CN107669513B - Olive oil/VE microemulsion gel with skin-care and bacteriostasis functions and preparation method thereof - Google Patents

Abstract

Mixing oleum Olivarum, vitamin E succinate, menthol, polyoxyethylene hydrogenated castor oil, span80, propylene glycol, phenoxyethanol, and Lavender essential oil at a certain proportion, and dropwise titrating with redistilled water under magnetic stirring to obtain microemulsion. Adding glycerol and chlorhexidine acetate into the microemulsion, stirring uniformly, adding carbomer 980, swelling completely, adjusting pH with triethanolamine, and stirring uniformly. The weight percentages of the components are respectively as follows: 0.5-4 parts of olive oil, 0.4-0.8 part of menthol, 0.1-1 part of vitamin E succinate, 2.5-12 parts of a mixture of polyoxyethylene hydrogenated castor oil and span80 in a mass ratio of 3:1, 2.5-12 parts of propylene glycol, 0.1 part of phenoxyethanol, 0.01-0.02 part of lavender essential oil, 5-10 parts of glycerol, 0.08-0.3 part of chlorhexidine acetate, 0.5-1 part of carbomer 980, 0.01-0.02 part of triethanolamine and the balance of water. The product is simple to prepare, can promote the absorption of vitamin E, has definite antibacterial effect and excellent moisturizing and moistening effects, and is particularly suitable for preventing and treating various skin problems caused by dryness and water shortage.

Description

Olive oil/VE microemulsion gel with skin-care and bacteriostasis functions and preparation method thereof

Technical Field

The invention relates to a skin care product, in particular to a skin care product with moisturizing, moistening, antioxidant and bacteriostatic effects, and specifically relates to olive oil/VE microemulsion gel with skin care and bacteriostatic effects and a preparation method thereof.

Background

Due to factors such as age, climate and environment, the body's intrinsic water and cellular water gradually decrease, and chronic physiological dehydration occurs, accompanied by dry skin, increased wrinkles, itching and infection caused by scratching. In addition to effective prevention, skin care and antisepsis are essential treatments for this.

The olive oil is pure vegetable oil, is rich in unsaturated fatty acid and various vitamins, can moisten and luster the skin, contains polyphenol with an antioxidant effect, and can effectively avoid the phenomena of color spots, wrinkles and the like caused by cell aging due to fat oxidation. Vitamin E is an excellent antioxidant, and helps skin to resist the invasion of free radicals, ultraviolet rays and pollutants, and prevents skin from losing elasticity and even aging. Glycerin is very hygroscopic and is the cheapest and most effective skin moisturizer. Chlorhexidine acetate (chlorhexidine) is a broad-spectrum antibacterial drug, and is mainly used for disinfection of skin and mucosa and wound infection. Menthol is a terpenoid compound, has high polarity, is slightly soluble in water, has the effects of diminishing inflammation, relieving itching and cooling, and is commonly used as a penetration enhancer in a transdermal drug delivery system. If the substances are combined to prepare a preparation, the skin-care and bacteriostatic effects are good. However, the loading and absorption of active substances in conventional emulsions and creams are not ideal.

The microemulsion is a transparent, low-viscosity and thermodynamically stable system formed by water, oil, surfactant and cosurfactant, and is known to be an excellent transdermal drug delivery carrier due to strong solubilization effect on water-insoluble substances and skin permeation promotion effect. The olive oil is used as an oil phase and is designed into a microemulsion preparation, and unfortunately, the test result shows that the microemulsion preparation has very small microemulsion area and the loading amount of the olive oil is less than 0.2 percent when the olive oil is used as the oil phase.

In view of the problems of low loading amount of the existing transdermal delivery carrier and less ideal loading and absorption of the effective substances in the preparation, the preparation with high loading amount of the effective substances, good absorption of human skin, obvious antibacterial and bacteriostatic effects and remarkable moisturizing and moistening effects needs to be developed.

Disclosure of Invention

The invention provides a preparation with skin care and bacteriostasis functions for local and systemic use of skin for preventing and treating dry skin, wrinkle increase, pruritus, infection caused by scratching and the like caused by physiological dehydration, in particular to olive oil/VE microemulsion gel with skin care and bacteriostasis functions and a preparation method thereof.

An olive oil/VE microemulsion gel with skin-care and bacteriostasis functions is prepared from the following raw materials in percentage by weight: 0.5-4% of olive oil, 0.1-1% of vitamin E succinate, 0.4-0.8% of menthol, 2.5-12% of surfactant, 2.5-12% of cosurfactant, 0.1% of preservative, 0.01-0.02% of lavender essential oil, 5-10% of glycerol, 0.08-0.3% of chlorhexidine acetate, 0.5-1% of carbomer 980, 0.01-0.02% of triethanolamine and the balance of water.

The literature indicates that except olive oil, most pure vegetable oils such as soybean oil and corn oil have small micro-emulsion areas, and peppermint oil with larger polarity and micro-molecular carboxylic ester substances form larger micro-emulsion areas. It is suggested that the present invention attempts to use a mixed oil phase, that is, vitamin E succinate, which is also an ester, and menthol, which is a main ingredient of peppermint oil, together are dissolved in olive oil to adjust the polarity of the oil phase, thereby increasing the micro-emulsion area. As a result, the adoption of the mixed oil phase greatly improves the loading amount of the olive oil, so that the preparation of the microemulsion preparation taking the olive oil as the moisturizing component becomes possible.

The invention takes olive oil, vitamin E succinate and glycerin as components with the effects of moistening, moisturizing, resisting oxidation and protecting skin, chlorhexidine acetate as a skin antibacterial and bacteriostatic agent, and microemulsion with excellent solubilizing and percutaneous permeation promoting effects as a carrier to design and prepare the preparation.

Menthol with the effects of relieving itching, cooling and diminishing inflammation is selected as an auxiliary oil phase and a penetration enhancer, and vitamin E is selected from vitamin E succinate which is a derivative thereof so as to adjust the polarity of the oil phase, increase the loading amount of olive oil and improve the percutaneous absorption effect of the preparation.

Selecting safe and odorless polyoxyethylene hydrogenated castor oil (RH 40) as a main surfactant, taking the loading amount of oil-soluble substances as an evaluation index, and screening the surfactant combination by adjusting the hydrophilic-lipophilic balance value. The solubilization effect is best when the mass ratio of RH40 to Span80 is 3:1 (HLB is 12.6).

Selecting propylene glycol with a moisturizing effect as a cosurfactant, wherein the mass ratio of the propylene glycol to the cosurfactant is 1: 1.

The carbomer 980 is used for adjusting the viscosity of the microemulsion to enable the microemulsion to be in a gel state, so that the defects of low viscosity of the microemulsion, poor skin adhesion and difficulty in uniform coating are overcome, and the skin is fine and smooth after the microemulsion is used.

A preparation method of olive oil/VE microemulsion gel with skin-care and bacteriostasis functions comprises the following steps:

(1) mixing olive oil, vitamin E succinate and menthol, and stirring to obtain oil phase;

(2) adding a surfactant and a cosurfactant into the oil phase in the step (1);

(3) adding preservative phenoxyethanol and lavender essential oil into the mixed liquid in the step (2), and fully stirring to obtain a uniform oil-soluble solution;

(4) dropwise adding the redistilled water into the oil-soluble solution obtained in the step (3) under the magnetic stirring action at 40 ℃ to obtain a microemulsion;

(5) adding glycerol and chlorhexidine acetate into the microemulsion obtained in the step (4), and fully and uniformly mixing;

(6) adding carbomer 980 into the microemulsion of step (5), swelling sufficiently, and adjusting pH to 5-7 with triethanolamine to obtain the final product;

(7) the weight percentages of the components are respectively as follows: 0.5-4 parts of olive oil, 0.4-0.8 part of menthol, 0.1-1 part of vitamin E succinate, 2.5-12 parts of surfactant, 2.5-12 parts of cosurfactant, 0.1 part of preservative, 0.01-0.02 part of lavender essential oil, 5-10 parts of glycerol, 0.08-0.3 part of chlorhexidine acetate, 0.5-1 part of carbomer 980, 0.01-0.02 part of triethanolamine and the balance of water.

Furthermore, the surfactant polyoxyethylene hydrogenated castor oil and the span80 are mixed according to the mass ratio of 3:1, the cosurfactant is propylene glycol, and the preservative is phenoxyethanol.

The microemulsion gel with definite antibacterial and bacteriostatic effects can be prepared only by adopting the steps of the method.

The invention has simple preparation, convenient use and strong skin permeability, and has definite antibacterial and bacteriostatic effects and moisturizing and moistening effects.

Drawings

Figure 1 microscopic morphology of example 7 before addition of carbomer 980.

Figure 2 microscopic morphology of the microemulsion gel described in example 7.

Fig. 3 is a moisturizing effect evaluation chart of example 7.

Detailed Description

Example 1 mixing 2g of olive oil, 0.5g of vitamin E succinate and 0.4g of menthol, stirring uniformly, adding 6g of a mixture of polyoxyethylene hydrogenated castor oil and span80 in a mass ratio of 3:1, 6g of propylene glycol, 0.1g of phenoxyethanol and 0.01g of lavender essential oil, slowly dropwise adding 79.4g of distilled water under the magnetic stirring action at 40 ℃, then adding 5g of glycerin and 0.08g of chlorhexidine acetate, stirring uniformly, then spreading 0.5g of carbomer 980 on the surface, fully swelling, and adding 0.01g of triethanolamine. The product is slightly yellow, transparent, has pH of 5.4, and has no substance precipitation and appearance change after standing for several months.

Example 2g of olive oil, 0.5g of vitamin E succinate and 0.4g of menthol are mixed, stirred uniformly, then 6g of polyoxyethylene hydrogenated castor oil and span80 in a mass ratio of 3:1, 6g of propylene glycol, 0.1g of phenoxyethanol and 0.01g of lavender essential oil are added, then 79.16g of distilled water is slowly dropped dropwise under the magnetic stirring action at 40 ℃, then 5g of glycerin and 0.3g of chlorhexidine acetate are added, stirred uniformly, then 0.5g of carbomer 980 is sprinkled on the surface, and after full swelling, 0.01g of triethanolamine is added, thus obtaining the vitamin E succinate oral liquid. The product is slightly yellow, transparent, has pH of 5.5, and has no substance precipitation and appearance change after standing for several months.

Example 3 mixing 2g of olive oil, 0.5g of vitamin E succinate and 0.4g of menthol, stirring uniformly, adding 6g of a mixture of polyoxyethylene hydrogenated castor oil and span80 in a mass ratio of 3:1, 6g of propylene glycol, 0.1g of phenoxyethanol and 0.01g of lavender essential oil, slowly dropwise adding 78.83g of distilled water under the magnetic stirring action at 40 ℃, then adding 5g of glycerin and 0.15g of chlorhexidine acetate, stirring uniformly, then spreading 980 g of carbomer on the surface, fully swelling, and adding 0.01g of triethanolamine. The product is slightly yellow, transparent, has pH of 5.6, and has no substance precipitation and appearance change after standing for several months.

Example 4g olive oil, 1g vitamin E succinate and 0.8g menthol are mixed, after stirring uniformly, 12g polyoxyethylene hydrogenated castor oil and span80 in a 3:1 mass ratio mixture, 4g propylene glycol, 0.1g phenoxyethanol, 0.02g lavender essential oil are added, then 72.45g distilled water is slowly dropped dropwise under the magnetic stirring action at 40 ℃, then 5g glycerin and 0.12g chlorhexidine acetate are added, after stirring uniformly, 0.5g carbomer 980 is scattered on the surface, after sufficient swelling, 0.01g triethanolamine is added, and the product is obtained. The product is slightly yellow, transparent, has pH of 5.2, and has no substance precipitation and appearance change after standing for several months.

Example 5 mixing 0.5g olive oil, 0.1g vitamin E succinate and 0.4g menthol, stirring well, adding 2.5g polyoxyethylene hydrogenated castor oil and span80 mixture in a mass ratio of 3:1, 2.5g propylene glycol, 0.1g phenoxyethanol, 0.01g lavender essential oil, slowly dropping 82.79g distilled water dropwise under the magnetic stirring action at 40 ℃, then adding 10g glycerin and 0.08g chlorhexidine acetate, stirring well, spreading 1g carbomer 980 on the surface, fully swelling, adding 0.02g triethanolamine, and obtaining the product. The product is slightly yellow, transparent, has pH of 6.8, and has no precipitation and appearance change after standing for several months.

Example 6 mixing 1g of olive oil, 0.4g of vitamin E succinate and 0.6g of menthol, stirring uniformly, adding 2.5g of a mixture of polyoxyethylene hydrogenated castor oil and span80 in a mass ratio of 3:1, 2.5g of propylene glycol, 0.1g of phenoxyethanol and 0.01g of lavender essential oil, slowly dropwise adding 81.79g of distilled water under the magnetic stirring action at 40 ℃, then adding 10g of glycerin and 0.08g of chlorhexidine acetate, stirring uniformly, then spreading 1g of carbomer 980 on the surface, fully swelling, and adding 0.02g of triethanolamine. The product is slightly yellow, transparent, has pH of 6.8, and has no precipitation and appearance change after standing for several months.

Example 7 mixing 2g of olive oil, 0.5g of vitamin E succinate and 0.5g of menthol, stirring uniformly, adding 3g of a mixture of polyoxyethylene hydrogenated castor oil and span80 in a mass ratio of 3:1, 3g of propylene glycol, 0.1g of phenoxyethanol and 0.01g of lavender essential oil, slowly dropwise adding 85.3g of distilled water under the magnetic stirring action at 40 ℃, then adding 5g of glycerin and 0.08g of chlorhexidine acetate, stirring uniformly, then spreading 0.5g of carbomer 980 on the surface, fully swelling, and adding 0.01g of triethanolamine. The product is slightly yellow, transparent, has pH of 5.4, and has no substance precipitation and appearance change after standing for several months.

Example 8 mixing 2g of olive oil, 0.5g of vitamin E succinate and 0.5g of menthol, stirring uniformly, adding 3g of a mixture of polyoxyethylene hydrogenated castor oil and span80 in a mass ratio of 3:1, 3g of propylene glycol, 0.1g of phenoxyethanol and 0.01g of lavender essential oil, slowly dropwise adding 85.52g of distilled water under the magnetic stirring action at 40 ℃, then adding 5g of glycerin and 0.3g of chlorhexidine acetate, stirring uniformly, then spreading 0.5g of carbomer 980 on the surface, fully swelling, and adding 0.01g of triethanolamine. The product is slightly yellow, transparent, has pH of 5.4, and has no substance precipitation and appearance change after standing for several months.

Test example 1

The microemulsion characteristics of the present invention were characterized by taking example 7 as a sample.

Example 7 was in the form of a clear liquid without carbomer 980, having an average particle size of 40.79nm, a polymerization index PDI of 0.082, a viscosity of 74.82 + -1.44 mPas, and a microscopic morphology as shown in FIG. 1. Therefore, the shape of the microscopic particles of the sample is round, the particle size is in the nano-scale range, and the distribution is uniform. All indexes meet the characteristics that the grain diameter of the microemulsion is less than 100nm and the viscosity is low.

The viscosity of example 7 was 20.14. + -. 0.34 Pa-s, at which the sample had better pick-up and spreading properties. FIG. 2 shows the microscopic morphology, which shows that the particles have rounded shapes and sizes in the nanometer range.

Test example 2

Evaluation of Using effects of example 7

(1) Evaluation of moisturizing effect 6 volunteers were randomly selected as test subjects, and moisturizing effects were examined by examining the moisture content of the skin before and after smearing microemulsion with normal saline and commercially available vitamin E anti-chapping and anti-bacterial olive oil (gan wei Xiao's syndrome 2010, No. 0076) as a control, with the results shown in fig. 3.

It can be seen that the moisture content of the skin of the 3 groups of samples reaches the peak after being applied to the skin for 1 hour, and then the moisture content is slightly reduced, so that the total moisture content is kept stable and higher than the level before application. Although the physiological saline group can increase the moisture of the skin, the moisture increasing percentage is obviously smaller than that of the physiological saline group in example 7, the P value of the moisturizing effect of the two groups is 0.02 and P is less than 0.05 through the statistical analysis of t test, and the significant difference is shown in the two groups. Example 7 shows no statistical difference from the commercial products, indicating that the products prepared by the present invention can achieve the moisturizing effect of the commercial products.

(2) Evaluation of bacteriostatic Effect

The bacteriostatic effect of the invention is examined by staphylococcus aureus, escherichia coli, pseudomonas aeruginosa and candida albicans. The nutrient broth and the sample of example 8 were added to the tubes inoculated with the bacteria and then added to each tube in sequence according to the fold dilution method. And (3) placing each test tube in a constant temperature box at 37 ℃ for incubation for 24 h, observing the bacteriostatic effect, and obtaining the minimum dilution concentration MIC value of aseptic growth, namely the minimum bacteriostatic concentration of the chlorhexidine acetate on bacteria. The results are 0.03 percent of staphylococcus aureus, 0.01875 percent of escherichia coli, 0.04688 percent of pseudomonas aeruginosa and 0.075 percent of candida albicans. For this reason, the concentration of chlorhexidine acetate in the present invention was determined to be 0.08%.

(3) Survey and evaluation of sensory Effect

The sensory effect of example 7 was evaluated by selecting 12 female volunteers aged about 22 and using commercial vitamin E anti-cracking and bacteriostatic olive oil (jiangwei Xiaozhao 2010, 0076) as a control, and the result shows that the skin of example 7 has fast penetration, is cool and smooth, and does not easily penetrate into the skin and has sticky feeling like the commercial product after use.

Claims (5)

1. An olive oil/VE microemulsion gel with skin-care and bacteriostasis functions is prepared from the following raw materials in percentage by weight: 0.5-4% of olive oil, 0.1-1% of vitamin E succinate, 0.4-0.8% of menthol, 2.5-12% of surfactant, 2.5-12% of cosurfactant, 0.1% of preservative, 0.01-0.02% of lavender essential oil, 5-10% of glycerol, 0.08-0.3% of chlorhexidine acetate, 0.5-1% of carbomer 980, 0.01-0.02% of triethanolamine and the balance of water; the surfactant is prepared by mixing polyoxyethylene hydrogenated castor oil and span80 in a mass ratio of 3: 1; the cosurfactant is propylene glycol.

2. The olive oil/VE microemulsion gel with skin care and bacteriostasis functions as claimed in claim 1, which is characterized in that: the preservative is any one of a mixture of sodium methyl hydroxybenzoate and sodium propyl hydroxybenzoate in a mass ratio of 1:1, imidazolidinyl urea and phenoxyethanol.

3. The olive oil/VE microemulsion gel with skin-care and bacteriostasis functions as claimed in claim 1 or 2, which is characterized in that: the antiseptic is phenoxyethanol.

4. The olive oil/VE microemulsion gel with skin care and bacteriostasis functions as claimed in claim 1, which is characterized in that: the surfactant is a mixture of polyoxyethylene hydrogenated castor oil and span80 in a mass ratio of 3:1, the cosurfactant is propylene glycol, and the preservative is phenoxyethanol; the raw material components by weight percentage are as follows: 2% of olive oil, 0.5% of menthol, 0.5% of vitamin E succinate, 3% of a mixture of polyoxyethylene hydrogenated castor oil and span80 in a mass ratio of 3:1, 3% of propylene glycol, 0.1% of phenoxyethanol, 0.01% of lavender essential oil, 5% of glycerin, 0.08% of chlorhexidine acetate, 0.5% of carbomer 980, 0.01% of triethanolamine and the balance of water.

5. A method for preparing the olive oil/VE microemulsion gel with skin care and bacteriostasis functions as claimed in any one of claims 1 to 4, which is characterized in that: the raw materials and the proportion of any one of claims 1 to 4 are adopted, and the method comprises the following steps:

(1) mixing olive oil, vitamin E succinate and menthol, and stirring to obtain oil phase;

(2) adding a surfactant and a cosurfactant into the oil phase in the step (1);

(3) adding a preservative and the lavender essential oil into the mixed liquid in the step (2), and fully stirring to obtain a uniform oil-soluble solution;

(4) slowly and dropwise adding the redistilled water into the oil-soluble solution in the step (3) under the magnetic stirring action at 40 ℃ to obtain microemulsion;

(5) adding glycerol and chlorhexidine acetate into the microemulsion obtained in the step (4), and fully and uniformly mixing;

(6) and (3) adding carbomer 980 into the microemulsion in the step (5), fully swelling, and adjusting the pH to be 5-7 by using triethanolamine.

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