Water-soluble squalane nanoemulsion composition as well as preparation method and application thereof

Abstract

The invention belongs to the technical field of cosmetics, and particularly relates to a water-soluble squalane nanoemulsion composition as well as a preparation method and application thereof. The water-soluble squalane nano-emulsion composition provided by the invention is prepared from the following components in percentage by mass: 5 to 60 weight percent of squalane, 4 to 20 weight percent of an emulsifying agent, 2 to 8 weight percent of a preservative, 10 to 60 weight percent of water, 10 to 40 weight percent of a penetration enhancer and 0.1 to 0.5 weight percent of a stabilizing agent, the emulsifier comprises at least three of sodium stearoyl glutamate, polyglycerol-10 myristate, hydrogenated lecithin and caprylic / capric triglyceride. According to the water-soluble squalane nano-emulsion composition, the system stability is greatly improved, the particle size can be basically kept unchanged at 4 DEG C, 25 DEG C and 50 DEG C, the phenomena of layering, demulsification and the like are avoided, and the loss of the squalane content in the water-soluble squalane nano-emulsion composition is small.

Description

Technical Field

[0001] The invention belongs to the technical field of cosmetics, and in particular relates to a water-soluble squalane nanoemulsion composition and a preparation method and application thereof. Background Art

[0002] Squalane is one of the main components of lipids on the skin surface. It is a transparent and non-irritating oil that can penetrate into human skin and increase the transport and absorption of other active substances by increasing compound diffusion and improving interaction with the skin. Squalane also has certain antioxidant properties. Studies have found that squalane can increase the retention time of polyphenols in the body, thereby enhancing the body's antioxidant level. However, squalane is an oil-soluble substance, and its insoluble nature in water greatly limits its application in cosmetics.

[0003] Nanoemulsion is a thermodynamically stable, isotropic, transparent or translucent homogeneous dispersion system with nanometer-scale particle size formed by water, oil, surfactants, etc. The excellent particle size range of nanoemulsion can penetrate the gaps on the surface of the skin, greatly improving the skin's absorption rate of oil-soluble functional ingredients. At present, the water solubility of squalane can be improved by preparing it in the form of nanoemulsion, increasing the absorption rate of the skin, thereby realizing its application in cosmetics. However, the existing squalane nanoemulsion kinetic system is unstable and has poor stability during storage. It will undergo changes such as flocculation and aggregation, which will eventually lead to the stratification of the oil and water phases in the entire system, and the loss of squalane components is large, causing irreversible damage to the product. Summary of the invention

[0004] Therefore, the technical problem to be solved by the present invention is to overcome the defects of the existing squalane nanoemulsion, such as poor stability during storage, easy oil-water phase separation in the whole system, and large loss of squalane components, thereby providing a water-soluble squalane nanoemulsion composition, a preparation method and application thereof.

[0005] The present invention provides a water-soluble squalane nanoemulsion composition. The components of the water-soluble squalane nanoemulsion composition, by mass percentage, include 5wt%-60wt% of squalane, 4wt%-20wt% of an emulsifier, 2wt%-8wt% of a preservative, 10wt%-60wt% of water, 10wt%-40wt% of a penetration enhancer, and 0.1wt%-0.5wt% of a stabilizer;

[0006] The emulsifier includes at least three of sodium stearoyl glutamate, polyglyceryl-10 myristate, hydrogenated lecithin and caprylic / capric triglyceride.

[0007] Optionally, the water includes but is not limited to at least one of ultrapure water and deionized water.

[0008] Preferably, the emulsifier is sodium stearoyl glutamate, polyglyceryl-10 myristate, hydrogenated lecithin and caprylic / capric triglyceride.

[0009] Preferably, the mass ratio of sodium stearoyl glutamate, polyglyceryl-10 myristate, hydrogenated lecithin and caprylic / capric triglyceride is (1-6):(0.5-1.5):(1-6):(1-6).

[0010] Optionally, the mass ratio of polyglycerol-10 myristate, hydrogenated lecithin and caprylic / capric triglyceride is (0.5-1.5):(1-6):(1-6).

[0011] Optionally, the mass ratio of sodium stearoyl glutamate, hydrogenated lecithin and caprylic / capric triglyceride is (1-6): (1-6): (1-6).

[0012] Optionally, the mass ratio of sodium stearoyl glutamate, polyglyceryl-10 myristate and caprylic / capric triglyceride is (1-6): (0.5-1.5): (1-6).

[0013] Optionally, the mass ratio of sodium stearoyl glutamate, polyglycerol-10 myristate and hydrogenated lecithin is (1-6): (0.5-1.5): (1-6).

[0014] Preferably, the preservative is selected from at least one of ethylhexylglycerin, 1,2-hexanediol, 1,3-butylene glycol, and phenoxyethanol;

[0015] The penetration enhancer is selected from glycerol;

[0016] The stabilizer is selected from PEG-10 soybean sterol.

[0017] Preferably, the preservatives are 1,2-hexanediol and 1,3-butanediol;

[0018] The mass ratio of the 1,2-hexanediol to the 1,3-butanediol is (1-4):(1-3).

[0019] Preferably, the mass ratio of water to penetration enhancer is (1-6):(2-3).

[0020] Optionally, the average particle size of the squalane emulsified particles in the water-soluble squalane nanoemulsion composition is 80-160 nm;

[0021] Optionally, after the water-soluble squalane nanoemulsion composition is stored at 50° C. for 3 months, the average particle size of the squalane emulsified particles in the water-soluble squalane nanoemulsion composition is 110-310 nm.

[0022] The present invention provides a method for preparing the water-soluble squalane nanoemulsion composition, comprising the following steps:

[0023] 1) an emulsifier, a preservative, a stabilizer and a penetration enhancer are mixed by a first stirring process, and then squalane is added and mixed by a second stirring process to obtain a mixed solution A;

[0024] 2) Mixing the mixed solution A and water by a third stirring step, and then homogenizing to obtain the water-soluble squalane nanoemulsion composition.

[0025] Preferably, in step 1), the first stirring temperature is 70-72° C., and the first stirring speed is 100-200 rpm;

[0026] In step 1), the second stirring temperature is 70-72° C., the second stirring speed is 100-200 rpm, and the second stirring time is 10-15 min.

[0027] Preferably, in step 2), the third stirring speed is 100-200 rpm, and the third stirring time is 15-25 min;

[0028] In step 2), the homogenization pressure is 60-100 bar, the homogenization flow rate is 28-32 L / h, and the homogenization times are not less than 3 times;

[0029] Preferably, the homogenization times are 3-6 times.

[0030] The present invention also provides an application of the water-soluble squalane nanoemulsion composition described above or the water-soluble squalane nanoemulsion composition prepared by the preparation method described above in cosmetics.

[0031] The technical solution of the present invention has the following advantages:

[0032] The water-soluble squalane nanoemulsion composition provided by the present invention comprises, by mass percentage, 5wt%-60wt% of squalane, 4wt%-20wt% of emulsifier, 2wt%-8wt% of preservative, 10wt%-60wt% of water, 10wt%-40wt% of penetration enhancer, and 0.1wt%-0.5wt% of stabilizer; the emulsifier comprises at least 3 of sodium stearoyl glutamate, polyglycerol-10 myristate, hydrogenated lecithin, and caprylic / capric triglyceride. The present invention selects a specific emulsifier for synergistic coordination, and the interaction with stabilizers, penetration enhancers, water-embedded substances, etc. can change the spatial arrangement of each substance, so that the nanoemulsion and the squalane in the nanoemulsion reach a relatively "most stable" state, thereby avoiding nanoemulsion stratification, demulsification, etc. for a long time. The water-soluble squalane nanoemulsion composition of the present invention greatly improves the stability of the system, can keep the particle size basically unchanged under the conditions of low temperature of 4°C, normal temperature of 25°C and high temperature of 50°C, without stratification, demulsification and the like, and the loss of squalane content in the water-soluble squalane nanoemulsion composition is small, which advantageously ensures the stability of product quality, thereby increasing the application scope of squalane in cosmetics.

[0033] The water-soluble squalane nanoemulsion composition provided by the present invention comprises sodium stearoyl glutamate, polyglycerol-10 myristate, hydrogenated lecithin and caprylic / capric triglyceride. The present invention selects specific emulsifiers for synergistic coordination. Sodium stearoyl glutamate and hydrogenated lecithin have relatively long hydrophobic chains, which are interspersed in the structure of caprylic / capric triglyceride and cooperate with the hydrophobic groups of polyglycerol-10-myristate. Squalane is interspersed between the hydrophobic chains and remains stable by the interaction therebetween. Polyglycerol-10-myristate also has relatively large hydrophilic groups, which interact with water molecules to maintain uniform distribution of the overall structure in water. The water-soluble squalane nanoemulsion composition obtained by the present invention has better stability by specifically selecting sodium stearoyl glutamate, polyglycerol-10 myristate, hydrogenated lecithin and caprylic / capric triglyceride as emulsifiers to cooperate with squalane. In particular, under high temperature conditions, the squalane content stability and particle size stability in the water-soluble squalane nanoemulsion composition are better.

[0034] The water-soluble squalane nanoemulsion composition of the invention has a high squalane content, and the particle size of the squalane-containing particles in the water-soluble squalane nanoemulsion composition is small. BRIEF DESCRIPTION OF THE DRAWINGS

[0035] In order to more clearly illustrate the specific implementation methods of the present invention or the technical solutions in the prior art, the drawings required for use in the specific implementation methods or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are some implementation methods of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative work.

[0036] Figure 1 Particle size distribution diagram of the water-soluble squalane nanoemulsion composition prepared in Example 2 of the present invention;

[0037] Figure 2 Particle size distribution diagram of the water-soluble squalane nanoemulsion composition prepared in Example 3 of the present invention;

[0038] Figure 3 The average particle size change diagram of the water-soluble squalane nanoemulsion composition prepared in Examples 1, 2 and 3 of the present invention after storage at 50° C. for 3 months;

[0039] Figure 4 The squalane content of the water-soluble squalane nanoemulsion composition prepared in Examples 2 and 3 of the present invention and Comparative Example 1 is stored at 50° C. for 3 months and changes over time;

[0040] Figure 5 The squalane content of the water-soluble squalane nanoemulsion composition prepared in Example 3 of the present invention is stored at 4° C., 25° C., and 50° C. for 3 months over time;

[0041] Figure 6 Photos of the water-soluble squalane nanoemulsion composition prepared in Example 3 of the present invention diluted 0 times (left), 10 times (middle), and 100 times (right). DETAILED DESCRIPTION

[0042] The following examples are provided for a better understanding of the present invention, but are not intended to limit the best mode of implementation, nor to limit the content and protection scope of the present invention. Any product identical or similar to the present invention obtained by anyone under the inspiration of the present invention or by combining the features of the present invention with other prior arts shall fall within the protection scope of the present invention.

[0043] If no specific experimental steps or conditions are specified in the examples, the conventional experimental steps or conditions described in the literature in the field can be used. If no manufacturer is specified for the reagents or instruments used, they are all conventional reagent products that can be obtained commercially.

[0044] Example 1-Example 7

[0045] Examples 1 to 7 respectively provide a water-soluble squalane nanoemulsion composition, the components and component contents of which are shown in Table 1;

[0046] Table 1

[0047]

[0048] The preparation method of the water-soluble squalane nanoemulsion composition provided in Examples 1 to 7 comprises the following steps:

[0049] 1) Add emulsifier, preservative, stabilizer and penetration enhancer into an emulsifying pot, raise the temperature to 70° C. at a stirring speed of 150 rpm, maintain the stirring speed and continue stirring until the materials are melted, add squalane and continue stirring at 70° C. and 150 rpm for 13 min to obtain a mixed solution A;

[0050] 2) The mixed solution A was slowly added into the water at a uniform speed and continued to be stirred at a stirring speed of 150 rpm for 20 min; and then homogenized 4 times in a high-pressure homogenizer at a homogenization pressure of 80 bar and a homogenization flow rate of 30 L / h to obtain the water-soluble squalane nanoemulsion composition.

[0051] Example 8

[0052] This embodiment provides a water-soluble squalane nanoemulsion composition, the components and component contents of which are shown in Table 2;

[0053] Table 2

[0054] Example 8 Squalane / g 5 Hydrogenated lecithin / g 2 Caprylic / capric triglyceride / g 2 PEG-10 soybean sterol / g 0.5 Sodium stearoyl glutamate / g 2 Polyglyceryl-10 myristate / g 0.5 1,3-Butanediol / g 3 1,2-Hexanediol / g 4 Glycerol / g 25.5 Deionized water / g 55.5

[0055] The preparation method of the water-soluble squalane nanoemulsion composition provided in this embodiment comprises the following steps:

[0056] 1) Add emulsifier, preservative, stabilizer and penetration enhancer into an emulsifying pot, raise the temperature to 71° C. at a stirring speed of 200 rpm, maintain the stirring speed and continue stirring until the materials are melted, add squalane and continue stirring at 71° C. and 200 rpm for 10 min to obtain a mixed solution A;

[0057] 2) The mixed solution A was slowly added into the water at a uniform speed and continued to be stirred at a stirring speed of 100 rpm for 25 min; and then homogenized 6 times in a high-pressure homogenizer at a homogenization pressure of 60 bar and a homogenization flow rate of 30 L / h to obtain the water-soluble squalane nanoemulsion composition.

[0058] Example 9

[0059] This embodiment provides a water-soluble squalane nanoemulsion composition, the components and component contents of which are shown in Table 3;

[0060] Table 3

[0061] Example 9 Squalane / g 50 Hydrogenated lecithin / g 3 Caprylic / capric triglyceride / g 6 PEG-10 soybean sterol / g 0.3 Sodium stearoyl glutamate / g 6 Polyglyceryl-10 myristate / g 1.5 1,3-Butanediol / g 1 1,2-Hexanediol / g 1 Glycerol / g 10 Deionized water / g 21.2

[0062] The preparation method of the water-soluble squalane nanoemulsion composition provided in this embodiment comprises the following steps:

[0063] 1) Add emulsifier, preservative, stabilizer and penetration enhancer into an emulsifying pot, raise the temperature to 72° C. at a stirring speed of 100 rpm, maintain the stirring speed and continue stirring until the materials are melted, add squalane and continue stirring at 72° C. and 100 rpm for 15 minutes to obtain a mixed solution A;

[0064] 2) The mixed solution A was slowly added into the water at a uniform speed and continued to be stirred at a stirring speed of 200 rpm for 15 min; and then homogenized 4 times in a high-pressure homogenizer at a homogenization pressure of 100 bar and a homogenization flow rate of 30 L / h to obtain the water-soluble squalane nanoemulsion composition.

[0065] Comparative Example 1-Comparative Example 5

[0066] Comparative Examples 1 to 5 respectively provide a water-soluble squalane nanoemulsion composition, and its components and component contents are shown in Table 4;

[0067] The preparation methods of the water-soluble squalane nanoemulsion compositions provided in Comparative Examples 1 to 5 are the same as that in Example 3.

[0068] Table 4

[0069] Comparative Example 1 Comparative Example 2 Comparative Example 3 Comparative Example 4 Comparative Example 5 Squalane / g 20 20 20 20 20 Hydrogenated lecithin / g 2 5.5 - - - Caprylic / capric triglyceride / g 2 - 5.5 - - PEG-10 soybean sterol / g 0.1 0.1 0.1 0.1 0.1 Sodium stearoyl glutamate / g - - - 5.5 - Polyglyceryl-10 myristate / g - - - - 5.5 1,3-Butanediol / g 1.4 1.4 1.4 1.4 1.4 1,2-Hexanediol / g 1.4 1.4 1.4 1.4 1.4 Glycerol / g 25.5 25.5 25.5 25.5 25.5 Deionized water / g 47.6 46.1 46.1 46.1 46.1

[0070] Test Case

[0071] The water-soluble squalane nanoemulsion compositions prepared in Examples 1-9 and Comparative Examples 1-5 were tested for the average particle size of the squalane emulsified particles in the water-soluble squalane nanoemulsion compositions using a particle size analyzer. The average particle size test results are shown in Table 5, wherein the particle size distribution diagram of Example 2 is shown in 1 (the abscissa is the particle size, unit nm; the ordinate is the differential distribution volume, unit %), and the particle size distribution diagram of Example 3 is shown in 2 (the abscissa is the particle size, unit nm; the ordinate is the differential distribution volume, unit %).

[0072] The water-soluble squalane nanoemulsion compositions prepared in Examples 1-9 and Comparative Examples 1-5 were stored at 50°C for 3 months, and the average particle size of the squalane emulsified particles in the water-soluble squalane nanoemulsion compositions was tested. The test results are shown in Table 5, and the difference in average particle size before and after storage at 50°C for 3 months is shown in Table 5. The average particle size of the water-soluble squalane nanoemulsion compositions prepared in Examples 1, 2, and 3 was tested for changes in average particle size over time during storage at 50°C for 3 months. The results are shown in Table 5. Figure 3 shown.

[0073] The water-soluble squalane nanoemulsion compositions prepared in Examples 1-9 and Comparative Examples 1-5 were stored at 50° C. for 3 months, and the mass content of squalane was tested. The detection method adopted gas chromatography, and the chromatographic test conditions were: HP-5 capillary column, column length 30 m, inner diameter 0.32 mm, film thickness 0.25 μm; carrier gas was high-purity nitrogen with a purity of 99.99%; constant pressure 110.32 kPa (16 psi); split ratio was 1:5; injection port temperature was 290° C.; the column temperature was programmed to increase from 160° C. to 220° C. at a rate of 15 K / min, maintained for 2 min, then increased to 280° C. at a rate of 5 K / min, maintained for 2 min, and finally increased to 310° C. at a rate of 30 K / min and maintained for 3 min. FID detector: temperature is 300°C, hydrogen flow rate is 40mL / min, air flow rate is 450mL / min, and tail gas flow rate is 25mL / min. The injection volume is 1.0μL. The test results of squalane mass content are shown in Table 5, and the results of squalane content loss rate after storage at 50°C for 3 months are shown in Table 5. The water-soluble squalane nanoemulsion compositions prepared in Examples 2, 3 and Comparative Example 1 were tested for squalane content that changed over time during storage at 50°C for 3 months. The results are shown in Table 5. Figure 4 shown.

[0074] The water-soluble squalane nanoemulsion composition prepared in Example 2 was stored at 4°C, 25°C, and 50°C for 3 months, and the squalane content that changed with time during the storage process was measured. The test method used gas chromatography, and the specific conditions were the same as above. The test results are as follows: Figure 5 The stability of the water-soluble squalane nanoemulsion composition is greatly affected by temperature. The higher the temperature, the worse the stability. Figure 5 The water-soluble squalane nanoemulsion composition was stored at 4°C, 25°C and 50°C for 3 months, and the change range of the squalane content remained basically the same. It can be seen that the specific water-soluble squalane nanoemulsion composition provided by the present invention has basically the same stability under the low temperature of 4°C, the normal temperature of 25°C and the high temperature of 50°C, that is, the stability under the low temperature of 4°C, the normal temperature of 25°C and the high temperature of 50°C is high.

[0075] The water-soluble squalane nanoemulsion composition obtained in Example 3 was diluted 0 times, 10 times, and 100 times, respectively, and then bottled. Figure 6 As shown, the water-soluble squalane nanoemulsion composition is milky white, the solution is uniform, and has a faint blue light.

[0076] Table 5

[0077]

[0078] Note: “-” indicates that the emulsion was separated and the particle size and content were not measured.

[0079] The water-soluble squalane nanoemulsion compositions obtained in Comparative Examples 2, 4 and 5 in Table 5 have been stratified after being stored at 50° C. for 3 months and cannot stably exist in the form of emulsions, that is, their stability is significantly poor.

[0080] Obviously, the above embodiments are merely examples for the purpose of clear explanation, and are not intended to limit the implementation methods. For those skilled in the art, other different forms of changes or modifications can be made based on the above description. It is not necessary and impossible to list all the implementation methods here. The obvious changes or modifications derived therefrom are still within the scope of protection of the invention.

Claims

1. A water-soluble squalane nanoemulsion composition, characterized in that: The components of the water-soluble squalane nanoemulsion composition include, by mass percentage, 5wt%-60wt% of squalane, 4wt%-20wt% of an emulsifier, 2wt%-8wt% of a preservative, 10wt%-60wt% of water, 10wt%-40wt% of a penetration enhancer, and 0.1wt%-0.5wt% of a stabilizer; The emulsifier includes at least three of sodium stearoyl glutamate, polyglyceryl-10 myristate, hydrogenated lecithin and caprylic / capric triglyceride.

2. The water-soluble squalane nanoemulsion composition according to claim 1, characterized in that: The emulsifiers are sodium stearoyl glutamate, polyglyceryl-10 myristate, hydrogenated lecithin and caprylic / capric triglyceride.

3. The water-soluble squalane nanoemulsion composition according to claim 2, characterized in that: The mass ratio of sodium stearoyl glutamate, polyglyceryl-10 myristate, hydrogenated lecithin and caprylic / capric triglyceride is (1-6):(0.5-1.5):(1-6):(1-6).

4. The water-soluble squalane nanoemulsion composition according to any one of claims 1 to 3, characterized in that: The preservative is selected from at least one of ethylhexylglycerin, 1,2-hexanediol, 1,3-butylene glycol, and phenoxyethanol; The penetration enhancer is selected from glycerol; The stabilizer is selected from PEG-10 soybean sterol.

5. The water-soluble squalane nanoemulsion composition according to any one of claims 1 to 4, characterized in that: The preservatives are 1,2-hexanediol and 1,3-butanediol; The mass ratio of the 1,2-hexanediol to the 1,3-butanediol is (1-4):(1-3).

6. The water-soluble squalane nanoemulsion composition according to any one of claims 1 to 4, characterized in that: The mass ratio of water to penetration enhancer is (1-6):(2-3).

7. A method for preparing the water-soluble squalane nanoemulsion composition according to any one of claims 1 to 6, characterized in that: The steps include: 1) an emulsifier, a preservative, a stabilizer and a penetration enhancer are mixed by a first stirring process, and then squalane is added and mixed by a second stirring process to obtain a mixed solution A; 2) Mixing the mixed solution A and water by a third stirring step, and then homogenizing to obtain the water-soluble squalane nanoemulsion composition.

8. The method for preparing the water-soluble squalane nanoemulsion composition according to claim 7, characterized in that: In step 1), the first stirring temperature is 70-72° C., and the first stirring speed is 100-200 rpm; In step 1), the second stirring temperature is 70-72° C., the second stirring speed is 100-200 rpm, and the second stirring time is 10-15 min.

9. The method for preparing the water-soluble squalane nanoemulsion composition according to claim 7 or 8, characterized in that: In step 2), the third stirring speed is 100-200 rpm, and the third stirring time is 15-25 min; In step 2), the homogenization pressure is 60-100 bar, the homogenization flow rate is 28-32 L / h, and the homogenization times are not less than 3 times; Preferably, the homogenization times are 3-6 times.

10. Use of the water-soluble squalane nanoemulsion composition according to any one of claims 1 to 6 or the water-soluble squalane nanoemulsion composition prepared by the preparation method according to any one of claims 7 to 9 in cosmetics.

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