Composition for promoting the formation of liquid crystal structure of cosmetics, preparation method and application thereof
The preparation of squalane liposomes through high-pressure homogenization method and combined with hydrogenated lecithin and other components has solved the problem of the reduction of the number of liquid crystals or the structure of liquid crystals during storage, and achieved the stability of the liquid crystal structure in cosmetics and The number of improvements improves moisturizing performance and skin feeling experience.
Patent Information
- Application Number
- CN202411631405.5
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-11-15
- Publication Date
- 2025-02-11
- Estimated Expiration
- 2044-11-15
AI Technical Summary
During the storage process, existing liquid crystal skin care products are prone to the problem of reducing the number of liquid crystals or disappearing the structure, which limits the application of liquid crystals in skin care products.
Squalane liposomes are prepared by high-pressure homogenization method, combined with hydrogenated lecithin and other components to form a stable liquid crystal structure, changing the oil solubility of squalane, so that it can be directly applied to aqueous systems.
It has achieved the improvement of the stability and quantity of liquid crystal structure in cosmetics, can be stored for a long time under different extreme conditions, and improved the moisturizing performance and skin feeling experience of cosmetics.
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Figure CN119112695B_ABST
Abstract
Description
Technical Field
[0001] The present invention belongs to the technical field of cosmetic preparations, and in particular relates to a composition for promoting the formation of a cosmetic liquid crystal structure, and a preparation method and application thereof. Background Art
[0002] Liquid crystal structure is an intermediate state that has some properties of crystals and liquids, and has the fluidity of liquids and the anisotropy of crystals. Liquid crystals have physical properties such as order and easy phase deformation, and are widely present in biological organisms. Biomolecules such as polypeptides, proteins, nucleic acids, lipids, polysaccharides, etc. in organisms often exist in the form of liquid crystals in solutions. These biomolecules are closely related to the growth and development of organisms, metabolism of the body, energy conversion of cells, information transmission, material transmission and other activities. The biological membrane itself is a double-layer membrane composed of flowing amphiphilic lipid molecules mainly composed of phospholipids and cholesterol. It has the characteristics of fluidity and regularity, and is also a typical liquid crystal substance.
[0003] Meridians are closely related to the functional activities of various organs in the human body and the occurrence of diseases. In recent years, new progress has been made in the study of meridians. Professor Deng Liangyue's team found that when acupoints are stimulated, specific liquid crystal substances rich in phospholipids and proteins can appear along the gaps in the meridian tissues. These gaps have low flow resistance characteristics, and liquid crystal substances are related to the regulatory effects of meridians. Fudan University Fei Lun's research team found that the material basis of human meridian acupoints is based on connective tissue, and the blood vessels, nerve plexuses and lymphatic vessels therein are interwoven into a complex system. These material structures are enriched with elements such as Ca, P, K, Fe, Zn, and Mn, and also contain liquid crystal collagen fibers that can exhibit the characteristics of high-efficiency transmission of infrared light. These research results provide a new perspective on the potential connection between the functionality of meridians and the biological effects of liquid crystal substances.
[0004] In terms of skin health care, the liquid crystal emulsification system can simulate the healthy skin barrier structure and repair damaged skin barriers due to its unique multi-layer structure of water, liquid crystal and oil, which is similar to the human epidermal tissue and intercellular matrix structure. At the same time, liquid crystal can be used as a "microcapsule" to encapsulate and protect active ingredients. However, at present, due to the stability of liquid crystal, liquid crystal skin care products often have a phenomenon of reduced amount of liquid crystal or even disappearance of structure during storage, which limits the application of liquid crystal in skin care products.
[0005] Squalane is a common raw material for skin care products and is also the closest lipid to human sebum, with good moisturizing and emollient effects. The present invention uses liposome carrier technology to construct squalane liposomes to obtain a composition that can promote the formation of cosmetic liquid crystal structures. The composition can change the oil solubility of squalane and allow squalane to be directly applied to aqueous systems; at the same time, the composition exists in the form of squalane liposomes, and forms a stable liquid crystal structure through supramolecular self-assembly, which effectively solves the problem of poor stability of the liquid crystal state in lotion and cream skin care products, and has broad application prospects. Summary of the invention
[0006] The present invention aims at the problems existing in the prior art and provides a composition for promoting the formation of liquid crystal structure of cosmetics and a preparation method and application thereof. The present invention uses cosmetic raw materials with high biological safety, prepares squalane liposomes (composition for promoting the formation of liquid crystal structure of cosmetics) by high-pressure homogenization method, and prepares liposomes with good stability and long-term storage under different extreme conditions by investigating the compatibility of phospholipid components. The whole process does not introduce organic reagents, is environmentally friendly and safe, is simple to operate, and can achieve scale-up production.
[0007] The squalane liposomes prepared by the present invention can change the oil solubility of squalane, can be directly used in the development of cosmetics of an aqueous system, and can also promote absorption, enhance skin feel and moisturizing performance; in the application process of cosmetics, the squalane liposomes of the present invention (compositions for promoting the formation of liquid crystal structures of cosmetics) can self-assemble with other ingredients, promote the formation of liquid crystal structures in cosmetics, increase the amount of liquid crystals in cosmetics and maintain long-term stability, and the promotion effect is dosage-dependent.
[0008] In order to achieve the above-mentioned purpose, in the first aspect, the present invention provides a composition for promoting the formation of liquid crystal structure of cosmetics, wherein the composition for promoting the formation of liquid crystal structure of cosmetics is in the form of squalane liposomes and comprises the following raw materials by weight percentage: squalane 10%-28%, hydrogenated lecithin 1%-3.5%, cholesterol 0.3%-1%, glycerol 55%-65% and the remainder water.
[0009] In a preferred embodiment, the hydrogenated lecithin is selected from at least one of NIKKOL LECINOL S-10, LIPOIDS75, PHOSPHOLIPON 80H, and Soya SPL 75H.
[0010] Preferably, the hydrogenated lecithin is NIKKOL LECINOL S-10.
[0011] In a preferred embodiment, the squalane is selected from at least one of animal squalane, plant squalane and synthetic squalane.
[0012] In a preferred embodiment, the animal squalane source is shark liver; the plant squalane sources include soybean oil, corn oil, rice bran oil, sunflower oil, olive oil, sugar cane, camellia and wheat germ oil; and the synthetic squalane is hydrogenated polyisobutene.
[0013] Preferably, the composition for promoting the formation of liquid crystal structure of cosmetics comprises the following raw materials by weight percentage: 15%-25% squalane, 1.5%-2.5% hydrogenated lecithin, 0.5%-0.75% cholesterol, 57%-63% glycerol and the remainder water.
[0014] In a preferred embodiment, the composition for promoting the formation of liquid crystal structure in cosmetics comprises the following raw materials by weight percentage: 20% squalane, 2% hydrogenated lecithin, 0.63% cholesterol, 60% glycerol and the remainder water.
[0015] In a preferred embodiment, the water is purified water.
[0016] Preferably, the composition for promoting the formation of liquid crystal structure of cosmetics is a composition that can change the oil solubility of squalane and enable squalane to be directly applied to an aqueous system.
[0017] Preferably, the composition for promoting the formation of liquid crystal structures in cosmetics, when applied to cosmetics, can promote the formation of liquid crystal structures, and increase the number and stability of liquid crystal structures.
[0018] In a second aspect, the present invention provides a method for preparing the aforementioned composition for promoting the formation of a liquid crystal structure in cosmetics, comprising the following steps:
[0019] (1) Mix glycerol and hydrogenated lecithin, add water, and heat to dissolve to obtain an aqueous phase;
[0020] (2) mixing squalane and cholesterol, and heating to dissolve them to obtain a mixture of squalane and cholesterol;
[0021] (3) adding the mixture of squalane and cholesterol from step (2) to the aqueous phase from step (1) under high-speed shearing conditions of 10,000-20,000 rpm for pre-homogenization;
[0022] (4) 7250-29000psi high pressure homogenization to obtain a composition that promotes the formation of liquid crystal structure of cosmetics.
[0023] In a preferred embodiment, in step (1), the heating temperature is 80-95°C.
[0024] Further preferably, in step (1), the heating temperature is 90°C.
[0025] In a preferred embodiment, in step (2), the heating temperature is 80-95°C.
[0026] Further preferably, in step (2), the heating temperature is 90°C.
[0027] In a preferred embodiment, in step (3), the pre-homogenization treatment is carried out at 12000-18000 rpm for 1-5 min.
[0028] Further preferably, in step (3), the pre-homogenization treatment condition is: 15000 rpm for 3 min.
[0029] In a preferred embodiment, in step (4), the high pressure homogenization conditions are: 11600-21750 psi, 10-60° C., and homogenization for 2-10 times.
[0030] Further preferably, in step (4), the high pressure homogenization conditions are: homogenization at 14500 psi and 10°C for 8 times.
[0031] In a third aspect, the present invention provides an application of a composition for promoting the formation of a liquid crystal structure of cosmetics in the preparation of cosmetics, wherein the cosmetics include facial creams, lotions, toners, essence water, eye creams and cleansing cosmetics;
[0032] The components of the facial cream include:
[0033] Phase A: emulsifier, co-emulsifier, squalane, polydimethylsiloxane, isononyl isononanoate, shea butter and VE acetate,
[0034] Phase B: water, glycerin, butylene glycol, EDTA-2Na, xanthan gum and thickener,
[0035] Phase C: a composition that promotes the formation of liquid crystal structures in cosmetics.
[0036] Phase D: Betaine and dipotassium glycyrrhizinate,
[0037] Phase E: Butylene glycol and hyaluronic acid,
[0038] Phase F: preservative;
[0039] The components of the emulsion include:
[0040] Phase A: emulsifier, co-emulsifier, squalane, emollient oil and VE acetate,
[0041] Phase B: water, glycerin, thickener and EDTA-2Na,
[0042] Phase C: a composition that promotes the formation of liquid crystal structures in cosmetics.
[0043] Phase D: Betaine, Hydroxyethyl Urea, Humectants and Preservatives,
[0044] Phase E: arginine;
[0045] The components of the essence water include:
[0046] Phase A: water, glycerin, PEG-1450, glyceryl polyether-26, allantoin, EDTA-2Na, thickener and trehalose,
[0047] Phase B: Butylene glycol and hyaluronic acid,
[0048] Phase C: moisturizer,
[0049] Phase D: 1,2-pentanediol, p-hydroxyacetophenone and dipropylene glycol,
[0050] Phase E: Compositions and preservatives that promote the formation of liquid crystal structures in cosmetics.
[0051] In a preferred embodiment, when the cosmetic is a facial cream, the emulsifier is selected from at least one of M202 and A165; and the co-emulsifier is 16 / 18 alcohol.
[0052] In a preferred embodiment, when the cosmetic is an emulsion, the emulsifier is A165, the co-emulsifier is 16 / 18 alcohol, and the humectant is sodium PCA.
[0053] In a preferred embodiment, when the cosmetic is essence water, the moisturizing agent is selected from at least one of trehalose, PEG-1450, PQ-51, and PCA sodium.
[0054] In a preferred embodiment, the composition for promoting the formation of liquid crystal structure of cosmetics is used in the preparation of cosmetics, and the preparation method of the cosmetics comprises the steps of: heating phase A and phase B to 70-80°C respectively, homogenizing at 11000rpm-15000rpm for 1-3min after mixing, stirring and cooling to 45-55°C, adding ingredients of other phases in sequence, mixing evenly to obtain cosmetics.
[0055] Further preferably, the method for preparing the cosmetic comprises the steps of: heating phase A and phase B to 80°C respectively, homogenizing at 13000 rpm for 2 min after mixing, cooling to 50°C with stirring, adding ingredients of other phases in sequence, and mixing evenly to obtain the cosmetic.
[0056] In a fourth aspect, the present invention provides a cosmetic having a high amount of liquid crystal structures and high liquid crystal structure stability, high moisturizing properties and a comfortable skin feel, the components of which include the aforementioned composition for promoting the formation of cosmetic liquid crystal structures.
[0057] In a preferred embodiment, the cosmetics having a high amount of liquid crystal structures and high liquid crystal structure stability include face cream, lotion, eye cream, facial cleanser, toner and essence water.
[0058] In a preferred embodiment, when the cosmetic having a high amount of liquid crystal structures and high liquid crystal structure stability is a face cream, the components include:
[0059] Phase A includes components: M202, A165, 16 / 18 alcohol, squalane, DC200 / 100cst, IN99, shea butter and VE acetate;
[0060] Phase B includes components: water, glycerin, butylene glycol, EDTA-2Na, xanthan gum and EMT-10;
[0061] Phase C includes components: a composition that promotes the formation of liquid crystal structure of cosmetics;
[0062] Phase D includes components: betaine and dipotassium glycyrrhizinate;
[0063] Phase E includes components: butanediol and HA;
[0064] Phase F includes the components: HCP.
[0065] In a preferred embodiment, when the cosmetic having a high amount of liquid crystal structures and high liquid crystal structure stability is an emulsion, the components include:
[0066] Phase A includes components: A165, 16 / 18 alcohol, squalane, DC345 and VE acetate;
[0067] Phase B includes components: water, glycerol, TR-1 and EDTA-2Na;
[0068] Phase C includes components: a composition that promotes the formation of liquid crystal structure of cosmetics;
[0069] Phase D includes components: betaine, hydroxyethyl urea, sodium PCA, and HCP;
[0070] Phase E includes the components: arginine.
[0071] In a preferred embodiment, the method for preparing the cosmetic having a high amount of liquid crystal structures and high liquid crystal structure stability comprises the steps of:
[0072] Phase A and phase B are heated to 70-80°C respectively, homogenized at 11000rpm-15000rpm for 1-3min after mixing, cooled to 45-55°C with stirring, and ingredients of other phases are added in sequence and mixed evenly to obtain cosmetics with high liquid crystal structure quantity and high liquid crystal structure stability.
[0073] Further preferably, the method for preparing the cosmetics having a high number of liquid crystal structures and high liquid crystal structure stability comprises the steps of:
[0074] Phase A and phase B are heated to 80°C respectively, homogenized at 13000 rpm for 2 minutes after mixing, cooled to 50°C with stirring, and ingredients of other phases are added in sequence and mixed evenly to obtain cosmetics with a high amount of liquid crystal structures and high liquid crystal structure stability.
[0075] Compared with the prior art, the present invention has the following beneficial effects:
[0076] 1. The present invention uses cosmetic raw materials with high biosafety to prepare squalane liposomes (compositions for promoting the formation of cosmetic liquid crystal structures) by a high-pressure homogenization method. The whole process does not introduce organic reagents, and the operation is simple, and scale-up production can be achieved. The squalane liposomes (compositions for promoting the formation of cosmetic liquid crystal structures) of the present invention have good stability and can be stored for a long time under different extreme conditions.
[0077] 2. The composition for promoting the formation of liquid crystal structure of cosmetics prepared by the present invention can change the oil solubility of squalane, realize direct addition in the aqueous system, and has the effects of promoting absorption, improving the skin feel experience and moisturizing performance of cosmetics.
[0078] 3. The composition for promoting the formation of liquid crystal structure in cosmetics of the present invention can self-assemble with other ingredients in cosmetics to promote the formation of liquid crystals in cosmetics, and this phenomenon becomes more obvious with the increase of the amount of liposomes added, and the liquid crystal structure can exist stably for a long time. BRIEF DESCRIPTION OF THE DRAWINGS
[0079] Figure 1 This is the particle size distribution diagram of the squalane liposomes in Example 1.
[0080] Figure 2 This is a diagram showing the morphology of the squalane liposomes of Example 1.
[0081] Figure 3 This is a graph showing the storage stability results of the squalane liposomes of Example 1.
[0082] Figure 4 This is a graph showing the high and low temperature cycling stability results of the squalane liposomes of Example 1.
[0083] Figure 5 This is a graph showing the short-term moisturizing effect of squalane and the squalane liposomes of Example 1.
[0084] Figure 6 This is a diagram showing the observation result of the squalane liposomes of Example 1 under a polarizing microscope.
[0085] Figure 7This is a diagram showing the liquid crystal observation results of squalane liposome cream A.
[0086] Figure 8 This is a diagram showing the liquid crystal observation results of squalane liposome cream B.
[0087] Fig. 9 This is a diagram showing the liquid crystal observation results of squalane liposome emulsion.
[0088] Fig.10 This is the result chart of the short-term moisturizing effect of Essence Water 1 and Essence Water 2. DETAILED DESCRIPTION
[0089] The following non-limiting examples can enable those skilled in the art to more fully understand the present invention, but do not limit the present invention in any way. The following content is merely an exemplary description of the scope of the present invention, and those skilled in the art can make various changes and modifications to the present invention based on the disclosed content, which should also fall within the scope of the present invention.
[0090] When the embodiments give numerical ranges, it should be understood that, unless otherwise specified in the present invention, both endpoints of each numerical range and any numerical value between the two endpoints can be selected. Unless otherwise defined, all technical and scientific terms used in the present invention have the same meanings as those generally understood by those of ordinary skill in the art to which the present invention belongs.
[0091] The present invention is further described below by way of specific examples. Unless otherwise specified, the various chemical reagents used in the examples of the present invention are obtained through conventional commercial channels, and their sources are not specifically limited.
[0092] In the following examples, the squalane used is hydrogenated polyisobutylene (MC30), purchased from SOPHIM. In the present invention, different types of squalane have no significant effect on the technical effect, and all can achieve the technical effect described in the present application.
[0093] The following sources of raw materials or equipment are provided as examples:
[0094] Hydrogenated lecithin: Model NIKKOL LECINOL S-10 (S-10), purchased from Japan Surfactant Industry Co., Ltd.; Model PHOSPHOLIPON 90H (90H), purchased from Lipoid Kosmetik AG; Model PHOSPHOLIPON 90G (90G) purchased from Lipoid Kosmetik AG; Model LIPOID S75 (S-75), purchased from Lipoid Kosmetik AG; Model PHOSPHOLIPON 80H (80H) purchased from Lipoid Kosmetik AG; Model Soya SPL 75H (75H) purchased from Neuropid Co., Ltd.
[0095] Cholesterol: purchased from Zhejiang Zhongxian Biotechnology Co., Ltd.;
[0096] Emulsifier: M202, purchased from SEPPIC SA;
[0097] Emulsifier: A165, purchased from Evonik Operations GmbH;
[0098] Co-emulsifier: 16 / 18 alcohol, purchased from Edenor Oleochemicals (M) Sdn. Bhd.;
[0099] Emollients: DC345 (cyclopentasiloxane), XIAMETER™ PMX-0345 CyclosiloxaneBlend, purchased from Dow (Zhangjiagang) Investment Co., Ltd.;
[0100] Caprylic / capric triglyceride: GTCC, purchased from Croda Singapore Pte Ltd;
[0101] Polydimethylsiloxane: DC200 / 100cst, purchased from Dow (Zhangjiagang) Investment Co., Ltd.;
[0102] Isononyl isononanoate: IN99, purchased from SEPPIC SA;
[0103] Shea butter: purchased from OLVEA;
[0104] VE acetate: purchased from BASF (China) Co., Ltd.;
[0105] Xanthan gum: purchased from Finnfeed Finland Oy;
[0106] EDTA-2Na: purchased from Nouryon Chemicals (Ningbo) Co., Ltd.;
[0107] Thickener: EMT-10, purchased from SEPPIC SA;
[0108] Betaine: purchased from Finnfeeds Finland Oy;
[0109] Hyaluronic acid: HA, purchased from Bloomage Biotech Co., Ltd.;
[0110] Preservative: HCP, purchased from INOLEN;
[0111] Moisturizer: PEG-1450, purchased from Dow Chemical (Shanghai) Co., Ltd.;
[0112] Glycerol polyether-26: EG-1, purchased from Borui (Guangzhou) New Material Technology Co., Ltd.;
[0113] Allantoin: purchased from Clariant Chemicals (China) Co., Ltd.
[0114] Thickener: 389, purchased from Danisco (China) Investment Co., Ltd.;
[0115] Thickener: ZEN, purchased from SEPPIC SA;
[0116] Moisturizer: Trehalose, purchased from Hayashibara Co., Ltd.;
[0117] Moisturizer: PQ-51, purchased from NOF CORPORATION;
[0118] Moisturizer: sodium PCA, purchased from Ajinomoto, Japan;
[0119] Thickener: TR-1, purchased from The Lubrizol Corporation;
[0120] 10% arginine: purchased from Dezhixin Flavors (Nantong) Co., Ltd.; the remaining raw materials are all commercially available.
[0121] Example 1 and Comparative Examples 1 to 5
[0122] The formula of the composition for promoting the formation of liquid crystal structure of cosmetics is shown in Table 1 according to weight percentage:
[0123] Table 1
[0124]
[0125] The preparation method of the composition for promoting the formation of liquid crystal structure of cosmetics is as follows:
[0126] (1) Mix glycerol and hydrogenated lecithin, add water, and heat to 90°C to dissolve to obtain an aqueous phase;
[0127] (2) After mixing squalane and cholesterol, heat to 90°C to dissolve, thereby obtaining a mixture of squalane and cholesterol;
[0128] (3) adding the mixture of squalane and cholesterol from step 2) to the aqueous phase of step 1) under high-speed shearing conditions of 15,000 rpm, and performing pre-homogenization for 3 minutes;
[0129] (4) High pressure homogenization was performed at 14500 psi and 10°C for 8 times to obtain a composition (squalane liposome) that promotes the formation of a cosmetic liquid crystal structure.
[0130] Example 2
[0131] A composition for promoting the formation of liquid crystal structure of cosmetics, comprising the following raw materials by weight: 15% squalane, 1.5% hydrogenated lecithin (S-10), 0.5% cholesterol, 57% glycerol and 26% water.
[0132] The preparation method of the composition for promoting the formation of liquid crystal structure of cosmetics is as follows:
[0133] (1) Mix glycerol and hydrogenated lecithin, add water, and heat to 80°C to dissolve to obtain an aqueous phase;
[0134] (2) After mixing squalane and cholesterol, heat to 80°C to dissolve, thereby obtaining a mixture of squalane and cholesterol;
[0135] (3) adding the mixture of squalane and cholesterol from step 2) to the aqueous phase of step 1) under high-speed shearing conditions of 10,000 rpm, and performing pre-homogenization for 5 minutes;
[0136] (4) High pressure homogenization was performed at 29,000 psi and 15°C for 6 times to obtain a composition (squalane liposome) that promotes the formation of a cosmetic liquid crystal structure.
[0137] Example 3
[0138] A composition for promoting the formation of liquid crystal structure of cosmetics, comprising the following raw materials in parts by weight: 25% squalane, 2.5% hydrogenated lecithin (S-10), 0.75% cholesterol, 63% glycerol and 8.75% water.
[0139] The preparation method of the composition for promoting the formation of liquid crystal structure of cosmetics is as follows:
[0140] (1) Mix glycerol and hydrogenated lecithin, add water, and heat to 95°C to dissolve to obtain an aqueous phase;
[0141] (2) After mixing squalane and cholesterol, heat to 95°C to dissolve, thereby obtaining a mixture of squalane and cholesterol;
[0142] (3) under high-speed shearing conditions of 20,000 rpm, the mixture of squalane and cholesterol obtained in step 2) was added to the aqueous phase of step 1) and pre-homogenized for 2 minutes;
[0143] (4) High pressure homogenization at 7250 psi and 10°C was performed 10 times to obtain a composition (squalane liposome) that promotes the formation of a cosmetic liquid crystal structure.
[0144] Example 4
[0145] A composition for promoting the formation of liquid crystal structure of cosmetics, comprising the following raw materials by weight: 10% squalane, 1% hydrogenated lecithin (S-75), 0.3% cholesterol, 55% glycerol and 33.7% water.
[0146] The rest are the same as in Example 1.
[0147] Example 5
[0148] A composition for promoting the formation of liquid crystal structure of cosmetics, comprising the following raw materials in parts by weight: 28% squalane, 3.5% hydrogenated lecithin (80H), 1% cholesterol, 65% glycerol and 2.5% water.
[0149] The rest are the same as in Example 1.
[0150] Example 6
[0151] A composition for promoting the formation of liquid crystal structure of cosmetics, comprising the following raw materials by weight: 20% squalane, 3% hydrogenated lecithin (75H), 1% cholesterol, 55% glycerol and 21% water.
[0152] The rest are the same as in Example 1.
[0153] Test Case
[0154] 1. Particle size characterization: The particle size of the squalane liposome (composition for promoting the formation of liquid crystal structure of cosmetics) of Example 1 was characterized by using Malvern Mastersizer 3000. The results are shown in Figure 1 .
[0155] The results showed that the average particle size of the squalane liposomes in Example 1 was 155 nm, and the particle size distribution range was 77-299 nm, and the particle size distribution was ideal.
[0156] 2. Electron microscopy characterization: The morphology of the squalane liposomes in Example 1 was characterized using an electron microscope (Hitachi SU8100 field emission scanning electron microscope). Figure 2 .
[0157] The results showed that the squalane liposomes in Example 1 were more in number and uniform in size.
[0158] 3. Stability observation
[0159] 3.1 Long-term storage at different temperatures and conditions
[0160] The squalane liposomes of the embodiment and the comparative example were stored under different conditions, and the average particle size (nm) was detected after a specific storage period. The storage stability test results of the squalane liposomes of the embodiment are shown in Tables 2.1 and 2.2; the storage stability test results of the squalane liposomes of the comparative example are shown in Table 2.3.
[0161] Table 2.1
[0162]
[0163] Table 2.2
[0164]
[0165] Table 2.3
[0166]
[0167] The storage stability results of the squalane liposomes of Example 1 are shown in Figure 3 , where the light is room temperature and natural light.
[0168] It can be seen from the investigation results that the squalane liposomes of the embodiment were stored for a long time under different conditions, and the particle size was analyzed on the 1st day, 3rd day, 8th day, 15th day, 30th day, 60th day, 105th day, 204th day and 270th day, respectively. It can remain stable for at least 270 days (9 months), and the particle size change is <30nm. The results show that the particle size of squalane liposomes is relatively stable.
[0169] The particle size of the squalane liposomes in Comparative Example 1 increased significantly (189 to 417 nm) after being stored under light for 90 days, the particle size of the squalane liposomes in Comparative Example 2 increased significantly (199 to 305 nm) after being stored under light for 60 days, the particle size of Comparative Example 3 changed significantly after being stored under different storage conditions for 1 day, the particle size of Comparative Example 4 changed by more than 30 nm after being stored at 45°C for 7 days, and the particle size of Comparative Example 5 changed by more than 30 nm after being stored under light or 45°C for 7 days, indicating that the long-term storage stability of the squalane liposomes in Comparative Examples 1 to Comparative Examples 5 is not good, and the difference between Comparative Examples 1 to Comparative Examples 5 and Example 1 is only the different types or dosage relationships of hydrogenated lecithin. It can be seen that for squalane liposomes, the type of hydrogenated lecithin and the dosage relationship of each component have a significant impact.
[0170] 3.2 Long-term storage under high and low temperature cycles
[0171] The high and low temperature cycling stability of the squalane liposomes in Example 1 was verified by detecting the average particle size (nm) before and after the cycle. The high and low temperature cycling stability results of the squalane liposomes are shown in Tables 3 and Figure 4 .
[0172] The results showed that the squalane liposomes of Example 1 were stored for a long time under high and low temperature cycling conditions (-15°C ~ 45°C), and the particle size was analyzed at the 2nd week, 3rd week, 4th week, 5th week, 6th week, 7th week, 8th week, 9th week, 10th week, 13th week, 19th week, 25th week, and 32nd week, respectively. The particle size can remain stable for at least 32 weeks (8 months), and the particle size change is <30nm. The results show that the particle size of squalane liposomes is relatively stable.
[0173] Table 3
[0174]
[0175] 3.3 Safety Assessment
[0176] The squalane liposomes of Example 1 were subjected to a human skin patch test, referring to the method of the skin closed patch test in the "Technical Specification for Safety of Cosmetics (2015 Edition)". Specifically, qualified patch test equipment was selected, and the closed patch test method was used. 0.020 mL of the test substance was placed in the patch tester, and a low-allergenic tape was applied to the inside of the subject's arm. The test substance was removed after 24 hours, and the skin reaction was observed 0.5 h, 24 h, and 48 h after removal, and the results were recorded according to the skin reaction grading standard in the "Technical Specification for Safety of Cosmetics (2015 Edition)".
[0177] The skin reaction scoring levels are shown in Table 4.1.
[0178] The summary results of cosmetic human skin patch tests are shown in Table 4.2.
[0179] Table 4.1
[0180]
[0181] Table 4.2
[0182]
[0183] Results: The results of the human skin patch test showed that no reaction occurred in 11 people, indicating that the squalane liposomes in Example 1 have good safety.
[0184] 3.4 Moisturizing efficacy test
[0185] The moisturizing effect of squalane and the squalane liposomes of Example 1 was verified by the following method: 140 healthy Chinese subjects with a stratum corneum moisture content of 20%-27% (Corneometer Unit, CU) at the arm test site were selected, and the age range was 25-40 years old. The test substance was used at a dosage of 2.0±0.1 mg / cm 2 , apply to an area of 3cm×3cm. Use the method of parallel comparison after using the product and before not using the product. Before using the test product (T 0 ), 1 hour after using the product (T 1 ) and 2 hours (T 2 ) were used to test the moisture content of the stratum corneum of the test parts of the subjects. The evaluation results before and after the use of the products were compared by statistical test methods to determine whether there were statistical differences. The test results of the moisture content of squalane and squalane liposomes in human skin are shown in Tables 5 and Figure 5 (20 people per group).
[0186] Table 5
[0187]
[0188] Results: The squalane liposomes of Example 1 had an immediate moisturizing effect within 2 hours after use, which was better than squalane.
[0189] 4. Formula application, liquid crystal observation, skin feel test
[0190] 4.1 Squalane liposomes
[0191] Experimental design: Squalane liposomes were observed under a polarizing microscope; eyepiece ×10, objective lens ×10, total magnification 100 times, the results are shown in Figure 6 It can be seen that the squalane liposomes of Example 1 themselves do not have liquid crystals under the observation conditions, but adding the squalane liposomes of the present invention to the preparation of cosmetics allows the cosmetics to produce a stable liquid crystal structure. The squalane liposomes of the present invention are an important component for promoting the liquid crystal structure of cosmetics.
[0192] 4.2 Facial Cream
[0193] Experimental design: Two base creams, Cream A and Cream B, were prepared, in which the oil content was the same, namely squalane and GTCC, respectively. 2% and 10% liposomes were added to the creams, and squalane or GTCC was reduced according to the proportion. No liposomes were added as a blank group to obtain squalane liposome cream A and squalane liposome cream B, respectively. The specific formulas of squalane liposome cream A and squalane liposome cream B are shown in Table 6. The liquid crystal was observed under a polarizing microscope. Figure 7-Figure 8, and recruited volunteers to conduct skin feel evaluation according to the "GB / T12315-2008 Sensory Analysis Methodology Ranking Method". The evaluators ranked the samples according to the standards (overall satisfaction), gave each sample a rank (i.e., rank), calculated the sum of the ranks, and then performed statistical comparisons. The results are shown in Tables 7 to 9.
[0194] Table 6
[0195]
[0196] Preparation process: Heat phase A and phase B to 80°C respectively, homogenize at 13000rpm for 2min after mixing; cool to 50°C with stirring, add phase C, D, E, and F in sequence, mix evenly, and discharge.
[0197] from Figure 7-Figure 8 It can be seen that after adding the squalane liposomes of Example 1, the degree of liquid crystallization of Cream A and Cream B is improved, and this state can still be maintained after being placed for 6 months.
[0198] Skin feel test of squalane liposome cream A and squalane liposome cream B: To further evaluate the application effect of squalane liposomes, 22 volunteers were recruited to evaluate the skin feel of squalane liposome cream A (1A, 2A and 3A) and cream B (1B, 2B and 3B). The results of the significance analysis of the overall skin feel satisfaction of squalane liposome cream A and cream B are shown in Table 7. The significant difference results in the results of Table 7 come from the comparison results of the sample rank sums statistically shown in Tables 8 and 9.
[0199] The ranking results and rank sum calculation results of skin satisfaction of squalane liposome cream A are shown in Table 8, and the ranking results and rank sum calculation results of overall skin satisfaction of squalane liposome cream B are shown in Table 9.
[0200] Table 7
[0201]
[0202] Table 8
[0203]
[0204] Table 9
[0205]
[0206] result:
[0207] ① Liquid crystal: Compared with the blank group (cream 1A and cream 1B), the squalane liposomes of Example 1 can significantly increase the amount of liquid crystals and maintain stability when used in the cream. The cream with squalane liposomes still has a lot of liquid crystals after being placed for 6 months. According to the observation results of the liquid crystal of squalane liposomes in part 4.1, the liquid crystal in the cream is not brought in by the liposomes; the liquid crystal phenomenon is enhanced after the addition of squalane liposomes to the cream, which shows that this phenomenon has nothing to do with the unencapsulated squalane in the formula.
[0208] ② Skin feel: The results show that there are significant differences in overall skin feel satisfaction among Cream 1A, Cream 2A, and Cream 3A, among which the rank sums of Cream 2A and Cream 3A are similar and greater than Cream 1A, indicating that the evaluators are more satisfied with the skin feel of Cream 2A and Cream 3A. There are significant differences in overall skin feel satisfaction among Cream 1B, Cream 2B, and Cream 3B, among which the rank sums of Cream 2B and Cream 3B are similar and greater than Cream 1B, indicating that the evaluators are more satisfied with the skin feel of Cream 2B and Cream 3B. This indicates that the application of the squalane liposomes of Example 1 in the cream can enhance the skin feel of the cream and give the formula a light and cool feeling.
[0209] 4.3 Emulsion
[0210] Experimental design: 5% and 10% squalane liposomes were added to the emulsion, and no squalane liposomes were added as a blank group to obtain squalane liposome emulsion. The formula of squalane liposome emulsion is shown in Table 10.
[0211] Preparation process: Phase A and phase B are heated to 80°C respectively, and homogenized at 13000rpm for 2min after mixing; cooled to 50°C with stirring, and phases C, D, and E are added in sequence, mixed evenly, and discharged.
[0212] The liquid crystal of the emulsion was observed under a polarizing microscope. The results are shown in Fig. 9 .
[0213] Twenty-two volunteers were recruited to evaluate the skin feel of three groups of lotions.
[0214] The results of the significance analysis of the overall satisfaction with the skin feel of squalane liposome emulsion are shown in Table 11. The significant differences in the results in Table 11 come from the sample rank sum comparison results statistically shown in Table 12.
[0215] The ranking results of skin satisfaction of squalane liposome emulsion and the calculation results of rank sum are shown in Table 12.
[0216] result:
[0217] ① Liquid crystal: Squalane liposomes can increase the amount of liquid crystals and promote their stability. Liquid crystals can still be present in the emulsion containing squalane liposomes after being left for 6 months.
[0218] ② Skin feel: The results show that there are significant differences in the overall satisfaction with skin feel among Lotion 1, Lotion 2 and Lotion 3, among which the rank sums of Lotion 2 and Lotion 3 are similar and greater than Lotion 1, indicating that the evaluators are more satisfied with the skin feel of Lotion 2 and Lotion 3. This indicates that the application of the squalane liposomes of Example 1 in the lotion can significantly improve the skin feel of the lotion, give the formula a light and thin feeling, and increase ductility.
[0219] Table 10
[0220]
[0221] Table 11
[0222]
[0223] Table 12
[0224]
[0225] 4.4 Essence Water
[0226] Experimental design: 5% squalane liposomes were added to the essence water, and no squalane liposomes were added as a blank group to obtain squalane liposome essence water. The formula of squalane liposome essence water is shown in Table 13. 22 volunteers were recruited to evaluate the skin feel of the two groups of essence waters. The results are shown in Tables 14-15, and the 2h short-term moisturizing effect was tested (the test method is the same as 3.4). The skin moisture content of the essence water (short-term moisturizing condition) is shown in Tables 16 and Fig.10 .
[0227] The results of the significance analysis of the satisfaction with the watery skin feel of squalane liposome essence are shown in Table 14. The significant differences in the results in Table 14 come from the comparison results of the sample rank sums statistically shown in Table 15.
[0228] The ranking results of the overall satisfaction with the watery skin feel of squalane liposome essence and the calculation results of the rank sum are shown in Table 15.
[0229] Table 13
[0230]
[0231] Preparation process: Phase A and phase B are heated to 80°C respectively, and homogenized at 13000rpm for 2min after mixing; cooled to 50°C with stirring, and phases C, D, and E are added in sequence, mixed evenly, and discharged.
[0232] Table 14
[0233]
[0234] Table 15
[0235]
[0236] Table 16
[0237]
[0238] result:
[0239] ① Skin feel: There is a significant difference in overall skin feel satisfaction between Essence Water 1 and 2, with Essence Water 2 being greater than Essence Water 1, indicating that the evaluators are more satisfied with the skin feel of Essence Water 2. This indicates that the squalane liposomes of Example 1 can be used in essence to bring a better water / oil skin feel.
[0240] ② Moisturizing effect: Squalane liposomes can achieve the stable addition of oil-soluble squalane in the essence, giving it stronger moisturizing properties.
[0241] The composition for promoting the formation of liquid crystal structure of cosmetics of the present invention: firstly, using cosmetic raw materials with high biosafety, squalane liposomes are prepared by high-pressure homogenization method, the whole process does not introduce organic reagents, and the operation is simple, and the scale-up production can be realized, and the obtained squalane liposomes have good stability and can be stored for a long time under different extreme conditions; secondly, squalane liposomes can change the oil solubility of squalane, and can be applied to various cosmetics such as aqueous systems / oily systems, thereby expanding the application scope of squalane in cosmetics; furthermore, when applied to the preparation of cosmetics, the composition for promoting the formation of liquid crystal structure of cosmetics of the present invention can self-assemble with other ingredients in the cosmetics, promote the formation of liquid crystal structure in the cosmetics, increase the number of liquid crystals in the cosmetics, and the liquid crystal structure and number can maintain long-term stability; in addition, the composition for promoting the formation of liquid crystal structure of cosmetics of the present invention can effectively improve the skin feel of the cosmetics, enhance the ductility, cooling feeling and moisturizing property of the cosmetics, and enhance the use experience of the product; finally, the composition for promoting the formation of liquid crystal structure of cosmetics of the present invention has a dose-dependent effect of promoting the formation of liquid crystal in cosmetic applications.
[0242] Finally, it should be noted that the above content is only used to illustrate the technical solution of the present invention, rather than to limit the scope of protection of the present invention. Simple modifications or equivalent substitutions of the technical solution of the present invention by ordinary technicians in this field do not deviate from the essence and scope of the technical solution of the present invention.
Claims
1. A composition for promoting the formation of liquid crystal structure in cosmetics, characterized in that: The composition for promoting the formation of liquid crystal structure of cosmetics is in the form of squalane liposomes, and comprises the following raw materials by weight percentage: squalane 10%-28%, hydrogenated lecithin 1%-3.5%, cholesterol 0.3%-1%, glycerol 55%-65% and the balance water; The hydrogenated lecithin is NIKKOL LECINOL S-10.
2. The composition for promoting the formation of liquid crystal structure in cosmetics according to claim 1, characterized in that: The invention comprises the following raw materials by weight percentage: squalane 15%-25%, hydrogenated lecithin 1.5%-2.5%, cholesterol 0.5%-0.75%, glycerol 57%-63% and the balance water.
3. The composition for promoting the formation of liquid crystal structure in cosmetics according to claim 1, characterized in that: The squalane is selected from at least one of animal squalane, plant squalane and synthetic squalane; The animal squalane is sourced from shark liver; The plant squalane sources include soybean oil, corn oil, rice bran oil, sunflower oil, olive oil, sugar cane, camellia and wheat germ oil; The synthetic squalane is hydrogenated polyisobutylene.
4. The method for preparing the composition for promoting the formation of liquid crystal structure of cosmetics according to any one of claims 1 to 3, characterized in that: The steps include: (1) Mix glycerol and hydrogenated lecithin, add water, and heat to dissolve to obtain an aqueous phase; (2) mixing squalane and cholesterol, and heating to dissolve them to obtain a mixture of squalane and cholesterol; (3) adding the mixture of squalane and cholesterol from step (2) to the aqueous phase from step (1) under high-speed shearing conditions of 10,000-20,000 rpm for pre-homogenization; (4) 7250-29000psi high pressure homogenization to obtain a composition that promotes the formation of liquid crystal structure of cosmetics.
5. The preparation method according to claim 4, characterized in that: In step (1), the heating temperature is 80-95°C; In step (2), the heating temperature is 80-95°C; In step (3), the pre-homogenization treatment conditions are: 12000-18000 rpm for 1-5 min; In step (4), the high pressure homogenization conditions are 11600-21750 psi, 10-60° C., and homogenization is performed 2-10 times.
6. Use of the composition for promoting the formation of liquid crystal structure in cosmetics according to any one of claims 1 to 3, characterized in that: The cosmetics include creams or lotions; The components of the facial cream include: Phase A: Emulsifier M202, Emulsifier A165, 16 / 18 alcohol, squalane, polydimethylsiloxane, isononyl isononanoate, shea butter and VE acetate, Phase B: water, glycerin, butylene glycol, EDTA-2Na, xanthan gum and thickener, Phase C: the composition for promoting the formation of liquid crystal structure of cosmetics according to any one of claims 1 to 3, Phase D: Betaine and dipotassium glycyrrhizinate, Phase E: Butylene glycol and hyaluronic acid, Phase F: preservative; The components of the emulsion include: Phase A: emulsifier A165, 16 / 18 alcohol, squalane, emollient oil and VE acetate, Phase B: water, glycerin, thickener and EDTA-2Na, Phase C: the composition for promoting the formation of liquid crystal structure of cosmetics according to any one of claims 1 to 3, Phase D: Betaine, Hydroxyethyl Urea, Humectants and Preservatives, Phase E: Arginine.
7. The use according to claim 6, characterized in that: The preparation method of the cosmetic comprises the steps of: heating phase A and phase B to 70-80° C. respectively, homogenizing at 11000 rpm-15000 rpm for 1-3 min after mixing, stirring and cooling to 45-55° C., adding components of other phases in sequence, and mixing evenly to obtain the cosmetic.
8. A cosmetic having a high amount of liquid crystal structures, high liquid crystal structure stability, high moisturizing properties and comfortable skin feel, characterized in that: The components include the composition for promoting the formation of liquid crystal structure in cosmetics according to any one of claims 1 to 3.
Citation Information
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