CN114306164B - Antibacterial acne-removing cream and preparation method thereof - Google Patents
Antibacterial acne-removing cream and preparation method thereof Download PDFInfo
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Abstract
The invention provides an antibacterial acne-removing cream, and belongs to the technical field of facial cleansing cream and daily chemicals. The antibacterial acne-removing cream comprises raspberry leaf extract, wherein the preparation method of the raspberry leaf extract comprises the steps of drying and crushing raspberry leaves, mixing the crushed raspberry leaves with tartaric acid, adding an ethanol solution for extraction, filtering insoluble substances after the extraction is finished, concentrating, extracting and decoloring by using ethyl acetate, and extracting an aqueous phase after the extraction by using n-butanol. And finally, rotationally evaporating the n-butanol phase to obtain a solid substance which is the raspberry leaf extract. The antibacterial acne-removing cream has the functions of resisting bacteria and removing acnes, can inhibit propionibacterium acnes for a long time, effectively solves the problem that facial acnes in puberty appear repeatedly, and can also enhance the antibacterial capability of skin after long-term use.
Description
Technical Field
The invention relates to the technical field of facial cleansing cream, in particular to an antibacterial acne-removing cream and a preparation method thereof.
Background
Acne is also called whelk, and facial acne is a common skin disease, is commonly seen in teenagers, and is not limited by age. Facial acne is of many types, and is mainly caused by polymorphic skin lesions such as facial acne, pimples, pustules, nodules and the like. Severe suppuration also occurs, so facial acne needs to be treated in time. The occurrence of acne is closely related to the factors such as hypersecretion of sebum, blockage of the pilosebaceous ducts, bacterial infection and inflammatory reaction. The levels of androgens, particularly testosterone, in humans rapidly rise after puberty, promoting sebaceous gland development and producing large amounts of sebum. If the grease can not be discharged in time to block pores, the anaerobic propionibacterium acnes are greatly proliferated to destroy epidermal cells, thereby triggering inflammatory reaction.
The Rubi fructus is an ancient Chinese medicine, and is dry fruit of Rubi fructus of Rosaceae. Distributed in Jiangsu, zhejiang, anhui, fujian, jiangxi, guangxi, guizhou and other places. Has effects of invigorating kidney, stopping nocturnal emission, reducing urination, nourishing liver, and improving eyesight. It is commonly used for seminal emission, spermatorrhea, enuresis, frequent urination, impotence, premature ejaculation, dim eyesight and dim flowers. In Ben Cao gang mu, it is recorded that Rubi fructus is a medicine for nourishing true yin, and is slightly sour in flavor, so Kou Zong is good at tonifying kidney and reducing stool, and it is also reasonable to take it while covering its drowning device. The book of this application mainly sets five zang organs and yin of the zang organs. All cases are firm and can tonify spleen and stomach, and acid can nourish yin of five zang organs to replenish essence and qi. All cases are heavy and can tonify kidney, but they are also dedicated to kidney yin, can strengthen kidney qi and strengthen the mind and power and nourish kidney yin.
The raspberry is vine shrub with a height of 1.5-3 m; thin branches, skin thorns and no fur. Single leaf, nearly round, 4-9 cm diameter, soft or nearly no hair on two sides along the veins, heart shape at the base, 5 deep cracks at the edge palm, thin 3 or 7 cracks, oval or rhombus oval shape at the split, tapering at the top, pinching at the base, nearly equal length or slightly longer top and side split, heavy sawtooth, 5 veins at the palm; the length of the petiole is 2-4 cm, the petiole is slightly soft or has no fur, and small skin thorns are dredged; the supporting leaf is shaped like a linear needle. Axillary growth of single flower with diameter of 2.5-4 cm; the pedicel is 2-3.5 (4) cm long and has no hair; the calyx hair is thinner or nearly hairless; the sepal is oval or oval, the top end is provided with a convex tip, and the outside is tightly covered by short soft hair; oval or oval petals, white, round top end, 1-1.5 cm long and 0.7-1.2 cm wide; a plurality of stamens and a plurality of filaments are wide and flat; the pistil is a plurality of with soft hair. The fruits are nearly spherical, red, and have a diameter of 1.5-2 cm, and are densely covered with gray and soft hairs; the nucleus has wrinkles. 3-4 months in flowering period and 5-6 months in fruit period.
The applicant obtains the raspberry leaf extract by extracting and purifying the effective components in the raspberry leaves, researches on various activities of the raspberry leaf extract, and discovers that the raspberry extract has very good antibacterial effect on gram positive bacteria such as propionibacterium acnes, staphylococcus aureus and the like, and then the applicant prepares a natural antibacterial acne-removing cream through a formula for enhancing the activity of oil removal and the like of skin care products, so that the problem of repeated occurrence of facial acne in adolescence can be effectively solved, and the antibacterial capability of skin can be enhanced after long-term use.
Disclosure of Invention
The invention aims to provide a facial cleansing cream capable of preventing and removing acnes, which comprises raspberry leaf extract, wherein the preparation method of the raspberry leaf extract comprises the steps of drying and crushing raspberry leaves, mixing the crushed raspberry leaves with tartaric acid, adding 50-75% ethanol solution in volume fraction, extracting for 10-120 min at 60-65 ℃, filtering out insoluble substances after extraction, concentrating, extracting and decoloring with ethyl acetate, and extracting the extracted water phase with n-butanol. And finally, rotationally evaporating the n-butanol phase to obtain a solid substance which is the raspberry leaf extract.
The antibacterial acne-removing cream consists of raspberry leaf extract, tartaric acid, glycerol, nicotinamide, hyaluronic acid, grape seed extract, rosemary extract and carbomer.
The antibacterial acne-removing cream also comprises a pure water of the leaf of the basin, wherein the pure water, tartaric acid and powder of the leaf of the basin are distilled, water vapor is collected, distilled turbid liquid is condensed and accumulated in a receiving bottle along with the hot vapor, the distilled liquid is stood, the distilled liquid is layered, the upper layer is essential oil, and the lower layer is the pure water of the leaf of the basin.
The invention provides an antibacterial acne-removing cream which comprises the following components: 0.1-5 mg/mL of raspberry leaf extract, 0.5-1 mg/mL of tartaric acid, 1-5% of glycerin by volume percent, 0.1-0.5 mg/mL of nicotinamide, 0.2-0.4 mg/mL of hyaluronic acid, 0.2-0.4 mg/mL of grape seed extract, 0.1-0.3 mg/mL of rosemary extract, 1.2-1.8 mg/mL of carbomer and the balance of pure water.
The invention provides another formula of antibacterial acne-removing cream, which comprises the following components: 0.1-5 mg/mL of raspberry leaf extract, 0.5-1 mg/mL of tartaric acid, 1-5% of glycerin by volume percent, 0.1-0.5 mg/mL of nicotinamide, 0.2-0.4 mg/mL of hyaluronic acid, 0.2-0.4 mg/mL of grape seed extract, 0.1-0.3 mg/mL of rosemary extract, 1.2-1.8 mg/mL of carbomer and the balance of raspberry leaf truffle.
Wherein the raspberry leaf extract is used for preparing antibacterial acne-removing cream and inhibiting propionibacterium acnes; the preparation method of the raspberry leaf extract comprises the steps of drying and crushing raspberry leaves, mixing crushed raspberry leaves with tartaric acid, adding an ethanol solution with the volume fraction of 50-75%, extracting for 10-120 min at the temperature of 60-65 ℃, filtering insoluble substances after extraction, concentrating, extracting and decoloring by using ethyl acetate, and extracting the water phase after extraction by using n-butanol. And finally, rotationally evaporating the n-butanol phase to obtain a solid substance which is the raspberry leaf extract.
Meanwhile, the extraction is carried out for 10-120 min by adopting ultrasonic auxiliary extraction under the condition of 150-250 w. The mass volume ratio of the crushed washbasin cotyledon to the ethanol water solution is 40-60 g/L, and the mass volume ratio of the tartaric acid to the ethanol water solution is 2.667-4 g/L. The mass volume ratio of the raspberry leaf powder to the pure water is 166.67-300 g/L, and the mass volume ratio of the tartaric acid to the pure water is 6.667-20 g/L.
Advantageous effects
The research of the research subject group shows that after the mixture of the raspberry leaves and the tartaric acid, the substances extracted by the ethanol have strong antibacterial effect on staphylococcus aureus and propionibacterium acnes, the antibacterial component has good antibacterial effect under the action of the tartaric acid, and the analysis reasons are that certain groups of the tartaric acid and flavonoid or polyphenol substances in the raspberry leaves have complexation or synergism, so that the raspberry leaves generate a strong antibacterial substance, the experimental results show that the antibacterial effect is longer, but the antibacterial component has certain instability, and the applicant also solves the problem of unstable property by adding natural antioxidant substances such as grape seed extract, rosemary extract and the like.
The extract of the leaf of the basin has good antibacterial effect, especially has good antibacterial effect on anaerobic microorganisms such as propionibacterium acnes, staphylococcus aureus and the like, so that the applicant prepares the antibacterial acne-removing cream which can be effectively absorbed by skin, and the antibacterial components in the antibacterial acne-removing cream can inhibit the growth of propionibacterium acnes, thereby effectively inhibiting the growth of propionibacterium acnes and achieving the acne-removing effect. Other pathological acne is temporarily unresolved.
The antibacterial acne-removing cream prepared by the invention has good antibacterial effect on Propionibacterium acnes, has the characteristics of good antibacterial effect, long persistence and the like, and has the advantages of natural components as all components, high safety and certain economic benefit.
Detailed Description
In this example, grape seed extract and rosemary extract are commercially available and the other reagents are analytically pure.
Example 1
The present example is an experiment of the bacteriostasis of the raspberry leaf extract.
Drying raspberry leaves, crushing the raspberry leaves into powder, weighing 30g of raspberry leaves and 2g of tartaric acid, adding 750mL of ethanol solution with the volume fraction of 60%, performing ultrasonic-assisted extraction for 30min at the temperature of 60-65 ℃ with 200w of power, filtering insoluble substances after extraction, performing rotary evaporation and concentration on the filtrate, concentrating to 20mL, extracting and decoloring with ethyl acetate with the same volume, and extracting the extracted water phase with n-butanol with the same volume. And finally, rotationally evaporating the n-butanol phase to obtain a solid substance, and obtaining the raspberry leaf extract.
The propionibacterium acnes cultured for 12 hours are used for measuring OD by a double dilution method 600 Post-positioning OD 600 1, 1 more: 100 are respectively diluted in 10 EP pipes, 20mg/mL of raspberry leaf extract or other traditional Chinese medicine extracts are added into a first pipe, the first pipe is fully and uniformly mixed, then 500uL is sucked and transferred into a second pipe, the second pipe is pushed until a ninth pipe is used as a reference, and the tenth pipe is placed in a constant temperature incubator for static culture for 24 hours, and experimental results are observed. This experiment was repeated three times.
Table 1 minimum inhibitory concentration of Rubi fructus leaf extract and Chinese medicinal material extract on Propionibacterium acnes
The research shows that the raspberry leaf extract extracted under the tartaric acid environment has a certain antibacterial effect on Propionibacterium acnes, the antibacterial effect is even far stronger than that of traditional antibacterial traditional Chinese medicinal materials, about 20-40 times of that of other traditional Chinese medicinal material extracts, and the results of the accelerated experiments of the raspberry leaf extract under the constant temperature condition of 40 ℃ are shown in the following table.
TABLE 2 influence of shelf-life of Rubi fructus leaf extract on minimum inhibitory concentration of Propionibacterium acnes
| MIC(mg/mL) | 0d | 2d | 4d | 8d | 16d |
| PA1 | 0.52 | 1.59 | 2.79 | 6.21 | 10.37 |
As can be seen from table 2, the antibacterial effect of the raspberry leaf extract after 8d storage at 40 ℃ is slightly reduced, and the antibacterial effect after 16d is significantly reduced, and it can be seen that the antibacterial active substances extracted by tartaric acid start to be destroyed.
Example 2
The embodiment provides an antibacterial acne-removing cream and a preparation method thereof, and the specific steps are as follows:
drying raspberry leaves, crushing the raspberry leaves into powder, weighing 30g of raspberry leaves and 2g of tartaric acid, adding 750mL of ethanol solution with the volume fraction of 75%, performing ultrasonic-assisted extraction for 60min at the temperature of 60-65 ℃ with the power of 150w, filtering insoluble substances after extraction, performing rotary evaporation and concentration on the filtrate, concentrating to 20mL, extracting and decoloring with ethyl acetate with the same volume, and extracting the extracted water phase with n-butanol with the same volume. And finally, rotationally evaporating the n-butanol phase to obtain a solid substance, and obtaining the raspberry leaf extract.
Preparation of the leaf hydrolat of the basin: 150mL of purified water, 1g of tartaric acid and 25g of raspberry leaf powder were placed in a distillation flask and placed on a heat source, and a condenser tube and a receiving flask were fitted. The pure water and raspberry leaf powder in the retort are heated to boiling to produce steam, the steam being distilled off carrying some volatile small substances. During distillation, turbid liquid is condensed with hot vapor and accumulated in a receiving bottle, and when distillation is nearly finished, the distilled liquid is clarified from turbid. The vapor of the mixture of organic matter and water is condensed into emulsion through a condensing pipe and enters a receiver. When all the steamed substances are steamed out, the steamed liquid is changed from turbidity to clarification, and 10-20 mL of transparent distillate is steamed out to stop distillation. Standing to separate distilled liquid, wherein the upper layer is essential oil, and the lower layer is Rubi fructus She Chunlou, and diluting with pure water for 1 time to obtain diluted leaf hydrolat.
100mL volume, raspberry leaf extract 100mg, tartaric acid 0.5g, glycerin 5mL, nicotinamide 0.1g, hyaluronic acid 0.2g, grape seed extract 0.2g, rosemary extract 0.1g, carbomer 1.5g, adopting diluted raspberry liquid to achieve a volume of 100mL, and uniformly mixing to obtain the antibacterial acne-removing cream.
Table 3: relation of carbomer concentration in 100mL system
| Concentration of | 0.0025％ | 0.005％ | 0.0075％ | 0.01％ | 0.015％ | 0.02％ |
| Viscosity of the product | - | - | + | ++ | +++ | +++ |
"-" means that the solution is very low in viscosity and "+" means the degree of viscosity
The 0.01 percent of the material is formed, but the solidification degree is insufficient, and the material still has certain fluidity; 0.02% has sufficient coagulability but too high viscosity and poor skin feel, so 0.015% was chosen as the final concentration.
The applicant carries out an accelerated experiment on the antibacterial acne-removing cream prepared in the embodiment under the constant temperature condition of 40 ℃, and the result of the minimum antibacterial concentration is shown in the following table.
TABLE 4 Effect of Rubi fructus leaf extract on minimum inhibitory concentration of Propionibacterium acnes
The results in the table show that the antibacterial stability of the antibacterial acne-removing cream is obviously improved, and the antibacterial effect is hardly reduced in the 20d accelerated experimental period.
The test results show that the skin of the tested mice has no phenomena such as erythema, allergy, edema and the like, and the antibacterial acne-removing cream has good safety and no stimulation to the skin.
After ensuring safety, the subject group summoned 20 testers with at least 10 acnes on the face between 18 and 20 years old, tested, and tested propionibacterium acnes in the vicinity of each acne and cultured.
The number of propionibacterium acnes colonies was determined as follows.
(1) Preparation: accurately weighing 2.90g of thioglycolate fluid culture medium powder, putting the powder into a high-pressure-resistant glass bottle, adding 1.50g of agar, adding 100mL of distilled water, heating, stirring, dissolving to boil, adding liquid paraffin with the thickness of 1cm, and sterilizing at 121 ℃ for 15min. The culture medium is cooled for standby after oxygen is removed by using a pre-boiling water bath for about 10 min.
(2) Sampling: the skin on the acne surface was sterilized with 75% ethanol, and after piercing the acne with a sterilizing needle, the acne content was pressed out and placed in the above medium, and gently shaken to sink under the liquid paraffin layer.
(3) Culturing: the acne content is picked up by an inoculating loop and placed on a sterile slide, and the sterile slide is repeated on the content, and the two slides are extruded, so that the content is pressed into a thin layer. The lamina, and in particular the central portion thereof, was picked up with an inoculating loop and streaked onto a GAM dish (specially for anaerobic cultivation). Placing the plate in an anaerobic bag, sealing, and culturing in an anaerobic tank at 37deg.C for more than three days. Anaerobic culture positive people need to be subjected to an oxygen tolerance test, and anaerobic growth is carried out while aerobic non-growth is carried out.
(4) And (3) identification: and (5) picking suspicious pathogenic bacteria colonies from the cultured plates for pure culture and identification. Propionibacterium colonies are convex, smooth, round, off-white, off-yellow or pale red brown, have diameters of about 1mm (72 h) or less, and smaller colonies are needle-pointed. The gram stain of the thallus is purple (positive), without spores and capsules, and the microbending is in a rod shape or a polymorphic shape (one end is pure round, the other end is thin or sharp, a sphere rod shape, a sphere shape or a fork shape). Propionibacterium acnes can be initially distinguished from other gram-positive anaerobic bacilli by colony morphology.
The antibacterial acne-removing cream is applied to 20 volunteers once a day at 8 am and at 8 pm respectively, secretion of 3 different acne-growing places is picked at 2 pm each day, the mixture is inoculated into a culture medium for culture, the number of bacterial colonies is counted after the culture, the average number of 20 culture samples is taken, and the average number of bacterial colonies in different periods is shown in the table below.
Table 5: colony count at volunteer acne growth sites on different days of application
| Days (d) | 1 | 2 | 3 | 4 | 5 | 6 |
| Average colony count | 16.75 | 8.30 | 1.65 | 0.85 | 0.80 | 0.70 |
The results show that after the antibacterial acne-removing cream disclosed by the invention is coated, propionibacterium acnes at the acne-growing positions of volunteers are obviously inhibited and reduced, and most of volunteers shrink or disappear at the acne-growing positions after 5 days, so that the antibacterial acne-removing cream disclosed by the invention has a certain inhibition effect on propionibacterium acnes and can be used for assisting in treating acne.
Example 3
The embodiment provides an antibacterial acne-removing cream and a preparation method thereof, and the specific steps are as follows:
drying raspberry leaves, crushing the raspberry leaves into powder, weighing 45g of raspberry leaves and 3g of tartaric acid, adding 750mL of ethanol solution with the volume fraction of 70%, performing ultrasonic-assisted extraction with power of 250w for 30min at 60-65 ℃, filtering insoluble substances after extraction, performing rotary evaporation and concentration on the filtrate, concentrating to 20mL, extracting and decoloring with ethyl acetate with equal volume, and extracting the extracted water phase with n-butanol with equal volume. And finally, rotationally evaporating the n-butanol phase to obtain a solid substance, and obtaining the raspberry leaf extract.
Preparation of the leaf hydrolat of the basin: 150mL of purified water, 3g of tartaric acid and 45g of raspberry leaf powder were placed in a distillation flask and placed on a heat source, and a condenser tube and a receiving flask were fitted. The pure water and raspberry leaf powder in the retort are heated to boiling to produce steam, the steam being distilled off carrying some volatile small substances. During distillation, turbid liquid is condensed with hot vapor and accumulated in a receiving bottle, and when distillation is nearly finished, the distilled liquid is clarified from turbid. The vapor of the mixture of organic matter and water is condensed into emulsion through a condensing pipe and enters a receiver. When all the steamed substances are steamed out, the steamed liquid is changed from turbidity to clarification, and 10-20 mL of transparent distillate is steamed out to stop distillation. Standing to separate distilled liquid, wherein the upper layer is essential oil, and the lower layer is Rubi fructus She Chunlou, and diluting with pure water for 1 time to obtain diluted leaf hydrolat.
Under the volume of 100mL, 0.5g of raspberry leaf extract, 0.2g of tartaric acid, 2mL of glycerol, 0.05g of nicotinamide, 0.1g of hyaluronic acid, 0.1g of grape seed extract, 0.05g of rosemary extract and 1.2g of carbomer are mixed uniformly to obtain the antibacterial acne-removing cream of the invention by adopting diluted raspberry liquid to achieve the volume of pure exposure to 100 mL.
Example 4
The embodiment provides a formulation of several antibacterial acne-removing creams, which is specifically as follows:
the antibacterial acne-removing cream is prepared by uniformly mixing 0.5g of raspberry leaf extract, 1.5g of tartaric acid, 5mL of glycerol, 0.2g of nicotinamide, 0.4g of hyaluronic acid, 0.2g of grape seed extract, 0.2g of rosemary extract and 1.8g of carbomer with pure water to a volume of 100mL under the volume of 100 mL.
The antibacterial acne-removing cream is prepared by adopting the pot-covered cotyledon hydrosol to reach the volume of 100mL, mixing uniformly, and solidifying completely, wherein the volume of the pot-covered cotyledon hydrosol is 0.1g, the tartaric acid is 0.5g, the glycerin is 1mL, the nicotinamide is 0.1g, the hyaluronic acid is 0.2g, the grape seed extract is 0.3g, the rosemary extract is 0.1g, the carbomer is 1.2 g.
Under the volume of 100mL, 0.3g of raspberry leaf extract, 1g of tartaric acid, 3mL of glycerol, 0.5g of nicotinamide, 0.4g of hyaluronic acid, 0.4g of grape seed extract, 0.3g of rosemary extract and 1.5g of carbomer are adopted, the volume of the raspberry leaf hydrosol is fixed to 100mL, and the raspberry leaf hydrosol is uniformly mixed and completely coagulated to obtain the antibacterial acne-removing cream.
Claims (2)
1. An acne-removing cream for inhibiting propionibacterium acnes, which is characterized in that: the specific formula is as follows: 1-5 mg/mL of raspberry leaf extract, 5-10 mg/mL of tartaric acid, 1-5% of glycerin by volume, 1-5 mg/mL of nicotinamide, 2-4 mg/mL of hyaluronic acid, 2-4 mg/mL of grape seed extract, 1-3 mg/mL of rosemary extract, 12-18 mg/mL of carbomer and the balance of raspberry leaf truffle;
the preparation method of the raspberry leaf extract comprises the steps of drying and crushing raspberry leaves, mixing crushed raspberry leaves with tartaric acid, adding an ethanol solution with the volume fraction of 50-75%, carrying out ultrasonic auxiliary extraction for 10-120 min under the conditions of the temperature of 60-65 ℃ and the ultrasonic power of 150-250 w, filtering insoluble substances after the extraction is finished, concentrating, extracting and decoloring by using ethyl acetate, and extracting the extracted water phase by using n-butanol; finally, the n-butanol phase is rotationally evaporated to obtain a solid substance which is the raspberry leaf extract; the mass volume ratio of the crushed washbasin cotyledon to the ethanol water solution is 40-60 g/L, and the mass volume ratio of tartaric acid to the ethanol water solution is 2.667-4 g/L;
the preparation method of the raspberry leaf hydrolat comprises the steps of distilling pure water, tartaric acid and raspberry leaf powder, collecting water vapor, condensing distilled turbid liquid along with the hot vapor, standing in a receiving bottle, layering distilled liquid, wherein the upper layer is essential oil, and the lower layer is the raspberry leaf hydrolat.
2. An application of raspberry leaf extract in preparing acne-removing cream for inhibiting propionibacterium acnes, which is characterized in that: the preparation method of the raspberry leaf extract comprises the steps of drying and crushing raspberry leaves, mixing the crushed raspberry leaves with tartaric acid, adding an ethanol solution with the volume fraction of 50-75%, carrying out ultrasonic auxiliary extraction for 10-120 min at the temperature of 60-65 ℃ and the ultrasonic power of 150-250 w, filtering insoluble substances after extraction, concentrating, extracting and decoloring by using ethyl acetate, extracting an aqueous phase after extraction by using n-butanol, and finally carrying out rotary evaporation on the n-butanol phase to obtain a solid substance, wherein the solid substance is the raspberry leaf extract.
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