration anionic or non-ionic polyether emulsifiers can cause irritation or allergic reactions to the skin. Emulsifiers containing ethoxy structures bring risks of dioxane and diethylene glycol, posing a potential threat to the human body in the long term. Therefore, minimizing the use of emulsifiers and forming a self-emulsifying homogeneous appearance between the oil phase and the water phase, creating the texture of white essence, lotion, and cream, while also avoiding the irritation of emulsifiers to the skin, making the prepared cosmetics more suitable for sensitive skin, is the new trend.

[0003] Chinese Patent CN201911142977.6 discloses an emulsification system and its application, an active composition and its application, and a cosmetic and its preparation method, which adopts an emulsification system with a synergistic combination of subtilisin lipopeptide sodium, enzymatically hydrolyzed lecithin, and batyl alcohol, which can bring excellent and delicate skin feel, is not easy to separate oil and water, and enables the absorption of active substances to be faster and the utilization rate to be higher. However, the stability of the emulsification system will significantly decline in high and low temperature environments. Subtilisin lipopeptide sodium belongs to a new type of amino acid surfactant and has the ability to load high amounts of oil. Chinese Patent CN20071-0012275.7 discloses a composite emulsifier and an emulsion prepared therefrom and its preparation method, which uses a combination of coenzyme Q 10 , soybean phospholipid, and HS 15 as a composite emulsifier, which can resist the destructive effects of heat and freeze-thaw, and has good emulsification effect, but has poor binding effect with the components in cosmetics and is not suitable for application in cosmetic products. Summary of the Invention

[0004] In order to avoid the use of external emulsifiers and prepare a self-emulsifying system with excellent emulsification performance and low irritation, which is specifically applied to cosmetics for sensitive skin, the first aspect of the present invention provides a self-emulsifying oil composition, and the preparation raw materials and addition ratios are as follows: the weight ratio of long-chain alkyl glycerol ether to oil emulsification stabilizer is (0.1 - 0.5):(0.1 - 2.0).

[0005] As a preferred embodiment, the carbon number of the long-chain alkyl glyceryl ether is ≥18.

[0006] As a preferred embodiment, the long-chain alkyl glyceryl ether is batyl alcohol.

[0007] The structural formula of batyl alcohol is as follows:

[0008]

[0009] As a preferred embodiment, the oil emulsion stabilizer is selected from one or a combination of rape sterols and hydrogenated coconut glycerides.

[0010] As a preferred embodiment, the raw materials for preparing the self-emulsifying oil composition include, by weight: 0.1-0.5 parts of long-chain alkyl glyceryl ether and 0.1-2.0 parts of oil emulsion stabilizer.

[0011] The self-emulsification mechanism of the self-emulsifying grease composition is speculated as follows:

[0012]

[0013] During the experiment, the applicant discovered that by adding a self-emulsifying composition, the oil can be self-emulsified to form a stable micelle system, forming creams with different textures, avoiding the use of external emulsifiers in cosmetics, reducing the irritation of emulsifiers to the skin, and being more friendly to sensitive skin. The self-emulsifying composition includes batyl alcohol and an oil emulsification stabilizer in a weight ratio of (0.1-0.5): (0.1-2.0). The reason why the self-emulsifying composition can cause the oil to self-emulsify may be that the fatty alcohol end of batyl alcohol is connected to a glycerol molecule and contains both hydrophilic and lipophilic groups. The lipophilic groups of batyl alcohol can be interspersed in the water-soluble high molecular polymer containing the lipophilic group. The introduction of the oil emulsification stabilizer can further improve the interfacial firmness, allowing it to maintain a creamy state in high and low temperature environments (-18 to 48°C). A weight ratio of (0.1-0.5): (0.5-2.0) of batyl alcohol and oil emulsion stabilizer can form a stable interface. When combined with an aqueous thickener, the combined effect of the water-soluble polymer and batyl alcohol can be maximized, forming a stable three-dimensional network structure, presenting a stable and dynamic micellar emulsification system, and exhibiting improved product stability. If the weight ratio exceeds the preferred range, the interfacial film will be weak. Especially in low-temperature environments, when the batyl alcohol content exceeds 0.5, the hydrophilicity is reduced, the interfacial film is affected, and the film will appear to be dregs. Similarly, in high-temperature environments, it will become jelly-like and the stability will be reduced.

[0014] A second aspect of the present invention provides an application of a self-emulsifying oil and fat composition in cosmetics, wherein the cosmetics are selected from one of an emulsion, an essence, a cream, and a facial mask.

[0015] As a preferred embodiment, the preparation raw materials applied to cosmetics include, by weight: 0.1 - 0.5 parts of a thickener, 0.1 - 25 parts of an oil phase, 0.1 - 5 parts of a self-emulsifying oil composition, 0.2 - 1 part of an anti-corrosion system, 0.1 - 10 parts of auxiliary components, and the water phase is supplemented to 100 parts.

[0016] As a preferred embodiment, the thickener is selected from PEMULEN TM TR-1 Polymer (rheology modifier), Carbopol Ultrez 30 Polymer (carbomer U30), PEMULEN TM TR-2 Polymer (rheology modifier), 981 Polymer (carbomer 981), 980 Polymer (carbomer 980), xanthan gum, SEPINOV EMT 10 (hydroxyethyl acrylate & acryloyldimethyltaurine sodium copolymer), Aristoflex Silk (sodium polyacryloyldimethyltaurate), Aristoflex AVC (acrylamide dimethyltaurine ammonium / VP copolymer), AQUPECHV-501E (acrylate cross-linked copolymer), AQUPEC HV-505E (acrylate cross-linked copolymer), SEPIMAX ZEN (SEPIMAX ZEN), or a combination of one or more of them.

[0017] As a preferred embodiment, the oil phase is selected from polydimethylsiloxane, cetearyl alcohol, beeswax, microcrystalline wax, behenyl alcohol, cetyl alcohol, stearyl alcohol, stearic acid, glyceryl behenate-eicosanedioate, isononyl isononanoate, isononyl isostearate, ethylhexyl palmitate, cetyl ethylhexanoate, triglyceride (ethylhexanoic acid), caprylic / capric triglyceride, coconut alcohol-caprylic / capric triglyceride, pentaerythrityl tetra(ethylhexanoate), C 12-13 alcohol lactate, pentaerythrityl tetra(isostearate), distearyl malate, caprylic / capric / myristic / stearic triglyceride, olive fruit oil, sunflower seed oil, squalane, shea butter, jojoba seed oil, or a combination of one or more of them.

[0018] As a preferred embodiment, the water phase includes, by weight, at least 1 - 10 parts of glycerol, 1 - 8 parts of polyol, and the water is supplemented to 100 parts.

[0019] As a preferred embodiment, the water phase includes, by weight, at least 1 - 5 parts of glycerol, 3 - 8 parts of polyol, and the water is supplemented to 100 parts.

[0020] As a preferred embodiment, the polyol is selected from one or a combination of polyethylene glycol, 1,3-propanediol, 1,3-butanediol, dipropylene glycol, etc.

[0021] As a preferred embodiment, the auxiliary components are selected from one or a combination of a humectant, a skin protectant, a neutralizing agent, an antioxidant, a fragrance, etc.

[0022] As a preferred embodiment, the anti-corrosion system includes, but is not limited to, p-hydroxyacetophenone, phenoxyethanol, potassium sorbate, etc.

[0023] As a preferred embodiment, the neutralizing agent includes, but is not limited to, one or a combination of arginine, sodium hydroxide, potassium hydroxide, triethanolamine, tromethamine.

[0024] As a preferred embodiment, the humectant includes, but is not limited to, one or a combination of trehalose, betaine.

[0025] As a preferred embodiment, the preparation method of the self-emulsifying oil composition applied to cosmetics includes the following steps:

[0026] The self-emulsifying oil composition is added to the oil phase, and then added to the mixture of the water phase, thickener, anti-corrosion system, and auxiliary components, heated and melted evenly, and homogenized at high speed to form a uniform emulsion.

[0027] As a preferred embodiment, the preparation method of the self-emulsifying oil composition applied to cosmetics includes the following steps:

[0028] 1) The water phase and the thickener are sequentially added to the water phase pot, stirred evenly at room temperature and then heated to 80-85°C and continue to stir until the material is uniform, pumped into the main pot, and kept warm for use;

[0029] 2) The oil phase and the self-emulsifying oil composition are sequentially added to the oil phase pot, stirred evenly at room temperature and then heated to 80-85°C, and kept warm for use;

[0030] 3) The main pot is started with low-speed homogenization at 2000-3000 rpm, the oil phase is slowly pumped into the main pot, and after the oil phase is pumped in completely, high-speed homogenization at 4000-6000 rpm is started and kept for 3-5 minutes until the material is uniform;

[0031] 4) The main pot is cooled to 40-45°C, the anti-corrosion system is added, stirred evenly, and the neutralizing agent is added until the material is uniform;

[0032] 5) After the main pot is cooled to 38±2°C, it is detected and discharged.

[0033] Compared with the prior art, the present invention has the following beneficial effects:

[0034] (1) The self-emulsifying oil composition of the present invention includes batyl alcohol and an oil emulsification stabilizer, which can cause the oil to self-emulsify to form a stable micelle system, form creams with different textures, and reduce the use of externally added emulsifiers in cosmetics.

[0035] (2) For the self-emulsifying oil composition of the present invention, the weight ratio of batyl alcohol to the oil emulsification stabilizer is (0.1 - 0.5):(0.1 - 2.0), which can keep the system in a stable state in high and low temperature environments (-18 to 48 °C) without deterioration.

[0036] (3) The self-emulsifying oil composition of the present invention can maintain the emulsion stability of the product. The preparation has a uniform particle size distribution, with a particle size of 1 - 5 microns, and is more friendly to sensitive skin when applied to cosmetics, has a delicate skin feel, and the ingredients are easily absorbed. Description of the Drawings

[0037] Figure 1 It is a picture of the particle size test for Example 1;

[0038] Figure 2 It is a picture of the layering problem that occurred after centrifugation for Comparative Example 1;

[0039] Figure 3 It is a picture of the tofu residue phenomenon that occurred after low-temperature freeze-thaw for Comparative Example 5. Detailed Description of the Invention

[0040] Examples

[0041] A self-emulsifying oil composition, the preparation raw materials of which include: long-chain alkyl glycerol ether and an oil emulsification stabilizer.

[0042] The long-chain alkyl glycerol ether is batyl alcohol.

[0043] The oil emulsification stabilizer is a combination of brassinosteroids and hydrogenated coconut oil glyceride. The model of the brassinosteroids is Phytosoothe LS 9766, purchased from BASF (China) Co., Ltd. The model of the hydrogenated coconut oil glyceride is 100, purchased from IOIOleo GmbH.

[0044] The model of polydimethylsiloxane in the oil phase is XIAMETER PMX-200 5CS. The model of jojoba oil is DW JOJOBA COLORLESS, purchased from Vantage Specialty Chemicals, Inc. The model of caprylic / capric triglyceride is TEGOSOFT CT & Crodamol GTCC & Myritol 318, purchased from BASF (China) Co., Ltd.

[0045] The self-emulsifying oil composition is used as a raw material for the preparation of cosmetics, and the parts by weight are shown in Table 1 and Table 2 below.

[0046] Table 1

[0047]

[0048]

[0049] Table 2

[0050]

[0051]

[0052] The preparation method of the self-emulsifying oil composition applied to the above comparative examples and examples includes the following steps:

[0053] 1) The aqueous phase and the thickener are sequentially added to the aqueous phase pot, stirred evenly at room temperature, then heated to 83°C and continuously stirred until the material is uniform, pumped into the main pot, and kept warm for use;

[0054] 2) The oil phase and the self-emulsifying oil composition are sequentially added to the oil phase pot, stirred evenly at room temperature, then heated to 83°C, and kept warm for use;

[0055] 3) The main pot is started with low-speed homogenization at 2500 rpm, the oil phase is slowly pumped into the main pot. After the oil phase is completely pumped in, high-speed homogenization is started at 5000 rpm and maintained for 4 minutes until the material is uniform;

[0056] 4) The temperature of the main pot is lowered to 40°C, the anti-corrosion system is added, and after stirring evenly, the neutralizer is added until the material is uniform;

[0057] 5) After the temperature of the main pot is lowered to 38°C, it is detected and discharged.

[0058] Performance Test

[0059] 1. Particle size test: The particle sizes in Examples 1-7 and Comparative Examples 1-6 were tested using a microscope. The test picture of Example 1 is shown in Figure 1 .

[0060] 2. Centrifugal stability: The products prepared in Examples 1-7 and Comparative Examples 1-6 were centrifuged at 3000 r / min for 30 minutes, and it was observed whether there was a layering problem. After centrifugation, Comparative Example 1 showed a layering problem. No layering was considered to pass the test, and layering was considered to fail the test. The test picture is shown in Figure 2 .

[0061] 3. High and low temperature stability: Store the products prepared in Examples 1-7 and Comparative Examples 1-6 at -18°C for 7 to 30 days and at 48°C for 7 to 30 days, and observe whether there are any problems with abnormal stability. In Comparative Example 5, a tofu-like phenomenon occurred after low-temperature freeze-thawing. See the picture in Figure 3 .

[0062] The test results are shown in Table 3.

[0063] Table 3

[0064]

[0065] The self-emulsifying composition of this oil in formula application and performance testing

[0066] Application of the essence in Example 8

[0067]

[0068]

[0069] Preparation steps:

[0070] 1) Add the aqueous phase, thickener, and humectant to the aqueous phase pot in sequence. After stirring evenly at room temperature, heat up to 83°C and continue stirring until the material is uniform. Then pump it into the main pot and keep it warm for use;

[0071] 2) Add the oil phase and the self-emulsifying oil composition to the oil phase pot in sequence. After stirring evenly at room temperature, heat up to 83°C and keep it warm for use;

[0072] 3) Start the main pot for low-speed homogenization at 2500 rpm, slowly pump the oil phase into the main pot. After the oil phase is pumped in completely, start high-speed homogenization at 5000 rpm and keep it for 4 minutes until the material is uniform;

[0073] 4) Cool the main pot to 40°C, add the anti-corrosion system and fragrance, stir evenly, and then add the neutralizer until the material is uniform;

[0074] 5) After the main pot is cooled to 38°C, detect and discharge the material.

[0075] Particle size: 1-3 μm.

[0076] Passed centrifugation.

[0077] Passed 3-month stability test.

[0078] Sensitive skin suitability test:

[0079] Scheme Design: Use a closed patch to damage the skin barrier function on the flexor side of the forearms, induce dermatitis symptoms artificially, and then use the test product for repair. Set a blank control and adopt random grouping measures to reduce or control bias; the evaluation indicators are (1) skin stratum corneum water content, transepidermal water loss rate of the skin, and skin color. (2) Environmental conditions: The laboratory environmental temperature is 21°C, and the relative humidity is 50%. (3) Product usage method: Take an appropriate amount on the arm test area and gently apply it until absorbed.

[0080] Test Procedure

[0081] (1) On the test day, the subject arrives, and the staff explains the test to the subject, and the subject signs the informed consent form. (2) The subject cleans the test site with clean water, gently dries it with a dry towel, marks the test sites on the inner sides of both arms, and the staff uses SLS to establish a skin barrier damage model. (3) After 24 hours, remove the patch, sit quietly in the constant temperature and humidity efficacy laboratory for 30 minutes, and measure the skin stratum corneum water content, transepidermal water loss rate of the skin, and skin color parameters of the test site of the subject respectively. (4) The staff distributes the test samples, and the subject uses the test samples continuously for 14 days according to the sample usage instructions. (5) The staff repeats the parameter measurement in step (3) on D3 and D7 respectively.

[0082] Test Instruments

[0083] (1) Skin stratum corneum water content measuring instrument CM825 is used to detect the skin stratum corneum water content. The increase in the measured value indicates a higher skin stratum corneum water content. (2) Transepidermal water loss rate measuring instrument of the skin TM300 is used to detect the transepidermal water loss rate of the skin. The decrease in the measured value indicates better water-locking ability of the skin and better skin barrier function. (3) Skin color measuring instrument Colorimeter CL400 is used to detect the color of the skin surface. The larger the measured value of L*, the brighter the color; the larger the measured value of a*, the more reddish the color; the larger the measured value of b*, the more yellowish the color.

[0084] Test Results:

[0085] 1) Skin stratum corneum water content ( CM825)

[0086] The increase in the measured value indicates a higher skin stratum corneum water content.

[0087] Table of skin stratum corneum water content

[0088]

[0089] Change rate =

(Water content of stratum corneum after trial - Water content of stratum corneum before trial) / Water content of stratum corneum before trial

[0090] Compared to pre-treatment, the average moisture content of the stratum corneum in the test area significantly increased by 77.04% at the follow-up time point D3 and by 189.40% at the follow-up time point D7. Compared to the blank sample change values, the change in moisture content in the stratum corneum in the test area showed significant differences at the follow-up time points D3 and D7.

[0091] Transepidermal water loss (TEWL) TM300)

[0092] A decrease in the measured value indicates that the skin's ability to lock in moisture is better and the skin barrier function is better.

[0093] 2) Transepidermal water loss rate ( TM300)

[0094] A decrease in the measured value indicates that the skin's ability to lock in moisture is better and the skin barrier function is better.

[0095] Transepidermal water loss rate

[0096]

[0097] Change rate = [(transepidermal water loss rate after trial - transepidermal water loss rate before trial) / transepidermal water loss rate before trial] * 100%

[0098] Compared to pre-treatment with the sample, the average transepidermal water loss (TEWL) rate in the test area significantly decreased by 12.42% at the follow-up time point D3 and by 25.92% at the follow-up time point D7. Compared to the change values of the blank sample, the TEL rate change in the test area showed significant differences at the follow-up time point D3 and at the follow-up time point D7.

[0099] 3) Skin color (Colorimeter CL400)

[0100] As the measured value a* increases, the skin color becomes more red.

[0101] Table skin color a*

[0102]

[0103] Change rate = [(skin color after trial a *-Skin color before trial a *) / Skin color before trial a 100%

[0104] Compared with before using the trial samples, the average skin color in the test area decreased significantly by 6.15% at the follow-up time point D3 and by 20.77% at the follow-up time point D7. Compared with the change value of the blank sample, there was no significant difference in the skin color change value in the test area at the follow-up time point D3, and there was a significant difference at the follow-up time point D7.

[0105] 4) Results of self-assessment by subjects and statistical analysis

[0106] A total of 35 subjects were enrolled, and 1 subject withdrew (due to personal reasons); the number of valid subjects was 34, including 12 males and 22 females, aged 19 - 36 years, with an average age of 25.88 ± 3.36 years.

[0107] After using the test product for 14 days, 91% of the subjects agreed that their skin became more elastic and tender after use; 97% of the subjects agreed that their skin was moisturized after use; 88% of the subjects agreed that their skin was delicate and shiny after use; 97% of the subjects agreed that their skin became more moisturized after use; 85% of the subjects agreed that their skin became more elastic; 88% of the subjects agreed that their skin became more firm; 85% of the subjects agreed that the degree of skin tingling was reduced; 82% of the subjects agreed that skin flushing was improved; 91% of the subjects agreed that skin discomfort was relieved; 94% of the subjects agreed that it was mild and comfortable. During the period of using the sample, 0 cases of skin adverse reactions occurred in sensitive skin subjects.

[0108] Conclusion of the trial

[0109] Through the use of the essence by 34 sensitive skin subjects for the efficacy tests of cosmetics in terms of moisturizing, soothing, repairing, firming, mildness and suitability for sensitive skin, the results showed that: (1) 0 cases of adverse reaction occurred in the subjects. (2) Objective quantitative evaluation analysis showed that compared with before using the product, after using the product, the water content of the skin stratum corneum of the subjects increased significantly, the trans-epidermal water loss rate decreased significantly, and the skin color a* value decreased significantly. Compared with the blank change value, after using the product, the water content of the skin stratum corneum of the subjects increased significantly, the trans-epidermal water loss rate decreased significantly, and the skin color a* value decreased significantly. (3) Subjective evaluation analysis of the subjects showed that after using the test product, statistically more than 50% of the subjects gave positive evaluations to all parameters in terms of the appearance, smell, texture, skin feel, etc. of the test product; statistically more than 50% of the subjects gave positive evaluations to all parameters in terms of the moisturizing, soothing, firming, mildness, etc. of the test product. In summary, under the conditions of this experiment, the product has the effects of moisturizing, soothing, repairing and firming, is mild and suitable for sensitive skin.

Claims

1. An auto-emulsifying oil-fat composition, characterized in that, The raw materials for preparing the self-emulsifying oil composition include, by weight: 0.1 - 0.5 parts of long-chain alkyl glyceryl ether, and 0.1 - 2.0 parts of oil emulsification stabilizer; The long-chain alkyl glyceryl ether is batyl alcohol; The oil emulsification stabilizer is selected from one or a combination of several of Phytosoothe LS 9766 and hydrogenated coconut oil glyceride.

2. Use of the self-emulsifying oil composition according to claim 1, characterized in that, When applied to cosmetics, the cosmetics are selected from one of lotion, essence, cream, and facial mask liquid.

3. Use of the self-emulsifying oil and fat composition according to claim 2, characterized in that In the preparation of the cosmetics in the above application, the raw materials include, by weight: 0.1 - 0.5 parts of thickener, 0.1 - 25 parts of oil phase, 0.2 - 2.5 parts of self-emulsifying oil composition, 0.2 - 1 part of preservative system, 0.1 - 10 parts of auxiliary components, and the water phase is supplemented to 100 parts.

4. Use of the self-emulsifying oil-fat composition according to claim 3, characterized in that, The thickener is selected from one or a combination of several of PEMULEN™ TR-1 Polymer, Carbopol Ultrez 30 Polymer, PEMULEN™ TR-2 Polymer, CARBOPOL® 981 Polymer, CARBOPOL® 980 Polymer, xanthan gum, SEPINOV EMT 10, AristoflexSilk, Aristoflex AVC, AQUPEC HV-501E, AQUPEC HV-505E, and SEPIMAX ZEN.

5. Use of the self-emulsifying oil composition according to claim 3, characterized in that, The oil phase is selected from one or a combination of the following: polydimethylsiloxane, cetearyl alcohol, beeswax, microcrystalline wax, behenyl alcohol, cetyl alcohol, stearyl alcohol, stearic acid, glyceryl behenate-eicosanedioate, isononyl isononanoate, isocetyl isononanoate, ethylhexyl palmitate, cetyl ethylhexanoate, glyceryl tri(ethylhexanoate), caprylic / capric triglyceride, caprylic / capric / lauric / stearic triglyceride, olive fruit oil, sunflower seed oil, squalane, shea butter, jojoba seed oil. 12-13 The alcohol lactate, pentaerythrityl tetra(isononanoate), distearyl malate, caprylic / capric / myristic / stearic triglyceride, and one or a combination of the above.

6. Use of the self-emulsifying oil and fat composition according to claim 3, characterized in that, The water phase includes, by weight: 1 - 10 parts of glycerol, 1 - 8 parts of polyol, and water is supplemented to 100 parts.

7. Use of the self-emulsifying oil composition according to claim 3, characterized in that, The auxiliary components are selected from one or a combination of several of thickener, humectant, skin protectant, and neutralizer.

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