Water-soluble retinol nanoemulsion 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 retinol nanoemulsion as well as a preparation method and application thereof. The water-soluble retinol nanoemulsion provided by the invention is prepared from the following components in percentage by mass: 3 to 10 weight percent of retinol, 10 to 15.3 weight percent of an emulsifier composition, 2 to 4 weight percent of an antioxidant, 10 to 30 weight percent of glycerol and the balance of water, the emulsifier composition is prepared from poloxamer, tween-20, caprylic / capric triglyceride and N, N, N-trimethyl glucose-1-ammonium chloride. The water-soluble retinol nanoemulsion with specific components and proportions has the advantages of small loss of retinol and strong stability when stored at normal temperature.

Description

Technical Field

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

[0002] Retinol is a form of vitamin A. Retinol not only promotes collagen formation, but also has great advantages in improving skin photoaging, fine lines, wrinkles and pigmentation. Therefore, it is widely used in cosmetics. However, the poor solubility of retinol, unstable chemical properties, and sensitivity to light, oxygen and high temperature limit the application of retinol. Existing retinol emulsions have a large loss of retinol and low stability when stored at room temperature, which has certain limitations in exploring more applications of retinol. Summary of the invention

[0003] Therefore, the technical problem to be solved by the present invention is to overcome the defects of existing retinol emulsions such as large retinol loss and low stability when stored at room temperature, thereby providing a water-soluble retinol nanoemulsion and a preparation method and application thereof.

[0004] The present invention provides a water-soluble retinol nanoemulsion, wherein the components of the water-soluble retinol nanoemulsion, by mass percentage, include 3wt%-10wt% retinol, 10wt%-15.3wt% emulsifier composition, 2wt%-4wt% antioxidant, 10wt%-30wt% glycerol, and the balance is water;

[0005] The emulsifier composition includes poloxamer, Tween-20, caprylic / capric triglyceride and N,N,N-trimethylglucose-1-ammonium chloride.

[0006] Preferably, the mass content of N,N,N-trimethylglucose-1-ammonium chloride in the water-soluble retinol nanoemulsion is not more than 0.5%;

[0007] Preferably, the mass ratio of poloxamer, Tween-20, caprylic / capric triglyceride and N,N,N-trimethylglucose-1-ammonium chloride is (2-6):(2-6):(1-4):(0.1-0.5).

[0008] Preferably, the mass ratio of poloxamer, Tween-20, caprylic / capric triglyceride and N,N,N-trimethylglucose-1-ammonium chloride is 2:2:1:0.1.

[0009] Preferably, the antioxidant is selected from at least two of α-tocopherol, rosemary oil, and butylated hydroxyanisole;

[0010] Preferably, the antioxidant is selected from α-tocopherol and rosemary oil;

[0011] The mass ratio of α-tocopherol to rosemary oil is (1-2): (1-2).

[0012] Preferably, the average particle size of the water-soluble retinol nanoemulsion is 20-200 nm.

[0013] Preferably, the average particle size of the water-soluble retinol nanoemulsion is 25-130 nm.

[0014] Optionally, the average particle size of the water-soluble retinol nanoemulsion after storage at 25° C. for 3 months is 80-303 nm.

[0015] The average particle size of the water-soluble retinol nanoemulsion mentioned in the present invention refers to the average particle size of the retinol emulsified particles contained in the water-soluble retinol nanoemulsion.

[0016] Preferably, the mass ratio of water to glycerol is (1-7):(1-3).

[0017] The present invention provides a method for preparing the above-mentioned water-soluble retinol nanoemulsion, comprising the following steps:

[0018] 1) The emulsifier composition is subjected to a first stirring and mixing process, and then an antioxidant and retinol are added thereto and subjected to a second stirring and mixing process to obtain a mixed solution A;

[0019] 2) mixing water and glycerol by a third stirring step to obtain a mixed solution B;

[0020] 3) The mixed solution A obtained in step 1) and the mixed solution B obtained in step 2) are mixed and homogenized by a fourth stirring step to obtain the water-soluble retinol nanoemulsion.

[0021] Preferably, in step 1), the first stirring speed is 100-200 rpm;

[0022] In step 1), the second stirring speed is 100-200 rpm, and the second stirring time is 30-50 min;

[0023] In step 2), the third stirring speed is 100-200 rpm, and the third stirring time is 15-25 min.

[0024] Preferably, in step 3), the fourth stirring speed is 100-200 rpm, and the fourth stirring time is 15-25 min;

[0025] In step 3), the homogenization pressure is 60-100 bar, the homogenization flow rate is 28-32 L / h, and the homogenization times are not less than 6 times;

[0026] Preferably, the homogenization times are 6-8 times.

[0027] The present invention also provides a use of the water-soluble retinol nanoemulsion described above or the water-soluble retinol nanoemulsion prepared by the preparation method described above in cosmetics.

[0028] The technical solution of the present invention has the following advantages:

[0029] The water-soluble retinol nanoemulsion provided by the present invention comprises, by mass percentage, 3wt%-10wt% retinol, 10wt%-15.3wt% emulsifier composition, 2wt%-4wt% antioxidant, 10wt%-30wt% glycerol, and the balance is water; the emulsifier composition comprises poloxamer, Tween-20, caprylic / capric triglyceride and N,N,N-trimethylglucose-1-ammonium chloride. Poloxamer and Tween 20 have a long hydrophobic chain at one end and a hydrophilic group at the other end, caprylic / capric triglyceride interacts with the hydrophilic groups of poloxamer and Tween 20, and N,N,N-trimethylglucose-1-ammonium chloride interacts with the hydrophobic long chain ends of poloxamer and Tween 20, and acts on the surface of retinol together, thereby forming a stable structure, achieving effective embedding of retinol, and achieving strong particle size stability and retinol content stability in the retinol emulsion. The water-soluble retinol nanoemulsion with specific components and proportions of the present invention has a small retinol loss amount and strong stability when stored at room temperature.

[0030] The water-soluble retinol nanoemulsion provided by the present invention comprises poloxamer, Tween-20, caprylic / capric triglyceride and N,N,N-trimethylglucose-1-ammonium chloride in a mass ratio of (2-5):(2-5):(1-1.5):(0.1-0.5). The structure of the nanoemulsion is more stable, the embedding effect of retinol is better, the retinol loss in the obtained retinol emulsion is smaller, and the stability is stronger.

[0031] The water-soluble retinol nanoemulsion provided by the present invention has a small particle size and a high retinol content. BRIEF DESCRIPTION OF THE DRAWINGS

[0032] 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.

[0033] Figure 1 Particle size distribution diagram of the water-soluble retinol nanoemulsion of Example 1;

[0034] Figure 2 Particle size distribution diagram of the water-soluble retinol nanoemulsion of Example 2;

[0035] Figure 3 A line graph showing the change in average particle size of the water-soluble retinol nanoemulsion prepared in Comparative Example 1-2 of Example 1-2 during storage at 25° C. for 3 months;

[0036] Figure 4 A line graph showing the change in retinol content in the water-soluble retinol nanoemulsion prepared in Example 1-2 during storage at 25° C. for one month. DETAILED DESCRIPTION

[0037] 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.

[0038] 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.

[0039] Example 1-Example 2

[0040] This embodiment provides a water-soluble retinol nanoemulsion, the components and component contents of which are shown in Table 1;

[0041] Table 1

[0042] Example 1 Example 2 Poloxamer / g 6 6 Tween-20 / g 6 6 Caprylic / capric triglyceride / g 3 3 α-Tocopherol / g 2 1 Rosemary oil / g 2 2 Retinol / g 5 5 Glycerol / g 25 28 N,N,N-Trimethylglucose-1-ammonium chloride / g 0.1 0.3 Water / g 50.9 48.7

[0043] The method for preparing the water-soluble retinol nanoemulsion provided in this embodiment comprises the following steps:

[0044] 1) adding an emulsifier into an emulsifying pot, stirring at a stirring speed of 100 rpm until the materials are uniformly mixed, then adding an antioxidant and retinol, and continuing to stir at a stirring speed of 100 rpm for 50 minutes to obtain a mixed solution A;

[0045] 2) Add water and glycerin into another emulsifying pot and stir at a stirring speed of 100 rpm for 10 min to obtain a mixed solution B;

[0046] 3) The mixed solution A was slowly added to the mixed solution B at a uniform speed and continued to be stirred at a stirring speed of 150 rpm for 20 min; and then homogenized 6 times in a high-pressure homogenizer at a homogenizing pressure of 80 bar and a homogenizing flow rate of 30 L / h to obtain the water-soluble retinol nanoemulsion.

[0047] Example 3

[0048] This embodiment provides a water-soluble retinol nanoemulsion, the components and component contents of which are shown in Table 2;

[0049] Table 2

[0050] Example 3 Poloxamer / g 4 Tween-20 / g 6 Caprylic / capric triglyceride / g 4 α-Tocopherol / g 2 Rosemary oil / g 2 Retinol / g 3 Glycerol / g 30 N,N,N-Trimethylglucose-1-ammonium chloride / g 0.2 Water / g 48.8

[0051] This embodiment provides a method for preparing a water-soluble retinol nanoemulsion, comprising the following steps:

[0052] 1) adding an emulsifier into an emulsifying pot, stirring at a stirring speed of 200 rpm until the materials are uniformly mixed, then adding an antioxidant and retinol, and continuing to stir at a stirring speed of 200 rpm for 30 minutes to obtain a mixed solution A;

[0053] 2) Add water and glycerin into another emulsifying pot and stir at a stirring speed of 200 rpm for 5 min to obtain a mixed solution B;

[0054] 3) The mixed solution A was slowly added to the mixed solution B at a uniform speed and continued to be stirred at a stirring speed of 150 rpm for 20 min; and then homogenized 6 times in a high-pressure homogenizer at a homogenizing pressure of 80 bar and a homogenizing flow rate of 30 L / h to obtain the water-soluble retinol nanoemulsion.

[0055] Example 4

[0056] This embodiment provides a water-soluble retinol nanoemulsion, the components and component contents of which are shown in Table 3;

[0057] Table 3

[0058]

[0059]

[0060] This embodiment provides a method for preparing a water-soluble retinol nanoemulsion, comprising the following steps:

[0061] 1) adding an emulsifier into an emulsifying pot, stirring at a stirring speed of 150 rpm until the materials are uniformly mixed, then adding an antioxidant and retinol, and continuing to stir at a stirring speed of 150 rpm for 40 minutes to obtain a mixed solution A;

[0062] 2) Add water and glycerin into another emulsifying pot and stir at a stirring speed of 150 rpm for 8 min to obtain a mixed solution B;

[0063] 3) The mixed solution A was slowly added to the mixed solution B at a uniform speed and continued to be stirred at a stirring speed of 200 rpm for 15 minutes; then, the mixture was homogenized 8 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 retinol nanoemulsion.

[0064] Comparative Examples 1-6

[0065] Comparative Examples 1-6 provide a water-soluble retinol nanoemulsion, the components and component contents of which are shown in Table 4;

[0066] The preparation methods of the water-soluble retinol nanoemulsions provided in Comparative Examples 1-6 are the same as those in Example 1.

[0067] Table 4

[0068]

[0069]

[0070] Test Case

[0071] The water-soluble retinol nanoemulsions prepared in Examples 1-4 and Comparative Examples 1-6 were tested for average particle size of the water-soluble retinol nanoemulsions using a particle size analyzer. The average particle size test results are shown in Table 5, wherein the particle size distribution diagram of the water-soluble retinol nanoemulsion of Example 1 is shown in 1 (the abscissa is particle size, unit nm; the ordinate is differential distribution volume, unit %), and the particle size distribution diagram of the water-soluble retinol nanoemulsion of Example 2 is shown in 2 (the abscissa is particle size, unit nm; the ordinate is differential distribution volume, unit %).

[0072] The water-soluble retinol nanoemulsions prepared in Examples 1-4 and Comparative Examples 1-6 were stored at 25°C for 3 months to test the average particle size of the water-soluble retinol nanoemulsions. The test results are shown in Table 5. The difference in average particle size before and after storage is shown in Table 5. The water-soluble retinol nanoemulsions prepared in Comparative Example 1-2 of Examples 1-2 were stored at 25°C for 3 months to test the average particle size of the water-soluble retinol nanoemulsions over time. The test results are shown in Table 5. Figure 3 shown.

[0073] The water-soluble retinol nanoemulsions prepared in Examples 1-4 and Comparative Examples 1-6 were stored at 25°C for 1 month, and the mass content of retinol in the water-soluble retinol nanoemulsions was determined by HPLC. The conditions for HPLC determination were as follows: chromatographic column: YSC-PACKODS-AQ 4.6*250mm 5μm, detection wavelength: 235nm, flow rate 1.0mL / min, mobile phase 0.1% phosphoric acid solution: methanol = 0:90, injection volume 5μL. The test results are shown in Table 5, and the amount of retinol loss before and after storage is shown in Table 5. During the storage of the water-soluble retinol nanoemulsions prepared in Examples 1-2 at 25°C for 1 month, the retinol content in the water-soluble retinol nanoemulsions was tested over time, and the test results are shown in Table 5. Figure 4 shown.

[0074] Table 5

[0075]

[0076] Note: “-” indicates that the emulsion was separated and the particle size and content were not measured.

[0077] The water-soluble retinol nanoemulsions of Comparative Examples 4 and 5 in Table 5 have stratified after being stored at 25° C. for 3 months and cannot stably exist in the form of emulsions, that is, their stability is significantly poor.

[0078] 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 retinol nanoemulsion, characterized in that: The components of the water-soluble retinol nanoemulsion include, by mass percentage, 3wt%-10wt% retinol, 10wt%-15.3wt% emulsifier composition, 2wt%-4wt% antioxidant, 10wt%-30wt% glycerol, and the balance is water; The emulsifier composition includes poloxamer, Tween-20, caprylic / capric triglyceride and N,N,N-trimethylglucose-1-ammonium chloride.

2. The water-soluble retinol nanoemulsion according to claim 1, characterized in that: The mass content of N,N,N-trimethylglucose-1-ammonium chloride in the water-soluble retinol nanoemulsion is not more than 0.5%; and / or, the mass ratio of the poloxamer, Tween-20, caprylic / capric triglyceride and N,N,N-trimethylglucose-1-ammonium chloride is (2-6):(2-6):(1-4):(0.1-0.5); Preferably, the mass ratio of poloxamer, Tween-20, caprylic / capric triglyceride and N,N,N-trimethylglucose-1-ammonium chloride is 2:2:1:0.

1.

3. The water-soluble retinol nanoemulsion according to claim 1 or 2, characterized in that: The antioxidant is selected from at least two of α-tocopherol, rosemary oil and butylated hydroxyanisole.

4. The water-soluble retinol nanoemulsion according to any one of claims 1 to 3, characterized in that: The antioxidant is selected from alpha-tocopherol and rosemary oil; The mass ratio of α-tocopherol to rosemary oil is (1-2): (1-2).

5. The water-soluble retinol nanoemulsion according to any one of claims 1 to 4, characterized in that: The average particle size of the water-soluble retinol nanoemulsion is 20-200 nm; Preferably, the average particle size of the water-soluble retinol nanoemulsion is 25-130 nm.

6. The water-soluble retinol nanoemulsion according to any one of claims 1 to 5, characterized in that: The mass ratio of water to glycerol is (1-7):(1-3).

7. A method for preparing the water-soluble retinol nanoemulsion according to any one of claims 1 to 6, characterized in that: The following steps are involved: 1) The emulsifier composition is mixed by a first stirring process, and then an antioxidant and retinol are added and mixed by a second stirring process to obtain a mixed solution A; 2) mixing water and glycerol by a third stirring step to obtain a mixed solution B; 3) The mixed solution A obtained in step 1) and the mixed solution B obtained in step 2) are mixed and homogenized by a fourth stirring step to obtain the water-soluble retinol nanoemulsion.

8. The method for preparing the water-soluble retinol nanoemulsion according to claim 7, characterized in that: In step 1), the first stirring speed is 100-200 rpm; In step 1), the second stirring speed is 100-200 rpm, and the second stirring time is 30-50 min; In step 2), the third stirring speed is 100-200 rpm, and the third stirring time is 15-25 min.

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

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

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