CN111529440A

CN111529440A - Preparation method of acne-removing emulsion

Info

Publication number: CN111529440A
Application number: CN202010323892.4A
Authority: CN
Inventors: 曾瑶波
Original assignee: China Academy of Chinese Medical Sciences CACMS
Current assignee: China Academy of Chinese Medical Sciences CACMS; Chongqing Academy of Chinese Materia Medica
Priority date: 2020-04-22
Filing date: 2020-04-22
Publication date: 2020-08-14

Abstract

The invention provides a preparation method of an acne-removing emulsion. The method comprises the steps of 1) heating and stirring a water phase matrix and an oil phase matrix to a molten state; step 2) adding the oil phase matrix into the water phase matrix, and emulsifying at a certain rotating speed; and 3) adding a skin conditioner and a humectant, and stirring and mixing uniformly. The method disclosed by the invention is simple in production process, mild in preparation conditions, free of damage to natural active ingredients, high in stability, safe, free of side effects and remarkable in acne removing effect.

Description

Preparation method of acne-removing emulsion

Technical Field

The invention belongs to the technical field of cosmetics, and particularly relates to a preparation method of an acne-removing emulsion.

Background

The emulsion cosmetic is a product which is prepared from an oily raw material and a water-based raw material under the action of a surfactant and has a light yellow to yellowish brown appearance. It is the most common type of skin care products, and cream, honey, milk and the like belong to emulsion products.

Emulsion products can be classified into two types, i.e., water-in-oil type and oil-in-water type, depending on the emulsification properties. Wherein the continuous part in the water-in-oil type product is oily raw material, and the water-based raw material is dispersed in the oily raw material in the form of very small droplets to form an oil-water dispersion system which is greasy and suitable for people with dry skin; the continuous part of the oil-in-water type product is an aqueous raw material, and the oily raw material is dispersed in the aqueous raw material in small liquid drops to form an oil-water dispersion system which is fresh and not greasy and is suitable for people with oily and neutral skin. Cosmetic enterprises often add proper functional or functional substances into basic substances of emulsion products to form cosmetics with various special effects such as whitening, freckle removing, sun protection and the like.

Emulsions are thermodynamically unstable. When the net reduction in interfacial area occurs, the droplets will rearrange from droplet morphology into two volumes of liquid, which is energetically favorable. Emulsion preparation is established by depending on experience for a long time, gradually fills and perfects the theory, and moves to the production guided by the theory. But in practice it still depends on the experience of the operator. Until now, experts who study and produce emulsified products still admit the importance of experience because there are many factors involved in the preparation of emulsions, and there is no theory that can quantitatively guide the emulsification operation, and even experienced operators have difficulty in ensuring that each batch is well emulsified; and the cosmetic emulsion is rich in a large amount of functional natural ingredients, and the natural ingredients can be damaged by the temperature, the emulsifying time and the stirring condition of the production process.

Therefore, a preparation method of the acne-removing emulsion with simple production process and mild preparation conditions without damaging natural active ingredients is needed in the prior art.

Disclosure of Invention

The invention aims to provide a preparation method of an acne-removing emulsion, which at least alleviates one of the technical problems in the prior art.

In order to achieve the purpose, the invention adopts the following technical scheme:

a preparation method of an acne-removing emulsion is characterized by comprising the following steps:

step 1) mixing a solvent, a humectant, a penetration enhancer, borneol, a red sage root extracting solution and a alkanna tinctoria root extract according to a certain proportion, stirring and heating to prepare a water phase matrix;

step 2) mixing the humectant, the lubricant and the emulsifier according to a certain proportion, stirring and heating to prepare an oil phase matrix;

step 3) slowly adding the oil phase matrix into the water phase matrix, and homogenizing at a certain rotating speed; adding xanthan gum solution with the final concentration of 5% (w/w), and continuously stirring;

step 4), adding the aloe vera leaf extract and the humectant into the mixture after passing through a high-pressure homogenizer, and stirring and mixing the mixture uniformly;

step 5) adding the antimicrobial agent to the final emulsion.

Preferably, the step 1) is that the aqueous phase matrix is stirred and heated to 60-100 ℃, and the temperature is kept for 15-25 minutes.

Preferably, the step 2) is to stir the oil phase matrix to raise the temperature to 60-100 ℃ and keep the temperature for 2-10 minutes.

Preferably, the step 3) is to slowly add the oil phase matrix into the water phase matrix, and homogenize at a certain rotation speed of 9500-11000rpm for 1-3 minutes; 5% xanthan gum solution was added and stirring was continued for 3-5 minutes at 12000-14000 rpm.

Preferably, the adding speed of slowly adding the oil phase matrix into the water phase matrix is 3-10kg/min, and the adding and stirring speed is 45-55 rpm.

Preferably, step 4) is carried out by three high-pressure homogenizers with two stages, the pressure being set at 300/30 bar.

Preferably, the temperature in the step 4) is reduced to 30-50 ℃, and the aloe barbadensis leaf extract and the humectant are added and stirred and mixed evenly.

Preferably, the method also comprises the following steps: soaking target Chinese medicinal materials in solvent; adding the wetted medicinal materials into a solvent for soaking for 24 hours; percolating the soaked Chinese medicinal materials at a percolation rate of 50-250 mL/min/kg; collecting percolate, vacuum concentrating and drying to obtain extract; wherein, the solvent is water, ethanol or a solution of the water and the ethanol mixed according to different proportions.

Preferably, the humectant in step 4) is 1, 2-ethanediol.

Preferably, the antimicrobial agent is 0.1% (w/w) methylparaben.

Preferably, in the step 1), the solvent in the water phase matrix is water and ethanol, the humectant is 1, 3-propylene glycol and glycerol, the freshener is borneol, the penetration enhancer is laurocapram, the humectant in the oil phase matrix is petrolatum, lanolin and sodium stearyl glutamate, the lubricant is polydimethylsiloxane, and the emulsifier is cetostearyl alcohol.

More preferably, the final ethanol content is 5% (w/w).

The invention has the beneficial technical effects that:

1. the preparation method provided by the invention is simple in process flow and easy for large-scale production.

2. The emulsion particles produced by the preparation method of the invention are in a sphere-like shape, and the particle diameter is smaller; the emulsion has high stability and is not easy to separate.

3. The emulsion produced by the preparation method has obvious bacteriostatic effect and can obviously improve the damaged skin of the acne patient.

Detailed Description

Embodiments of the present invention will be described in detail below with reference to examples, but it will be understood by those skilled in the art that the following examples are only illustrative of the present invention and should not be construed as limiting the scope of the present invention. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by manufacturers, and are all conventional products available on the market.

Example 1 preparation of an anti-acne cream according to the invention

Formula (the following are w/w):

the process comprises the following steps:

step 1) mixing the water, the glycerol, the salvia miltiorrhiza extract, the 1, 3-propylene glycol, the ethanol, the borneol, the laurocapram, the methylparaben and the alkanna tinctoria root extract according to the proportion, stirring and heating to 85 ℃, and keeping the temperature for 20 minutes;

step 2) mixing petrolatum, lanolin, polydimethylsiloxane, cetostearyl alcohol and sodium stearyl glutamate according to a certain proportion, stirring and heating to 85 ℃, and keeping the temperature for 5 minutes;

step 3) adding the oil phase matrix into the water phase matrix, wherein the adding speed is 3-10kg/min, the adding stirring rotating speed is 45-55rpm, and emulsifying for 1 minute at the rotating speed of 10000; adding a xanthan gum solution with the final concentration of 5% (w/w) and stirring for 4 minutes at 13000 rpm;

step 4), passing through a three-time two-stage high-pressure homogenizer, wherein the pressure is set to be 300/30 bar; cooling to 30-50 deg.C, adding Aloe Barbadensis Miller leaf extract and 1, 2-ethylene glycol, and stirring;

step 5) add 0.1% methylparaben to the final emulsion.

EXAMPLE 2 measurement of particle size and morphology of emulsion

The emulsion produced by the preparation method is diluted by 50 times by adding distilled water, a proper amount of the emulsion is uniformly coated on a glass slide, the shape of the emulsion is observed by adjusting the magnification of an optical microscope, and the particles in the emulsion are in a sphere-like shape and have the diameter of 30-100 mu m.

EXAMPLE 3 emulsion stability experiment

The emulsion produced by the preparation method is put into a 10cm centrifuge tube, and is centrifuged at the speed of 3750rpm for 5 hours, so that the emulsion is not layered. Each set of 3 replicates.

Example 4 Heat and Cold resistance test

The product is stored in a constant temperature and humidity incubator at 40 ℃ for 48 hours and then taken out, and the oil-water separation phenomenon is observed after the room temperature is recovered; and (3) taking out the emulsion after being placed in a refrigerator at the temperature of-8 ℃ for 48 hours, and observing the oil-water separation phenomenon after the room temperature is recovered, wherein the emulsion has no layering phenomenon. Each set of 3 replicates.

EXAMPLE 5 Rabbit skin Single dose toxicity test

The method comprises the following steps: selecting 60 New Zealand rabbits, and randomly dividing the rabbits into 6 groups: the whole skin blank control group, the whole skin matrix control group, the whole skin administration group, the damaged skin blank control group, the damaged skin matrix control group and the damaged skin administration group, wherein 6 rabbits (female and male halves) are applied to each group at an administration dose of 15g cream/rabbit (6.0g crude drug/rabbit) (maximum administration dose and maximum drug concentration), and the skin is applied and administered 3 times every day at intervals of 4h (the blank control group is given with physiological saline with the same volume, and the matrix control group is given with matrix with the same volume). After administration, the toxic reaction was observed for 28 consecutive days, and body weight, hematology, blood biochemistry and other indicators were measured.

After administration, no obvious abnormality was observed in the rabbits of the intact skin group and the damaged skin group, and no death occurred in the animals. No obvious influence is seen on the weight of each group of rabbits after administration and the weight increase. After the observation is finished, the rabbits are subjected to gross observation, and the skin and the main organs of the administration part of each group of rabbits have no obvious abnormality. After 24 hours of administration, the hematology and blood biochemistry indexes of each group of rabbits have no obvious influence.

Under the experimental condition, the maximum administration area and the maximum concentration (0.4g crude drug/g cream) of the skin smearing administration for three times within 24 hours have no obvious influence on the rabbits.

Example 6 active skin allergy test

The method comprises the following steps: 120 guinea pigs were selected for this study and randomized into 4 groups: the vehicle control group, the administration group-1 group, the administration group-2 group, the positive control group, and 30 guinea pigs (male and female halves) in each group were subjected to the guinea pig active systemic anaphylaxis test. The dose of the group-1 was 0.3g cream/body (0.12g crude drug/body) (maximum drug concentration), the dose of the group-2 was 0.3g cream/body (0.06g crude drug/body) (clinical drug concentration), the positive control group was administered 0.2ml of 1% 1-chloro-2, 4-dinitrobenzene, and the matrix control group was administered the same amount of matrix. Sensitization administration was performed on days 0, 7, 14, and 21, and priming administration was performed 21 days after the last sensitization, each time 0.3 g/body (0.2 ml of 0.1% 1-chloro-2, 4-dinitrobenzene was administered to the positive control group), and the skin was sufficiently contacted for 6 hours.

During sensitization administration, the substrate control group, the administration group-1 group and the administration group-2 group were applied to the skin for 3 times of sensitization administration, and no erythema or edema symptoms occurred in each animal. After the priming, the incidence of skin sensitization to guinea pigs was 0% within 168 hours after the priming of the vehicle control group, the administration group-1, and the administration group-2, and the mice were judged to have no skin allergy.

No obvious skin allergic reaction is observed in the matrix control group, the administration group-1 group and the administration group-2 group of the administration group.

Example 7 study of bacteriostatic Activity

Strain:

propionibacterium acnes standard strain ATCC1I827 and Staphylococcus aureus standard strain ATCC 100817.

Reagent:

acne propionibacterium acnes culture medium; brain heart infusion culture medium; culture medium of staphylococcus aureus beef extract

The culture medium is prepared by a conventional method, and the pH value is adjusted to 7.1-7.2. Sealing the culture medium in a conical flask, sterilizing in a sterilizing pot at 121 deg.C for 30min, cooling, and storing in a refrigerator at 4 deg.C.

The preparation of the bacterial suspension comprises the steps of respectively inoculating standard strains for culture and enrichment, culturing for 24h under the conventional culture conditions (culturing propionibacterium acnes for 48h by using an anaerobic glove box), diluting the absorbed bacterial liquid by using a culture medium to adjust the concentration to 0.5 McRIBU unit (about 1.5X108CFU/mL), continuously diluting the bacterial suspension by using the culture medium, and adjusting the concentration to 1X 105-106 CFU/mL by using a McRIBU turbidimeter for later use.

Determination of zone of inhibition

Respectively taking the bacterial suspensions under the aseptic operation condition, and uniformly coating the bacterial suspensions on a culture medium by using a coating rod. And lightly placing the oxford cup on the surface of the solidified culture medium by using sterile forceps, and lightly pressing the oxford cup to ensure good contact. And (3) sucking the test solution into an Oxford cup by using a disposable injection needle, culturing for 24 hours in an incubator at 37 ℃, taking out (culturing propionibacterium acnes for 48 hours by using an anaerobic glove box), and accurately measuring the diameter of the effective inhibition zone of the test solution in each culture dish by using a caliper. Each sample was repeated 3 times.

Experimental groups: the acne treatment cream described herein; control group: blank control group (culture medium), negative control group (culture medium, bacterial suspension, sterile water), and positive control group (culture medium, bacterial suspension, erythromycin). Specifically, as shown in table 1, it can be seen from table 1 that the anti-acne emulsion produced by the present invention has a significant antibacterial effect, and has a certain inhibitory effect on staphylococcus aureus and propionibacterium acnes.

TABLE 1 anti-acne cream bacteriostatic effect

Example 8 efficacy evaluation

Testing an instrument: VISIA 7, ANTERA-3D, Tewameter TM300

The test period was 5 weeks, during which the volunteers used the test samples in the morning and evening of the full face, in the order of use: face wash, test sample, moisturizing milk.

Volunteers visited before (W0), 1 week after (W1), 2 weeks after (W2), 3 weeks after (W3), and 5 weeks after (W4) the use (W5). The face was cleaned with a facial cleanser and sat in an evaluation room test environment for 20min during which time no water or beverage was available. After sitting still, VISIA, ant-3D facial image acquisition and facial water loss rate (TEWL) test were performed on the face. And fill out the questionnaire.

The effective test population is 30, the age is 18-35 years, the face has skin damage, namely: stage I: acne alone; and II, stage: inflammatory papules; grade III: pustules.

And (3) testing environment: temperature (22 +/-1) DEG C and humidity (55 +/-5)%, and real-time dynamic monitoring is carried out.

The test results are summarized as table 2, and it can be seen from table 2 that indexes such as facial pores, facial protrusions, heme, TEWL and the like are reduced to a certain extent after the test population uses the acne-removing emulsion for 5 weeks, the volume and the area of the facial pores are reduced, the number of the facial pores is reduced, the volume of the facial protrusions is reduced, the affected area of the heme is reduced, and the TEWL is reduced; and after the use for 1 week and 2 weeks, each index is obviously reduced, and as the use time is prolonged, each index is continuously reduced, and after the use for about 4 weeks, the data have a stable trend.

TABLE 2 analysis of facial indices

The results of the survey questionnaire of the tested population show that: the acceptance degree of testers on the mildness and the acne removing effect of the test sample is high, and 95% of testers think that the test sample has an obvious inhibition effect on acne; 92% of the testers considered that the test sample had a better improvement effect on the skin; the 87% of the testers considered the test sample to be milder and non-irritating to the skin.

The combination of facial test data and questionnaire results shows that the product of the invention can significantly inhibit acne, improve damaged skin, and is non-irritating both when and after use.

The results show that the preparation method has simple flow and is easy for large-scale production; the preparation condition is mild, and the natural activity of the skin conditioner is not damaged; the produced acne-removing emulsion has obvious antibacterial effect, can obviously improve the damaged skin of acne patients, and is obviously superior to the prior art.

Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.

Claims

1. The preparation method of the acne-removing emulsion is characterized by comprising the following steps:

step 1) mixing a solvent, a humectant, a penetration enhancer, borneol, a salvia miltiorrhiza extract and a alkanna tinctoria root extract according to a certain proportion, stirring and heating to prepare a water phase matrix;

step 5) adding an antimicrobial agent to the final emulsion.

2. The preparation method according to claim 1, wherein the step 1) is to heat the aqueous phase matrix to 60-100 ℃ with stirring and keep the temperature constant for 15-25 minutes.

3. The preparation method according to claim 1, wherein the step 2) is to heat the oil phase matrix to 60-100 ℃ with stirring and keep the temperature constant for 2-10 minutes.

4. The preparation method as claimed in claim 1, wherein the step 3) is to slowly add the oil phase matrix into the water phase matrix, and homogenize at 9500-11000rpm for 1-3 minutes; 5% xanthan gum solution was added and stirring was continued for 3-5 minutes at 12000-14000 rpm.

5. The preparation method according to claim 4, wherein the adding speed is 3-10kg/min, and the adding stirring speed is 45-55 rpm.

6. The method of claim 1, wherein step 4) is performed by a three-stage two-stage high pressure homogenizer at a pressure set at 300/30 bar.

7. The preparation method according to claim 1, wherein the temperature in step 4) is reduced to 30-50 ℃, and the aloe vera leaf extract and the humectant are added, stirred and mixed uniformly.

8. The method according to claim 1, further comprising a process of preparing an extract: soaking target Chinese medicinal materials in solvent; adding the wetted medicinal materials into a solvent for soaking for 24 hours; percolating the soaked Chinese medicinal materials at a percolation rate of 50-250 mL/min/kg; collecting percolate, vacuum concentrating and drying to obtain extract; wherein, the solvent is water, ethanol or a solution of the water and the ethanol mixed according to different proportions.

9. The method of claim 1, wherein the antibacterial agent is 0.1% (w/w) methylparaben.

10. The preparation method according to claim 1, wherein in step 1), the solvent in the aqueous phase matrix is water or ethanol, the humectant is 1, 3-propylene glycol or glycerin, the penetration enhancer is laurocapram, the humectant in the oil phase matrix is petrolatum, lanolin or sodium stearyl glutamate, the lubricant is polydimethylsiloxane, and the emulsifier is cetostearyl alcohol; wherein the final content of ethanol is 5% (w/w).

11. The method according to claim 1, wherein the humectant in the step 4) is 1, 2-ethanediol.