A kind of horse oil microemulsion gel and preparation method thereof

Abstract

The present invention relates to the technical field of cosmetics, and discloses a horse oil microemulsion gel and a preparation method thereof. The horse oil microemulsion gel comprises an oil phase, an aqueous phase, an emulsifier and an emulsifier co-phase, a gel matrix and a moisturizer. The present invention uses horse oil as a main raw material to prepare the horse oil microemulsion gel, effectively solving the problems of poor solubility, easy rancidity, instability, etc. of horse oil, and provides a new idea and approach for the development of horse oil products. In addition, the preparation process of the horse oil microemulsion gel is simple, the preparation cost is low, it has good moisturizing performance and antioxidant activity, and its market benefits are very considerable.

Description

Technical Field

[0001] The invention belongs to the technical field of cosmetics, and particularly relates to a horse oil microemulsion gel and a preparation method thereof. Background Art

[0002] Horse oil is made from horse fat through a series of processing techniques such as extraction and refining. Its essential fatty acid content is about 17.4%, and it is rich in nutrients such as VA and VE. It is a typical nutritional oil. Because of its antibacterial and anti-inflammatory, moisturizing, whitening and anti-aging effects, it is a good raw material for the development of cosmetics.

[0003] Horse oil is rich in unsaturated fatty acids, which makes it easy to oxidize and become rancid during production and transportation, affecting its deep processing and high-value utilization. In order to overcome this limitation, horse oil is combined with microencapsulation technology to improve its physical and antioxidant stability. Microemulsion, as a water-in-oil colloidal dispersion, is one of the common microencapsulation technologies. It is usually distributed in the system with a particle size of 20 to 500 nm and has good physical stability. However, as a liquid preparation, it has strong fluidity and low viscosity, which makes it inconvenient to apply to the skin, and it is easy to become turbid during storage. In order to improve the adhesion between the microemulsion and the skin and its storage stability, it can be combined with a gel matrix to prepare a microemulsion gel. Microemulsion gel is a nanostructured system obtained by adding a thickener to the water phase or oil phase of the microemulsion. It successfully combines the physicochemical properties of microemulsion and gel. The use of microemulsion gel preparations can not only enhance the stability of horse oil, but also improve its moisturizing effect and antioxidant activity. The preparation process of microemulsion gel is simple and the preparation cost is low, so its market benefits are very considerable, which will provide new ideas and approaches for the development of horse oil cosmetics. Summary of the invention

[0004] The purpose of the present invention is to improve the stability, moisture retention and antioxidant activity of horse oil by using an effective matrix, and to provide new ideas and methods for the subsequent development of horse oil products.

[0005] On one hand, the present invention provides a horse oil microemulsion gel and a preparation method thereof, which consists of two parts: preparation of horse oil microemulsion and preparation of horse oil microemulsion gel. The horse oil microemulsion gel is prepared from horse oil microemulsion, carbomer-980 and glycerol; the horse oil microemulsion is prepared from an oil phase, an emulsifier, an auxiliary emulsifier and water; the oil phase is horse oil and an oil phase solvent; and the horse oil microemulsion is an O / W type microemulsion.

[0006] The invention provides a horse oil microemulsion, which is prepared according to the following mass ratio: 1-5 parts of horse oil, 5-10 parts of oil phase solvent, 7-12 parts of emulsifier, 7-12 parts of auxiliary emulsifier and 120-160 parts of water.

[0007] Preferably, the horse oil microemulsion is prepared according to the following mass ratio: 4 parts of horse oil, 8 parts of oil phase solvent, 9 parts of emulsifier, 9 parts of co-emulsifier and 150 parts of water.

[0008] The percentage of carbomer-980 in the horse oil microemulsion is 0.5-1.0%, preferably 0.8%; the percentage of glycerol in the horse oil microemulsion is 2-8%, preferably 5%.

[0009] Preferably, the emulsifier is Cremophor RH-40; the co-emulsifier is PEG-40; and the oil phase solvent is IPM.

[0010] The present invention also provides a method for preparing the horse oil microemulsion gel described in the above technical solution, comprising the following steps:

[0011] (1) mixing the horse oil, the oil phase solvent, the emulsifier, and the co-emulsifier to obtain a mixture;

[0012] (2) mixing and emulsifying the obtained mixture with water to obtain a horse oil microemulsion;

[0013] (3) mixing the horse oil microemulsion, carbomer-980 and glycerol to obtain a mixture and letting it stand for 24 hours;

[0014] (4) Add 20% triethanolamine solution to the mixture to adjust the pH to 5-6 to obtain horse oil microemulsion gel.

[0015] In the above method, the emulsification temperature is 28-32° C.; the emulsification speed is 650-750 r / min.

[0016] The present invention also provides a horse oil microemulsion gel, comprising the horse oil microemulsion described in the above technical solution, carbomer-980 and glycerol, and is prepared according to the following mass ratio: the mass percentage of carbomer-980 in the horse oil microemulsion is 0.5-1.0%, and the mass percentage of glycerol in the horse oil microemulsion is 2-8%.

[0017] Preferably, the percentage of carbomer-980 in the horse oil microemulsion is 0.8%, and the percentage of glycerol in the horse oil microemulsion is 5%.

[0018] The present invention also provides a method for preparing the horse oil microemulsion gel described in the above technical solution, comprising the following steps:

[0019] (1) mixing the horse oil microemulsion, carbomer-980 and glycerol to obtain a mixture and letting it stand for 24 hours;

[0020] (2) Add 20% triethanolamine solution to the mixture to adjust the pH to 5-6.

[0021] The present invention also provides the effect of the horse oil microemulsion described in the above technical solution on improving the stability, moisture retention and antioxidant activity of horse oil.

[0022] Compared with the prior art, the present invention has the following beneficial effects:

[0023] Due to its high content of unsaturated fatty acids, horse oil is easily rancid and oxidized during production and transportation. It is necessary to use an effective matrix to improve the stability and effectiveness of horse oil. Microemulsion gel has the advantages of both microemulsion and gel dosage forms. By combining horse oil with microemulsion gel preparations, its stability, moisturizing properties and antioxidant properties can be enhanced, providing new ideas and methods for the subsequent development of horse oil products. BRIEF DESCRIPTION OF THE DRAWINGS

[0024] Figure 1 Transmission electron microscopy images of horse oil microemulsion (scale bars are 100 and 20 nm, respectively);

[0025] Figure 2.1 Particle size distribution of horse oil microemulsion;

[0026] Figure 2.2 Zeta potential distribution of horse oil microemulsion;

[0027] Figure 3 Results of Sudan red III and methylene blue staining of horse oil microemulsion;

[0028] Figure 4 Horse oil microemulsion gel;

[0029] Figure 5 Evaluation of the moisturizing properties of horse oil microemulsion gel;

[0030] Figure 6 Comparison of DPPH free radical scavenging ability of refined horse oil, horse oil microemulsion gel and vitamin C;

[0031] Figure 7 Comparison of the ABTS free radical scavenging abilities of refined horse oil, horse oil microemulsion gel and vitamin C. DETAILED DESCRIPTION

[0032] The implementation modes of the present invention are described below in conjunction with the accompanying drawings and relevant embodiments. The implementation modes of the present invention are not limited to the following embodiments, and the present invention relates to relevant necessary components in the technical field, which should be regarded as the known technology in the technical field and can be known and mastered by the technical personnel in the technical field.

[0033] Example 1

[0034] According to the mass ratio of 9:9:8:4, 50g of Cremophor RH-40, PEG-400, IPM (isopropyl myristate) and horse oil were weighed and placed in a beaker, the speed of the constant temperature magnetic stirrer was adjusted to 700r / min, and 50mL of distilled water was added dropwise at 30°C to prepare horse oil microemulsion for use. 1.0g of Carbomer-980 powder was weighed and mixed with 5g of glycerol, distilled water and horse oil microemulsion, and then allowed to stand for 24h to fully swell, and an appropriate amount of 20% triethanolamine solution was added dropwise to adjust the pH value to 5.5, and the horse oil microemulsion gel was prepared by centrifugation at 4000r / min for 10min.

[0035] Example 2

[0036] According to the mass ratio of 7:7:4:2, 50g of Cremophor RH-40, PEG-400, IPM and horse oil were weighed and placed in a beaker, the speed of the constant temperature magnetic stirrer was adjusted to 600r / min, and 50mL of distilled water was added dropwise at 28°C to prepare horse oil microemulsion for use. 1.0g of Carbomer-980 powder was weighed and mixed with 8g of glycerol, distilled water and horse oil microemulsion, and then allowed to stand for 24h to fully swell, and an appropriate amount of 20% triethanolamine solution was added dropwise to adjust the pH value to 5.5, and the horse oil microemulsion gel was prepared by centrifugation at 4000r / min for 10min.

[0037] Example 3

[0038] According to the mass ratio of 12:12:4:2, 50g of Cremophor RH-40, PEG-400, IPM and horse oil were weighed and placed in a beaker, the speed of the constant temperature magnetic stirrer was adjusted to 700r / min, and 50mL of distilled water was added dropwise at 28°C to prepare horse oil microemulsion for use. 0.5g of Carbomer-980 powder was weighed and mixed with 5g of glycerol, distilled water and horse oil microemulsion, and then allowed to stand for 24h to fully swell, and an appropriate amount of 20% triethanolamine solution was added dropwise to adjust the pH value to 5.5, and the horse oil microemulsion gel was prepared by centrifugation at 4000r / min for 10min.

[0039] Example 4

[0040] According to the mass ratio of 27:27:4:2, 50g of Cremophor RH-40, PEG-400, IPM and horse oil were weighed and placed in a beaker, the speed of the constant temperature magnetic stirrer was adjusted to 700r / min, and 50mL of distilled water was added dropwise at 28°C to prepare horse oil microemulsion for use. 0.5g of Carbomer-980 powder was weighed and mixed with 2g of glycerol, distilled water and horse oil microemulsion, and then allowed to stand for 24h to fully swell, and an appropriate amount of 20% triethanolamine solution was added dropwise to adjust the pH value to 5.0, and the horse oil microemulsion gel was prepared by centrifugation at 4000r / min for 10min.

[0041] Example 5

[0042] According to the mass ratio of 9:9:8:4, 50g of Cremophor RH-40, PEG-400, IPM and horse oil were weighed and placed in a beaker, the speed of the constant temperature magnetic stirrer was adjusted to 700r / min, and 50mL of distilled water was added dropwise at 28°C to prepare horse oil microemulsion for use. 0.5g of Carbomer-980 powder was weighed and mixed with 8g of glycerol, distilled water and horse oil microemulsion, and then allowed to stand for 24h to fully swell, and an appropriate amount of 20% triethanolamine solution was added dropwise to adjust the pH value to 6.0, and the horse oil microemulsion gel was prepared by centrifugation at 4000r / min for 10min.

[0043] The quality of the horse oil microemulsion and horse oil microemulsion gel prepared by the present invention is evaluated by the following examples:

[0044] 1. Morphological observation: The morphology of horse oil microemulsion was observed using a transmission electron microscope (TEM). Before observation, a small amount of horse oil microemulsion was dipped into a copper mesh and soaked in a 2% phosphotungstic acid solution for 2 minutes. After taking it out and drying it at room temperature, its morphology was observed. Figure 1 shown.

[0045] It was determined that the horse oil microemulsion was white spherical or ellipsoidal under a transmission electron microscope after negative staining with phosphotungstic acid, and was evenly distributed without aggregation. The droplet size of the microemulsion was below 100 nm, which was in line with the particle size range defined by the microemulsion.

[0046] 2. Determination of particle size, polydispersity index (DPI) and potential: Malvern zeta potential particle size analyzer was used to detect the particle size and Zeta potential of horse oil microemulsion. When measuring the particle size, the horse oil microemulsion sample solution (1 mg / mL) was slowly injected into the sample pool and ensured that no bubbles were generated, and then placed in the injection slot to measure the particle size and distribution. When measuring the Zeta potential, the actual horse oil microemulsion sample was slowly added to the Y-type sample pool and ensured that no bubbles were generated, and then placed in the injection slot to detect the potential. The results are shown in Figure 2. Figure 2.1 This is the particle size distribution diagram of horse oil microemulsion. Figure 2.2 This is the zeta potential distribution diagram of horse oil microemulsion.

[0047] The particle size distribution and size of microemulsion are important indicators reflecting the stability of the microemulsion system. The particle size of horse oil microemulsion is unimodal, with an average particle size of (26.15±0.21) nm and a polydispersity index (PDI) value of (0.27±0.11), which is within the definition of microemulsion. That is, the particle size of microemulsion is mostly unimodal, and the polydispersity index (PDI) value is in the range of 0 to 1. The smaller the PDI value, the more concentrated the particle size distribution. Zeta potential is an important indicator for evaluating the stability of colloidal dispersion system. The larger the zeta potential, the greater the mutual repulsion between particles, the less likely the particles are to agglomerate, and the better the stability of the dispersion system. In general, only the dispersion system with an absolute value of zeta potential greater than 25mV is considered a stable system. The zeta potential distribution diagram of horse oil microemulsion has a zeta potential value of (-28±0.43) mV, indicating that the horse oil microemulsion system is stable.

[0048] 3. Identification of microemulsion type: Take an equal amount of horse oil microemulsion and place it in a glass test tube, add 1 mL of methylene blue solution and Sudan red III solution respectively, and observe the diffusion of these two dye solutions in the horse oil microemulsion. Figure 3 shown.

[0049] The dyeing method is a basic method to determine the type of microemulsion based on the diffusion rate of different dyes in the microemulsion. Sudan red III is an oil-soluble dye, while methylene blue is a water-soluble dye. Therefore, in O / W type microemulsion, the diffusion rate of methylene blue is faster than that of Sudan red III. Similarly, in W / O type microemulsion, the diffusion rate of Sudan red III is faster than that of methylene blue. From the dyeing results, it can be seen that horse oil microemulsion is an O / W type microemulsion.

[0050] 4. Sensory index evaluation: Place the horse oil microemulsion gel in a glass culture dish, observe and record its appearance and aroma. Figure 4 shown.

[0051] Horse oil microemulsion gel is a semi-solid gel that is clear and transparent, has moderate viscosity, good ductility, is non-greasy, and has no special odor.

[0052] 5. Evaluation of physical and chemical indicators: pH determination test: Put the horse oil microemulsion gel in a small beaker, use a pH acidometer to measure and record the value; Heat stability test: Place the horse oil microemulsion gel in a (40±1)℃ oven for 24 hours, take it out and cool it at room temperature, and observe whether the horse oil microemulsion gel has unstable phenomena such as stratification and turbidity; Cold stability test: Place the horse oil microemulsion gel in a (-8±2)℃ refrigerator for 24 hours, take it out and thaw it at room temperature, and observe whether the horse oil microemulsion gel has unstable phenomena such as stratification and turbidity.

[0053] The pH value of horse oil microemulsion gel was 5.4-5.5. There was no significant difference before and after being placed in a (40±1)℃ oven for 24 hours and in a (-8±2)℃ refrigerator for 24 hours.

[0054] 6. Viscosity determination: Put the horse oil microemulsion gel in an EP tube, use a viscometer to measure the viscosity of the horse oil microemulsion gel in parallel and record the value.

[0055] The viscosities of horse oil microemulsion gels were measured by viscometer and were 53422 mPa·s, 53527 mPa·s and 53438 mPa·s respectively.

[0056] 7. Evaluation of moisturizing performance: Weigh an appropriate amount of horse oil microemulsion gel, evenly spread it on a glass slide, and place it in a sealed desiccator at room temperature (25±2)°C and relative humidity (RH) of 55% (saturated potassium carbonate solution) for 12, 24, 36, and 48 hours, then take it out, measure the mass of the horse oil microemulsion gel of Example 1 after different placement times, calculate its moisturizing rate according to the following formula, and compare it with refined horse oil and commercially available moisturizing gel as the control group. The results are as follows Figure 5 shown.

[0057]

[0058] Where:

[0059] mt,55%: represents the mass of horse oil microemulsion gel after being placed under relative humidity of 55% for t hours;

[0060] m0,55%: indicates the mass of the horse oil microemulsion gel when placed at a relative humidity of 55% for 0 hours.

[0061] During the entire storage process, the moisturizing rate of horse oil microemulsion gel was higher than that of commercially available moisturizing gel and the difference between the two was obvious, indicating that horse oil microemulsion gel had a better moisturizing effect than commercially available moisturizing gel. If horse oil microemulsion gel is combined with other cosmetic raw materials, it can be further developed into related moisturizing products.

[0062] 8. Evaluation of antioxidant properties:

[0063] DPPH free radical scavenging test: horse oil microemulsion gel was diluted with anhydrous ethanol to sample solutions with mass concentrations of 1, 2, 3, 4, 5, and 6 mg / mL, respectively. 2 mL of the above solutions were taken into test tubes, mixed with 2 mL of 0.2 mmol / L DPPH free radical solution, and then allowed to stand in the dark for 30 minutes. After standing, the absorbance of the solution was measured at 517 nm. The DPPH free radical scavenging rate of refined horse oil and horse oil microemulsion gel was calculated according to the following formula, and vitamin C was used as a positive control for comparison. The results are as follows: Figure 6 shown.

[0064]

[0065] Where:

[0066] A1: absorbance values ​​of DPPH solution and sample solutions of different concentrations;

[0067] A2: absorbance values ​​of sample solutions with different concentrations and anhydrous ethanol;

[0068] A3: Absorbance values ​​of DPPH solution and anhydrous ethanol solution.

[0069] Horse oil and its microemulsion gel have a certain scavenging effect on DPPH free radicals, which increases with the increase of concentration in the range of 1-6 mg / mL, and the scavenging rate of horse oil microemulsion gel on DPPH is greater than that of refined horse oil at the same concentration. When the mass concentration increases from 1 mg / mL to 6 mg / mL, the scavenging rate of vitamin C on DPPH free radicals is higher than that of horse oil microemulsion gel and refined horse oil at the corresponding concentrations at all concentrations, and the scavenging rate of DPPH free radicals does not change much. The scavenging rate of horse oil microemulsion gel on DPPH free radicals increased from 15.3% to 38.20%, and the IC50 (solution mass concentration when the free radical scavenging rate is 50%) is 8.20 mg / mL. The scavenging rate of horse oil on DPPH free radicals increased from 13.7% to 35.3%, and the IC50 is 9.23 mg / mL, indicating that the construction of horse oil microemulsion gel system can enhance the scavenging ability of refined horse oil on DPPH free radicals.

[0070] ABTS free radical scavenging test: Mix equal volumes of 2.45mmol / L potassium persulfate solution and 7mmol / L ABTS solution, and react at room temperature in the dark for 12 hours to obtain ABTS cation free radical solution. Take 10mL of ABTS cation free radical solution and dilute it with anhydrous ethanol so that its absorbance at 734nm is (0.70±0.02) and set it aside. Use anhydrous ethanol to dilute the horse oil microemulsion gel into sample solutions with mass concentrations of 1, 2, 3, 4, 5, and 6mg / mL. Take 1mL of the above sample solutions in test tubes, mix them with 4mL ABTS cation free radical solution, and let them stand in the dark for 10 minutes. After standing, measure the absorbance at 734nm. The ABTS cation free radical scavenging rate of refined horse oil and horse oil microemulsion gel was calculated according to the following formula, and vitamin C was used as a positive control for comparison. The results are as follows Figure 7 shown.

[0071]

[0072] Where:

[0073] A1: absorbance value of the mixed solution of ABTS cation free radical solution and anhydrous ethanol,

[0074] A2: Absorbance values ​​of ABTS solution and sample solutions of different concentrations

[0075] The scavenging rate of ABTS cationic radicals by refined horse oil and horse oil microemulsion gel in the mass concentration range of 1 to 6 mg / mL is positively correlated with the concentration, and under the same concentration conditions, the scavenging rate of ABTS cationic radicals by horse oil microemulsion gel is higher than that of refined horse oil. In order to further measure the scavenging ability of refined horse oil and horse oil microemulsion gel on ABTS cationic radicals, the IC50 of scavenging rates of refined horse oil and horse oil microemulsion gel on ABTS cationic radicals were calculated to be 7.56 mg / mL and 5.33 mg / mL, respectively, indicating that constructing a microemulsion gel system can enhance the antioxidant capacity of refined horse oil.

[0076] The above is only a preferred embodiment of the present invention. It should be pointed out that ordinary technicians in this technical field can make several improvements and modifications without departing from the principle of the present invention. These improvements and modifications should also be regarded as the scope of protection of the present invention.

Claims

1. A horse oil microemulsion gel, characterized in that: The horse oil microemulsion gel is prepared from horse oil microemulsion, carbomer-980 and glycerol; the horse oil microemulsion is prepared from oil phase, emulsifier, co-emulsifier and water; the oil phase is horse oil and oil phase solvent; the horse oil microemulsion is an O / W type microemulsion.

2. The horse oil microemulsion gel according to claim 1, characterized in that: The horse oil microemulsion is prepared according to the following mass ratio: 1-5 parts of horse oil, 5-10 parts of oil phase solvent, 7-12 parts of emulsifier, 7-12 parts of auxiliary emulsifier and 120-160 parts of water.

3. The horse oil microemulsion gel according to claim 1, characterized in that: The percentage of the carbomer-980 in the horse oil microemulsion is 0.5-1.0%, and the percentage of the glycerol in the horse oil microemulsion is 2-8%.

4. The horse oil microemulsion gel according to claim 1, characterized in that: The percentage of the carbomer-980 in the horse oil microemulsion is 0.8%, and the percentage of the glycerol in the horse oil microemulsion is 5%.

5. The horse oil microemulsion gel according to claim 1, characterized in that: It is prepared according to the following mass ratio: 4 parts of horse oil, 8 parts of oil phase solvent, 9 parts of emulsifier, 9 parts of co-emulsifier, and 150 parts of water.

6. The horse oil microemulsion gel according to claim 1, characterized in that: The emulsifier is Cremophor RH-40.

7. The horse oil microemulsion gel according to claim 1, characterized in that: The co-emulsifier is PEG-40.

8. The horse oil microemulsion gel according to claim 1, characterized in that: The oil phase solvent is IPM.

9. A method for preparing the horse oil microemulsion gel according to any one of claims 1 to 8, characterized in that: The method for preparing the horse oil microemulsion comprises the following steps: (1) mixing the horse oil, the oil phase solvent, the emulsifier, and the co-emulsifier to obtain a mixture; (2) emulsifying the obtained mixture with water to obtain a horse oil microemulsion; (3) mixing the horse oil microemulsion, carbomer-980 and glycerin to obtain a mixture and then allowing it to stand; (4) Add triethanolamine solution to the mixture to adjust the pH to 5-6 to obtain horse oil microemulsion gel.

10. The preparation method according to claim 9, characterized in that: The emulsification temperature is 28-32° C.; the emulsification speed is 650-750 r / min.

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