CN117695190B - Preparation method and application of oil-control acne-removing composition - Google Patents
Preparation method and application of oil-control acne-removing composition Download PDFInfo
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
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Abstract
A preparation method and application of an oil-control acne-removing composition belong to the technical field of cosmetics, and the method comprises the steps of preparing a mountain large leaf extract, preparing a sunflower pistil extract, preparing female Xijiang yellow croaker protein peptide, and compounding the mountain large leaf extract, the sunflower pistil extract, the female Xijiang yellow croaker protein peptide, the mother chrysanthemum extract, the centella asiatica extract, the tea extract, the white willow bark extract, the witch hazel extract and the like. The invention designs a special extraction method, prepares the mountain large leaf extract, the sunflower pistil extract and the female Xijiang yellow croaker protein peptide, has good acne-removing and anti-acne effects, cooperates with other plant extract components to perform combined action on the skin with acne, can remove acne and acne marks rapidly, has stable oil control and difficult recurrence, improves the nursing effect of cosmetics in the aspects of oil control and acne removal, can repair the skin to form a natural barrier, radically improves the skin state, and solves the problem of repeated acne attack.
Description
Technical Field
The invention belongs to the technical field of cosmetics, and particularly relates to a preparation method and application of an oil-control acne-removing composition.
Background
Acne, pimples and the like belong to acne, mainly exist on the face of a human body, are collectively called facial sores, and can be cured quickly or by means of medicines; however, inflammatory acne is difficult to heal or cure rapidly, such as infection of microorganisms such as staphylococcus, corynebacterium acnes, pityrosporum ovale or mites, red swelling and suppuration are caused, acne marks are generated after healing, and are difficult to eradicate rapidly, if continuous infection is carried out, acne is prone to occur, skin is provided with a plurality of induration, cysts, erythema, acne marks or scars, the skin is not healed for a long time, cells at the acne position are damaged and are poor in metabolism, pigments are deposited, the skin appears dark, the color value is seriously affected, and mental health is disturbed.
The main reasons for acne include bacterial infection (propionibacterium acnes, staphylococcus aureus and the like), cosmetic allergy, drug allergy, endocrine dyscrasia, excessive secretion of grease, pore blockage, inflammation and the like, various cosmetics with acne removing effects are developed on the market for beautifying the appearance of the face, and the traditional Chinese medicine components are utilized for bacteriostasis, anti-inflammation and acne removing, and grease secretion inhibition, acne generation prevention and acne removal, so that the acne removing product is mild and free of stimulation, but the existing acne removing product is various in variety, good in effect and uneven in effect, and the problems of long acne removing treatment course, unstable oil control effect, easiness in recurrence and poor acne mark recovery effect are generally existed. Therefore, there is a need for improved development of acne-removing products to achieve the effects of faster, more efficient and less recurrence.
Disclosure of Invention
Aims at solving the problems of long acne treatment course, unstable oil control effect, easy recurrence and poor recovery effect of acne marks and acne marks in the existing acne treatment products. The invention provides a preparation method and application of an oil-control acne-removing composition, and designs a special extraction method to prepare a mountain large leaf extract, a sunflower pistil extract and a female Xijiang yellow croaker protein peptide, so that the oil-control acne-removing composition has good acne-removing and anti-acne effects, and can be used for rapidly removing acnes and acne marks by combining a chamomile extract, a centella asiatica extract, a tea extract, a white willow bark extract and a witch hazel extract to act on skin with acnes caused by grease. The specific technical scheme is as follows:
a preparation method of an oil-control acne-removing composition comprises the following steps:
s1: according to the mass parts, 4 to 8 parts of mountain large leaf extract, 3 to 5 parts of sunflower pistil extract, 4 to 6 parts of female Xijiang yellow croaker protein peptide, 1 to 3 parts of chamomile extract, 3 to 5 parts of centella asiatica extract, 1 to 3 parts of tea extract, 0.5 to 2 parts of white willow bark extract, 0.5 to 2 parts of witch hazel extract and 10 to 30 parts of purified water are prepared;
s2: heating purified water to 55-60 ℃, adding the chamomile extract, the centella asiatica extract, the tea extract, the white willow bark extract and the witch hazel extract, uniformly mixing, cooling to 45-50 ℃, adding the mountain large leaf extract and the sunflower pistil extract, continuously uniformly mixing, cooling to 38-42 ℃, adding the female Xijiang yellow croaker protein peptide, and uniformly mixing to obtain the oil-control acne-removing composition.
In the technical scheme, the preparation method of the mountain large leaf extract comprises the following steps: crushing mountain flour Yan She, adding purified water with the mass of 8-10 times, mixing and soaking for 20-30 min at 90-95 ℃, cooling to 35-36 ℃, adding lactobacillus plantarum and subtilisin, fermenting and hydrolyzing for 20-24 h, keeping a water bath at 100 ℃ for 15-20 min, cooling to room temperature, obtaining fermentation enzymolysis liquid, adding absolute ethyl alcohol, stirring and mixing, filtering by adopting a 3kDa ultrafiltration membrane, collecting filtrate with the mass of less than 3kDa, concentrating, and freeze-drying to obtain mountain flour leaf extract.
In the technical scheme, the adding amount of the lactobacillus plantarum is 1-2% of the mass of the mountain large Yan She; the addition amount of the subtilisin is 0.5-1% of the mass of the mountain flour Yan She; the addition amount of the absolute ethyl alcohol is 5% -15% of the volume of the fermentation enzymolysis liquid; the stirring and mixing time is 10-20 min.
In the technical scheme, the preparation method of the sunflower pistil extract comprises the following steps: crushing sunflower pistil, adding 8-10 times of water, soaking at 90-95 ℃ for 20-30 min, filtering, collecting filtrate, concentrating to a concentrated solution with the relative density of 1.05-1.15; adding hemicellulase, beta-glucanase, papain and xylanase into the concentrated solution, carrying out enzymolysis for 1.5-2 hours at 48-52 ℃ and pH 4.5-pH 5.0, then keeping the mixture in a water bath at 100 ℃ for 15-20 minutes, and cooling to room temperature to obtain an enzymolysis solution; adsorbing the enzymolysis liquid with macroporous resin, eluting with ethanol water solution, collecting eluate, concentrating, and freeze drying to obtain sunflower pistil extract.
In the technical scheme, the addition amount of the hemicellulase, the beta-glucanase, the papain and the xylanase is 0.3-1% of the mass of the sunflower pistil; the macroporous resin is nonpolar resin or weak polar resin with pores of 300 nm-800 nm; the volume concentration of the ethanol water solution is 30-40%.
In the technical scheme, the preparation method of the female Xijiang yellow croaker protein peptide comprises the following steps:
n1: taking the skin of female Xijiang yellow croaker, washing with water, mincing, soaking in warm water at 40-45 ℃ for 30-40 min, immediately cooling, freezing to remove acid, taking out for thawing, washing with water again, filtering, and draining to obtain a raw material A;
n2: adding NaOH solution into the raw material A, soaking for 4-6 h, then washing with water until the pH value is neutral, centrifugally separating, collecting precipitate, and drying to obtain powder B;
and N3: suspending the powder B in 8-10 times of hydrochloric acid solution with the mass of pH of 2.0-2.5, adding pepsin, carrying out enzymolysis for 1-1.5 h in a water bath at 36-38 ℃, maintaining in the water bath at 100 ℃ for 15-20 min, cooling to room temperature, centrifuging, collecting supernatant, and carrying out vacuum freeze-drying to obtain a freeze-dried product C;
n4: suspending the freeze-dried product C in purified water with the mass of 8-10 times and the temperature of 36-38 ℃, adjusting the pH value to 7.6-8.2, adding trypsin, carrying out ultrasonic enzymolysis reaction for 1-1.5 h at 25-35 kHZ, keeping the temperature in a water bath at 100 ℃ for 15-20 min, cooling to room temperature, filtering by adopting a 1kDa ultrafiltration membrane to obtain ultrafiltrate smaller than 1kDa, and carrying out vacuum freeze-drying to obtain female Xijiang yellow croaker protein peptide.
In the N2 of the preparation method, the mass concentration of the NaOH solution is 1.5% -2.5%; the addition amount of NaOH solution is 7-8 times of the mass of the raw material A.
In the N3 of the preparation method, the addition amount of the pepsin is 1-2% of the mass of the powder B.
In the N4 prepared by the preparation method, the addition amount of the trypsin is 0.5-1.5% of the mass of the freeze-dried product C.
In the above technical scheme, the flos Matricariae Chamomillae extract, herba Centellae extract, folium Camelliae sinensis extract, salix alba bark extract and Hamamelis mollis extract are all water or alcohol solvent extracts.
The oil-control acne-removing composition obtained by the preparation method is mixed with cosmetic auxiliary agents for use, or is used independently for controlling oil and removing acne of facial skin; the cosmetic auxiliary agents include moisturizers, emulsifiers, preservatives, thickeners and penetration enhancers.
The preparation method and the application of the oil-control acne-removing composition have the beneficial effects that compared with the prior art, the oil-control acne-removing composition has the following advantages:
1. the invention adopts the mountain large leaf extract, the sunflower pistil extract, the female Xijiang yellow croaker protein peptide, the chamomile extract, the centella asiatica extract, the tea extract, the white willow bark extract and the witch hazel extract as main active ingredients for controlling oil and removing acnes and repairing skin, and the components are reasonably compatible for use, so that the quick and efficient oil control and acne removal can be realized, the recovery of acne mark skin is quick, the skin is mild and has no stimulation, the safety is high, the oil control and acne removal effects are stable, the recurrence is not easy, and the problem of repeated acne attack is solved.
2. The method designs the mountain large Yan Shejing-95 ℃ hot water soaking, then simultaneously ferments by lactobacillus plantarum and carries out enzymolysis by subtilisin to obtain a fermentation enzymolysis product with the molecular weight of less than 3kDa, has antibacterial effect on propionibacterium acnes, has the effects of detumescence and anti-inflammation, has a certain oil control effect, and has a good acne removal promoting effect.
3. According to the method, the sunflower pistil is subjected to enzymolysis by hemicellulase, beta-glucanase, papain and xylanase, and macroporous resin is adopted for adsorption to obtain an eluate, so that the eluate has antibacterial and anti-inflammatory effects, the acne removing effect can be greatly promoted by being matched with the folium isatidis extract, the antibacterial effect on Propionibacterium acnes can be remarkably improved by being matched with the folium isatidis extract and the sunflower pistil extract, the oil control effect is greatly improved, and the skin is not easily damaged by Propionibacterium acnes repeatedly.
4. According to the method disclosed by the invention, female Xijiang yellow croaker is designed, after acid removal and NaOH soaking, the fishskin components are subjected to enzymolysis by pepsin and trypsin step by step to obtain the small molecular peptide with the molecular peptide of less than 1kDa, so that the absorption speed is high, the skin is quickly repaired, the acne mark removing effect is excellent, the skin is enabled to recover the elasticity and the health state, the skin can quickly form a natural barrier of the skin, the resistance is improved, and the repeated attacks of acne are prevented.
5. The flos Matricariae Chamomillae extract has excellent oil control effect, has biological activities of resisting bacteria, resisting oxidation, resisting inflammation, relieving allergy, and preventing allergy, acne and aging.
6. Centella asiatica extract is a common component of cosmetics, has a promoting effect on the activity of scar fibroblast, has a good promoting effect on removing acne marks, and also has the effects of improving skin, whitening and resisting aging.
7. The tea extract has good oil control effect, has the functions of resisting bacteria, building skin and delaying skin aging, can remove various free radicals in the body, achieves the effect of resisting oxidation, and also has the effect of promoting elimination of pigmentation.
8. The white willow bark extract has good anti-inflammatory effect, has analgesic and repercussive effects, and is commonly used for treating acne, dermatitis and other symptoms.
9. Hamamelis mollis extract
The Hamamelis mollis extract has antiinflammatory, antioxidant, antiallergic, skin cell metabolism improving, antiaging, skin elasticity maintaining, and wrinkle resisting effects.
In summary, the invention designs a special extraction method to prepare the mountain large leaf extract, the sunflower pistil extract and the female Xijiang yellow croaker protein peptide, which has good acne-removing and anti-acne effects, and cooperates with the chamomile extract, the centella asiatica extract, the tea extract, the white willow bark extract and the witch hazel extract to perform the combined action on the skin with acne on grease, so that the acne and acne marks can be removed quickly, the oil is controlled stably, the relapse is not easy, the nursing effect of the cosmetics in the aspects of oil control and acne removal is improved, the skin can be repaired to form a natural barrier, the skin state is improved fundamentally, the problem of repeated acne attack is solved, and the invention has good practical value.
Detailed Description
The invention will be further illustrated with reference to specific examples, but the invention is not limited to these examples.
Example 1
A preparation method of an oil-control acne-removing composition comprises the following steps:
s1: preparing materials according to the parts by weight, including 6 parts of mountain large leaf extract, 4 parts of sunflower pistil extract, 5 parts of female Xijiang yellow croaker protein peptide, 2 parts of chamomile extract, 4 parts of centella asiatica extract, 2 parts of tea extract, 1 part of white willow bark extract, 1 part of witch hazel extract and 20 parts of purified water;
s2: heating purified water to 58 ℃, adding the chamomile extract, the centella asiatica extract, the tea extract, the white willow bark extract and the witch hazel extract, uniformly mixing, cooling to 46 ℃, adding the mountain large-leaf extract and the sunflower pistil extract, continuously uniformly mixing, cooling to 40 ℃, adding the female Xijiang yellow croaker protein peptide, and uniformly mixing to obtain the oil-control acne-removing composition.
The preparation method of the mountain large leaf extract comprises the following steps: crushing mountain flour Yan She, adding 9 times of purified water, mixing and soaking at 92 ℃ for 25min, cooling to 35 ℃, adding 1.5% of lactobacillus plantarum and 0.8% of subtilisin of mountain flour Yan She by mass of mountain flour Yan She, fermenting and hydrolyzing for 22h, maintaining in a water bath at 100 ℃ for 18min, cooling to room temperature to obtain fermentation enzymolysis liquid, adding 10% absolute ethyl alcohol of the volume of the fermentation enzymolysis liquid, stirring and mixing for 15min, filtering by a 3kDa ultrafiltration membrane, collecting filtrate below 3kDa, concentrating, and freeze-drying to obtain mountain flour leaf extract.
The preparation method of the sunflower pistil extract comprises the following steps: pulverizing sunflower pistil, adding 9 times of water, soaking at 92 deg.C for 25min, filtering, collecting filtrate, and concentrating to obtain concentrated solution with relative density of 1.12; adding hemicellulase, beta-glucanase, papain and xylanase into the concentrated solution, wherein the addition amount of each enzyme is 0.8% of the mass of the sunflower pistil, carrying out enzymolysis for 1.5h at 50 ℃ and pH4.8, keeping the mixture in a water bath at 100 ℃ for 18min, and cooling to room temperature to obtain an enzymolysis solution; adsorbing the enzymolysis liquid by using nonpolar macroporous resin with 300-800 nm pores, eluting by using ethanol water solution with the volume concentration of 35%, collecting eluent, concentrating, and freeze-drying to obtain the sunflower pistil extract.
The preparation method of the female Xijiang yellow croaker protein peptide comprises the following steps:
n1: taking the skin of female Xijiang yellow croaker, washing with water, mincing, soaking in warm water at 42 ℃ for 35min, immediately cooling, freezing to remove acid, taking out, thawing, washing with water again, filtering, and draining to obtain a raw material A;
n2: adding NaOH solution with the mass of 7.5 times that of the raw material A, soaking for 5 hours, washing with water until the pH value is neutral, centrifugally separating, collecting precipitate, and drying to obtain powder B;
and N3: suspending powder B in hydrochloric acid solution with the weight being 9 times of that of the hydrochloric acid solution and the pH value being 2.2, adding pepsin with the weight being 1.5 percent of that of the powder B, carrying out enzymolysis for 1.5 hours in a 37 ℃ water bath, keeping the temperature in a 100 ℃ water bath for 18 minutes, cooling to room temperature, centrifuging, collecting supernatant, and carrying out vacuum freeze-drying to obtain a freeze-dried product C;
n4: suspending the freeze-dried product C in purified water with the mass of 9 times of 37 ℃, adjusting the pH value to 8.0, adding trypsin with the mass of 1% of the freeze-dried product C, carrying out ultrasonic enzymolysis reaction for 1h at 30kHZ, keeping the temperature in a water bath at 100 ℃ for 18min, cooling to room temperature, filtering by adopting a 1kDa ultrafiltration membrane to obtain ultrafiltrate smaller than 1kDa, and carrying out vacuum freeze-drying to obtain female Xijiang yellow croaker protein peptide.
Wherein the flos Matricariae Chamomillae extract, herba Centellae extract, folium Camelliae sinensis extract, cortex Salicis Babylonicae extract and radix Hamamelis mollis extract are all water or alcohol solvent extracts.
The oil-control acne-removing composition obtained by the preparation method is mixed with cosmetic auxiliary agents for use, or is used independently for controlling oil and removing acne of facial skin; the cosmetic auxiliary agents include moisturizers, emulsifiers, preservatives, thickeners and penetration enhancers.
Example 2
A preparation method of an oil-control acne-removing composition comprises the following steps:
s1: preparing materials by mass parts, namely 4 parts of mountain large leaf extract, 3 parts of sunflower pistil extract, 4 parts of female Xijiang yellow croaker protein peptide, 1 part of mother chrysanthemum extract, 3 parts of centella asiatica extract, 1 part of tea extract, 0.5 part of white willow bark extract, 0.5 part of witch hazel extract and 10 parts of purified water;
s2: heating purified water to 55deg.C, adding flos Matricariae Chamomillae extract, herba Centellae extract, folium Camelliae sinensis extract, cortex Salicis Babylonicae extract and radix Hamamelis mollis extract, mixing, cooling to 45deg.C, adding folium Pimentae Indicae extract and sunflower pistil extract, mixing, cooling to 38deg.C, adding female Xijiang yellow bone fish protein peptide, and mixing to obtain oil-controlling acne-removing composition.
The preparation method of the mountain large leaf extract comprises the following steps: pulverizing semen Ardisiae Crispae Yan She, adding 8 times of purified water, mixing at 90deg.C, soaking for 20min, cooling to 35deg.C, adding Lactobacillus plantarum of 1% by mass of semen Ardisiae Crispae and subtilisin of 0.5% by mass of semen Ardisiae Crispae Yan She, fermenting and hydrolyzing for 20h, maintaining in water bath at 100deg.C for 15min, cooling to room temperature to obtain fermented enzymolysis solution, adding 5% absolute ethanol by volume of the fermented enzymolysis solution, stirring and mixing for 10min, filtering with 3kDa ultrafiltration membrane, collecting filtrate below 3kDa, concentrating, and lyophilizing to obtain folium Ardisiae Crispae extract.
The preparation method of the sunflower pistil extract comprises the following steps: pulverizing sunflower pistil, adding 8 times of water, soaking at 90deg.C for 20min, filtering, collecting filtrate, and concentrating to obtain concentrated solution with relative density of 1.05; adding hemicellulase, beta-glucanase, papain and xylanase into the concentrated solution, wherein the addition amount of each enzyme is 0.3% of the mass of sunflower pistil, carrying out enzymolysis for 1.5h at 48 ℃ and pH4.5, keeping the solution in a water bath at 100 ℃ for 15min, and cooling to room temperature to obtain an enzymolysis solution; absorbing the enzymolysis liquid by using weak polar macroporous resin with 300-800 nm pores, eluting by using ethanol water solution with volume concentration of 30%, collecting eluent, concentrating, and freeze-drying to obtain the sunflower pistil extract.
The preparation method of the female Xijiang yellow croaker protein peptide comprises the following steps:
n1: taking the skin of female Xijiang yellow croaker, washing with water, mincing, soaking in warm water at 40 ℃ for 30min, immediately cooling, freezing to remove acid, taking out, thawing, washing with water again, filtering, and draining to obtain a raw material A;
n2: adding NaOH solution with the mass of 7 times into the raw material A, wherein the mass concentration of the NaOH solution is 1.5%, soaking for 4 hours, then washing with water until the pH value is neutral, centrifugally separating, collecting precipitate, and drying to obtain powder B;
and N3: suspending powder B in 8 times of hydrochloric acid solution with pH of 2.0, adding pepsin with 1% of powder B, performing enzymolysis in water bath at 36 deg.C for 1 hr, maintaining in water bath at 100 deg.C for 15min, cooling to room temperature, centrifuging, collecting supernatant, and vacuum lyophilizing to obtain lyophilized product C;
n4: suspending the freeze-dried product C in purified water with the mass of 8 times of 36 ℃, adjusting pH7.6, adding trypsin with the mass of 0.5% of the freeze-dried product C, carrying out ultrasonic enzymolysis reaction for 1h at 25kHZ, maintaining in a water bath at 100 ℃ for 15min, cooling to room temperature, filtering by adopting a 1kDa ultrafiltration membrane to obtain ultrafiltrate smaller than 1kDa, and carrying out vacuum freeze-drying to obtain female Xijiang yellow croaker protein peptide.
Wherein the flos Matricariae Chamomillae extract, herba Centellae extract, folium Camelliae sinensis extract, cortex Salicis Babylonicae extract and radix Hamamelis mollis extract are all water or alcohol solvent extracts.
The oil-control acne-removing composition obtained by the preparation method is mixed with cosmetic auxiliary agents for use, or is used independently for controlling oil and removing acne of facial skin; the cosmetic auxiliary agents include moisturizers, emulsifiers, preservatives, thickeners and penetration enhancers.
Example 3
A preparation method of an oil-control acne-removing composition comprises the following steps:
s1: preparing materials according to the mass parts, namely 8 parts of mountain large leaf extract, 5 parts of sunflower pistil extract, 6 parts of female Xijiang yellow croaker protein peptide, 3 parts of chamomile extract, 5 parts of centella asiatica extract, 3 parts of tea extract, 2 parts of white willow bark extract, 2 parts of witch hazel extract and 30 parts of purified water;
s2: heating purified water to 60 ℃, adding the chamomile extract, the centella asiatica extract, the tea extract, the white willow bark extract and the witch hazel extract, uniformly mixing, cooling to 50 ℃, adding the mountain large-leaf extract and the sunflower pistil extract, continuously uniformly mixing, cooling to 42 ℃, adding the female Xijiang yellow croaker protein peptide, and uniformly mixing to obtain the oil-control acne-removing composition.
The preparation method of the mountain large leaf extract comprises the following steps: crushing mountain flour Yan She, adding purified water with the mass being 10 times, mixing and soaking for 30min at 95 ℃, cooling to 36 ℃, adding lactobacillus plantarum with the mass being 2% of mountain flour Yan She and subtilisin with the mass being 1% of mountain flour Yan She, fermenting and hydrolyzing for 24h, keeping in a water bath with the temperature being 100 ℃ for 20min, cooling to room temperature, obtaining fermentation enzymolysis liquid, adding absolute ethyl alcohol with the volume being 15% of the fermentation enzymolysis liquid, stirring and mixing for 20min, filtering by adopting a 3kDa ultrafiltration membrane, taking filtrate with the mass being less than 3kDa, concentrating and freeze-drying to obtain the mountain flour extract.
The preparation method of the sunflower pistil extract comprises the following steps: pulverizing sunflower pistil, adding 10 times of water, soaking at 95deg.C for 30min, filtering, collecting filtrate, and concentrating to obtain concentrated solution with relative density of 1.15; adding hemicellulase, beta-glucanase, papain and xylanase into the concentrated solution, wherein the addition amount of each enzyme is 1% of the mass of the sunflower pistil, carrying out enzymolysis for 2 hours at 52 ℃ and pH5.0, keeping a water bath at 100 ℃ for 20 minutes, and cooling to room temperature to obtain an enzymolysis solution; adsorbing the enzymolysis liquid by using nonpolar macroporous resin with 300-800 nm pores, eluting by using ethanol water solution with volume concentration of 40%, collecting eluent, concentrating, and freeze-drying to obtain sunflower pistil extract.
The preparation method of the female Xijiang yellow croaker protein peptide comprises the following steps:
n1: taking the skin of female Xijiang yellow croaker, washing with water, mincing, soaking in 45 ℃ warm water for 40min, immediately cooling, freezing to remove acid, taking out, thawing, washing with water again, filtering, and draining to obtain a raw material A;
n2: adding NaOH solution with the mass of 8 times into the raw material A, wherein the mass concentration of the NaOH solution is 2.5%, soaking for 6 hours, then washing with water until the pH value is neutral, centrifugally separating, collecting precipitate, and drying to obtain powder B;
and N3: suspending powder B in hydrochloric acid solution with the mass of 10 times and the pH of 2.5, adding pepsin with the mass of 2% of the powder B, carrying out enzymolysis for 1.5h in a water bath at 38 ℃, maintaining in the water bath at 100 ℃ for 20min, cooling to room temperature, centrifuging, collecting supernatant, and carrying out vacuum freeze-drying to obtain a freeze-dried product C;
n4: suspending the freeze-dried product C in purified water with the mass of 10 times and the temperature of 38 ℃, adjusting the pH value to 8.2, adding trypsin with the mass of 1.5 percent of the freeze-dried product C, carrying out ultrasonic enzymolysis reaction for 1.5 hours at 35kHZ, keeping the temperature in a water bath at 100 ℃ for 20 minutes, cooling to room temperature, filtering by adopting a 1kDa ultrafiltration membrane to obtain ultrafiltrate smaller than 1kDa, and carrying out vacuum freeze-drying to obtain female Xijiang yellow croaker protein peptide.
Wherein the flos Matricariae Chamomillae extract, herba Centellae extract, folium Camelliae sinensis extract, cortex Salicis Babylonicae extract and radix Hamamelis mollis extract are all water or alcohol solvent extracts.
The oil-control acne-removing composition obtained by the preparation method is mixed with cosmetic auxiliary agents for use, or is used independently for controlling oil and removing acne of facial skin; the cosmetic auxiliary agents include moisturizers, emulsifiers, preservatives, thickeners and penetration enhancers.
Example 4
A preparation method of an oil-control acne-removing composition comprises the following steps:
s1: preparing materials by mass parts of a mountain large leaf extract, 3.5 parts of a sunflower pistil extract, 4.5 parts of female Xijiang yellow croaker protein peptide, 1.5 parts of a chamomile flower extract, 3.5 parts of a centella asiatica extract, 1.5 parts of a tea leaf extract, 0.8 part of a white willow bark extract, 0.8 part of a witch hazel extract and 15 parts of purified water;
s2: heating purified water to 56 ℃, adding the chamomile extract, the centella asiatica extract, the tea extract, the white willow bark extract and the witch hazel extract, uniformly mixing, cooling to 46 ℃, adding the mountain large-leaf extract and the sunflower pistil extract, continuously uniformly mixing, cooling to 39 ℃, adding the female Xijiang yellow croaker protein peptide, and uniformly mixing to obtain the oil-control acne-removing composition.
The preparation method of the mountain large leaf extract comprises the following steps: crushing mountain flour Yan She, adding purified water with the mass being 8.5 times, mixing and soaking for 22min at 91 ℃, cooling to 35 ℃, adding lactobacillus plantarum with the mass being 1.2% of mountain flour Yan She and subtilisin with the mass being 0.6% of mountain flour Yan She, carrying out fermentation and enzymolysis for 21h, keeping a water bath at 100 ℃ for 16min, cooling to room temperature, obtaining fermentation enzymolysis liquid, adding absolute ethanol with the volume being 7% of the fermentation enzymolysis liquid, stirring and mixing for 12min, filtering by adopting a 3kDa ultrafiltration membrane, taking filtrate with the mass being less than 3kDa, concentrating and freeze-drying to obtain the mountain flour leaf extract.
The preparation method of the sunflower pistil extract comprises the following steps: pulverizing sunflower pistil, adding 8.5 times of water, soaking at 91 deg.C for 22min, filtering, collecting filtrate, and concentrating to obtain concentrated solution with relative density of 1.08; adding hemicellulase, beta-glucanase, papain and xylanase into the concentrated solution, wherein the addition amount of each enzyme is 0.4% of the mass of the sunflower pistil, carrying out enzymolysis for 1.5h at 49 ℃ and pH4.6, keeping the mixture in a water bath at 100 ℃ for 16min, and cooling to room temperature to obtain an enzymolysis solution; adsorbing the enzymolysis liquid by using nonpolar macroporous resin with 300-800 nm pores, eluting by using ethanol water solution with the volume concentration of 32%, collecting eluent, concentrating, and freeze-drying to obtain the sunflower pistil extract.
The preparation method of the female Xijiang yellow croaker protein peptide comprises the following steps:
n1: taking the skin of female Xijiang yellow croaker, washing with water, mincing, soaking in warm water at 41 ℃ for 32min, immediately cooling, freezing to remove acid, taking out, thawing, washing with water again, filtering, and draining to obtain a raw material A;
n2: adding NaOH solution with the mass of 7.2 times that of the raw material A, wherein the mass concentration of the NaOH solution is 1.8%, soaking for 4.5 hours, then washing with water until the pH value is neutral, centrifugally separating, collecting precipitate, and drying to obtain powder B;
and N3: suspending powder B in hydrochloric acid solution with the mass of 8.5 times and the pH of 2.1, adding pepsin with the mass of 1.2% of the powder B, carrying out enzymolysis for 1.5h in a 36 ℃ water bath, maintaining in a 100 ℃ water bath for 16min, cooling to room temperature, centrifuging, collecting supernatant, and carrying out vacuum freeze-drying to obtain a freeze-dried product C;
n4: suspending the freeze-dried product C in purified water with the mass of 8.5 times of 36 ℃, adjusting pH7.8, adding trypsin with the mass of 0.6% of the freeze-dried product C, carrying out ultrasonic enzymolysis reaction for 1.5h at 28kHZ, keeping in a water bath at 100 ℃ for 16min, cooling to room temperature, filtering by adopting a 1kDa ultrafiltration membrane to obtain ultrafiltrate smaller than 1kDa, and carrying out vacuum freeze-drying to obtain female Xijiang yellow croaker protein peptide.
Wherein the flos Matricariae Chamomillae extract, herba Centellae extract, folium Camelliae sinensis extract, cortex Salicis Babylonicae extract and radix Hamamelis mollis extract are all water or alcohol solvent extracts.
The oil-control acne-removing composition obtained by the preparation method is mixed with cosmetic auxiliary agents for use, or is used independently for controlling oil and removing acne of facial skin; the cosmetic auxiliary agents include moisturizers, emulsifiers, preservatives, thickeners and penetration enhancers.
Example 5
A preparation method of an oil-control acne-removing composition comprises the following steps:
s1: preparing 7 parts of mountain large leaf extract, 4.5 parts of sunflower pistil extract, 5.5 parts of female Xijiang yellow croaker protein peptide, 2.5 parts of chamomile extract, 4.5 parts of centella asiatica extract, 2.5 parts of tea extract, 1.5 parts of white willow bark extract, 1.5 parts of witch hazel extract and 25 parts of purified water according to parts by mass;
s2: heating purified water to 58 ℃, adding the chamomile extract, the centella asiatica extract, the tea extract, the white willow bark extract and the witch hazel extract, uniformly mixing, cooling to 48 ℃, adding the mountain large-leaf extract and the sunflower pistil extract, continuously uniformly mixing, cooling to 41 ℃, adding the female Xijiang yellow croaker protein peptide, and uniformly mixing to obtain the oil-control acne-removing composition.
The preparation method of the mountain large leaf extract comprises the following steps: crushing mountain flour Yan She, adding 9.5 times of purified water, mixing and soaking at 93 ℃ for 28min, cooling to 36 ℃, adding lactobacillus plantarum with the mass of 1.8% of mountain flour Yan She and subtilisin with the mass of 0.8% of mountain flour Yan She, fermenting and hydrolyzing for 23h, keeping in a water bath at 100 ℃ for 18min, cooling to room temperature to obtain fermentation enzymolysis liquid, adding absolute ethanol with the volume of 12% of the fermentation enzymolysis liquid, stirring and mixing for 18min, filtering by a 3kDa ultrafiltration membrane, collecting filtrate with the mass of less than 3kDa, concentrating, and freeze-drying to obtain the mountain flour leaf extract.
The preparation method of the sunflower pistil extract comprises the following steps: pulverizing sunflower pistil, adding 9.5 times of water, soaking at 93 deg.C for 28min, filtering, collecting filtrate, and concentrating to obtain concentrated solution with relative density of 1.13; adding hemicellulase, beta-glucanase, papain and xylanase into the concentrated solution, wherein the addition amount of each enzyme is 0.8% of the mass of the sunflower pistil, carrying out enzymolysis for 2 hours at the temperature of 51 ℃ and the pH value of 4.8, keeping the mixture in a water bath at the temperature of 100 ℃ for 18 minutes, and cooling to the room temperature to obtain an enzymolysis solution; absorbing the enzymolysis liquid by using weak polar macroporous resin with 300-800 nm pores, eluting by using ethanol water solution with volume concentration of 38%, collecting eluent, concentrating, and freeze-drying to obtain the sunflower pistil extract.
The preparation method of the female Xijiang yellow croaker protein peptide comprises the following steps:
n1: taking the skin of female Xijiang yellow croaker, washing with water, mincing, soaking in warm water at 44 ℃ for 38min, immediately cooling, freezing to remove acid, taking out, thawing, washing with water again, filtering, and draining to obtain a raw material A;
n2: adding NaOH solution with the mass of 7.8 times that of the raw material A, wherein the mass concentration of the NaOH solution is 2.2%, soaking for 5.5 hours, then washing with water until the pH value is neutral, centrifugally separating, collecting precipitate, and drying to obtain powder B;
and N3: suspending powder B in hydrochloric acid solution with the mass of 9.5 times and the pH of 2.4, adding pepsin with the mass of 1.8% of the powder B, carrying out enzymolysis for 1.5h in a 37 ℃ water bath, maintaining in a 100 ℃ water bath for 18min, cooling to room temperature, centrifuging, collecting supernatant, and carrying out vacuum freeze-drying to obtain a freeze-dried product C;
n4: suspending the freeze-dried product C in purified water with the mass of 9.5 times of 37 ℃, adjusting the pH value to 8.1, adding trypsin with the mass of 1.4% of the freeze-dried product C, performing ultrasonic enzymolysis for 1.5 hours at the temperature of 100 ℃, maintaining the temperature in a water bath for 18 minutes, cooling to room temperature, filtering by adopting a 1kDa ultrafiltration membrane to obtain ultrafiltrate smaller than 1kDa, and performing vacuum freeze-drying to obtain female Xijiang yellow croaker protein peptide.
Wherein the flos Matricariae Chamomillae extract, herba Centellae extract, folium Camelliae sinensis extract, cortex Salicis Babylonicae extract and radix Hamamelis mollis extract are all water or alcohol solvent extracts.
The oil-control acne-removing composition obtained by the preparation method is mixed with cosmetic auxiliary agents for use, or is used independently for controlling oil and removing acne of facial skin; the cosmetic auxiliary agents include moisturizers, emulsifiers, preservatives, thickeners and penetration enhancers.
Preparation of comparative example 1
The oil control and acne removal composition was free of mountain leaf extract, and the other parameters were the same as in example 1.
Preparation of comparative example 2
The oil control and acne removal composition was not added with the extract of sunflower stamen, and the other parameters were the same as in example 1.
Preparation of comparative example 3
The oil control and acne removal composition was free of mountain leaves extract and Japanese sunflower core extract, and the other parameters were the same as in example 1.
Preparation of comparative example 4
The oil control and acne removal composition was free of female Xijiang yellow croaker protein peptide, and the other parameters were the same as in example 1.
The oil control and acne removal compositions of examples 1 to 5, and the oil control and acne removal compositions of comparative examples 1 to 4 were each prepared by adding 0.5% by mass of a hexanediol preservative, 1.5% by mass of a carbomer thickener, 1.2% by mass of a tween 80 emulsifier, 6% by mass of a sodium hyaluronate humectant, and 0.8% by mass of a tetrahydropiperine penetration enhancer to cosmetic samples, and performing the test.
1. Safety experiment
According to the cosmetic safety test method, each cosmetic sample is subjected to an animal skin irritation test, a skin sensitization test and an in-vitro cytotoxicity test respectively, and the results are all safe and nontoxic.
2. In vitro bacteriostasis experiment
Propionibacterium acnes was subjected to bacteriostasis test, propionibacterium acnes suspension was uniformly smeared on the surface of a culture medium, a cosmetic sample was added to the center of the culture medium, and cultured in an incubator at 37 ℃ for 2 days, 3 parallel samples were prepared, and the average diameter of the zone of bacteriostasis was measured, and the results are shown in table 1 below:
TABLE 1 antibacterial test results of Propionibacterium acnes
| Cosmetic sample | Average inhibition zone diameter (mm) |
| Example 1 | 22.32 |
| Example 2 | 22.22 |
| Example 3 | 22.18 |
| Example 4 | 22.25 |
| Example 5 | 22.30 |
| Comparative example 1 | 20.23 |
| Comparative example 2 | 20.35 |
| Comparative example 3 | 18.36 |
| Comparative example 4 | 19.96 |
From the above results, the antibacterial effect of the samples of examples 1 to 5 on propionibacterium acnes is very remarkable, wherein according to the comparative example results, both the mountain large leaf extract and the sun sunflower core extract have a certain antibacterial effect on propionibacterium acnes, and the combination of the mountain large leaf extract and the sun sunflower core extract can remarkably improve the antibacterial effect; in addition, female Xijiang yellow croaker protein peptide has good antibacterial effect on Propionibacterium acnes.
3. Acne removal effect experiment
90 oily skin volunteers (20 years to 26 years, the course of the disease is 1 year to 2 years) with repeated acne, pimple on the face were selected, and divided into 9 groups of 10 persons each, each group being respectively applied with the cosmetic samples of examples 1 to 5 and comparative examples 1 to 4, and each face being applied once daily after cleansing the face in the morning and evening, and the following detection results were shown in table 2 below:
TABLE 2 acne removal test results
| Cosmetic testing Sample | 15-day grease Percent decrease% | Under 30 days of grease Percent of decrease | Counting the number of days of eliminating acnes of each acnes, calculate the average number of days (days) for acne removal | Counting the elimination of each acne mark after acne removal Day, calculate average day of elimination (day) | Continuously smearing and continuously observing for 6 months How many (10 people total) of internal recrudescence |
| Example 1 | 50.03% | 63.23% | 7 | 14 | 0 |
| Example 2 | 50.06% | 63.16% | 8 | 16 | 1 |
| Example 3 | 50.02% | 63.20% | 7 | 15 | 2 |
| Example 4 | 50.10% | 63.25% | 7 | 15 | 1 |
| Example 5 | 50.08% | 63.12% | 6 | 14 | 3 |
| Comparative example 1 | 44.23% | 51.32% | 10 | 20 | 6 |
| Comparative example 2 | 46.35% | 58.23% | 11 | 19 | 5 |
| Comparative example 3 | 40.03% | 48.65% | 15 | 23 | 7 |
| Comparative example 4 | 49.98% | 63.08% | 9 | 16 | 17 |
From the above results, the cosmetics of examples 1 to 6 have a very high acne removing speed, i.e. acne marks, and have a very good oil control effect, and are not easy to recur, and the occurrence of acne, pimples or pimples is basically eradicated. From the comparative example, the mountain large leaf extract and the sunflower pistil extract have good promotion effect on acne removal, the female Sijiang yellow croaker protein peptide has good effect on skin repair, the acne mark is quickly recovered, the skin can be repaired to form a natural barrier, the skin is not easy to be infected by bacteria and inflammation, the skin state is fundamentally improved, and the acne is not easy to relapse.
Claims (7)
1. The preparation method of the oil-control acne-removing composition is characterized by comprising the following steps of:
s1: according to the mass parts, 4 to 8 parts of mountain large leaf extract, 3 to 5 parts of sunflower pistil extract, 4 to 6 parts of female Xijiang yellow croaker protein peptide, 1 to 3 parts of chamomile extract, 3 to 5 parts of centella asiatica extract, 1 to 3 parts of tea extract, 0.5 to 2 parts of white willow bark extract, 0.5 to 2 parts of witch hazel extract and 10 to 30 parts of purified water are prepared;
s2: heating purified water to 55-60 ℃, adding the chamomile extract, the centella asiatica extract, the tea extract, the white willow bark extract and the witch hazel extract, uniformly mixing, cooling to 45-50 ℃, adding the mountain large leaf extract and the sunflower pistil extract, continuously uniformly mixing, cooling to 38-42 ℃, adding the female Xijiang yellow croaker protein peptide, and uniformly mixing to obtain the oil-control acne-removing composition;
the preparation method of the mountain large leaf extract comprises the following steps: crushing mountain flour Yan She, adding purified water with the mass of 8-10 times, mixing and soaking for 20-30 min at 90-95 ℃, cooling to 35-36 ℃, adding lactobacillus plantarum and subtilisin, fermenting and hydrolyzing for 20-24 h, keeping a water bath at 100 ℃ for 15-20 min, cooling to room temperature to obtain a fermentation enzymolysis liquid, adding absolute ethyl alcohol, stirring and mixing, filtering by adopting a 3kDa ultrafiltration membrane, collecting filtrate with the mass of less than 3kDa, concentrating, and freeze-drying to obtain mountain flour leaf extract;
the preparation method of the sunflower pistil extract comprises the following steps: crushing sunflower pistil, adding 8-10 times of water, soaking at 90-95 ℃ for 20-30 min, filtering, collecting filtrate, concentrating to a concentrated solution with the relative density of 1.05-1.15; adding hemicellulase, beta-glucanase, papain and xylanase into the concentrated solution, carrying out enzymolysis for 1.5-2 hours at 48-52 ℃ and pH 4.5-pH 5.0, then keeping the mixture in a water bath at 100 ℃ for 15-20 minutes, and cooling to room temperature to obtain an enzymolysis solution; adsorbing the enzymolysis liquid by macroporous resin, eluting by ethanol water solution, collecting eluent, concentrating, and freeze drying to obtain sunflower pistil extract;
the preparation method of the female Xijiang yellow croaker protein peptide comprises the following steps: n1: taking the skin of female Xijiang yellow croaker, washing with water, mincing, soaking in warm water at 40-45 ℃ for 30-40 min, immediately cooling, freezing to remove acid, taking out for thawing, washing with water again, filtering, and draining to obtain a raw material A;
n2: adding NaOH solution into the raw material A, soaking for 4-6 h, then washing with water until the pH value is neutral, centrifugally separating, collecting precipitate, and drying to obtain powder B;
and N3: suspending the powder B in 8-10 times of hydrochloric acid solution with the mass of pH of 2.0-2.5, adding pepsin, carrying out enzymolysis for 1-1.5 h in a water bath at 36-38 ℃, maintaining in the water bath at 100 ℃ for 15-20 min, cooling to room temperature, centrifuging, collecting supernatant, and carrying out vacuum freeze-drying to obtain a freeze-dried product C;
n4: suspending the freeze-dried product C in purified water with the mass of 8-10 times and the temperature of 36-38 ℃, adjusting the pH value to 7.6-8.2, adding trypsin, carrying out ultrasonic enzymolysis reaction for 1-1.5 h at 25-35 kHZ, keeping the temperature in a water bath at 100 ℃ for 15-20 min, cooling to room temperature, filtering by adopting a 1kDa ultrafiltration membrane to obtain ultrafiltrate smaller than 1kDa, and carrying out vacuum freeze-drying to obtain female Xijiang yellow croaker protein peptide.
2. The preparation method of the oil-control acne-removing composition according to claim 1, wherein the addition amount of the lactobacillus plantarum is 1-2% of the mass of the mountain flour Yan She; the addition amount of the subtilisin is 0.5-1% of the mass of the mountain flour Yan She; the addition amount of the absolute ethyl alcohol is 5% -15% of the volume of the fermentation enzymolysis liquid; the stirring and mixing time is 10-20 min.
3. The preparation method of the oil-control acne-removing composition according to claim 1, wherein the addition amount of the hemicellulase, the beta-glucanase, the papain and the xylanase is 0.3-1% of the mass of the sunflower pistil; the macroporous resin is nonpolar resin or weak polar resin with pores of 300 nm-800 nm; the volume concentration of the ethanol water solution is 30-40%.
4. The preparation method of the oil-control acne-removing composition according to claim 1, wherein the mass concentration of the NaOH solution in N2 is 1.5% -2.5%; the addition amount of NaOH solution is 7-8 times of the mass of the raw material A.
5. The preparation method of the oil-control acne-removing composition according to claim 1, wherein the adding amount of pepsin in N3 is 1-2% of the mass of the powder B.
6. The preparation method of the oil-control acne-removing composition according to claim 1, wherein the adding amount of trypsin in N4 is 0.5-1.5% of the mass of the freeze-dried product C.
7. An oil-control acne-removing composition prepared by the preparation method of the oil-control acne-removing composition according to any one of claims 1-6, wherein the oil-control acne-removing composition is mixed with cosmetic auxiliary agents or used independently for controlling oil and removing acne of facial skin; the cosmetic auxiliary agents include moisturizers, emulsifiers, preservatives, thickeners and penetration enhancers.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20120021881A (en) * | 2010-08-20 | 2012-03-09 | 곽한무 | A method of an emulsifier by a sunflower |
| CN105832940A (en) * | 2016-05-12 | 2016-08-10 | 张玉兰 | Medicine for treating acne and acne pits and preparing method thereof |
| CN111905597A (en) * | 2020-08-04 | 2020-11-10 | 林小红 | Acne-removing, anti-wrinkle and whitening mask rich in marine extract |
| CN113384642A (en) * | 2021-07-15 | 2021-09-14 | 忧立舒医药科技(广东)有限公司 | Natural extraction compound with acne removing effect and preparation method and application thereof |
| CN116270367A (en) * | 2023-05-12 | 2023-06-23 | 广州俏姿颜化妆品有限公司 | Face-cleaning acne-removing essence and preparation method thereof |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20120021881A (en) * | 2010-08-20 | 2012-03-09 | 곽한무 | A method of an emulsifier by a sunflower |
| CN105832940A (en) * | 2016-05-12 | 2016-08-10 | 张玉兰 | Medicine for treating acne and acne pits and preparing method thereof |
| CN111905597A (en) * | 2020-08-04 | 2020-11-10 | 林小红 | Acne-removing, anti-wrinkle and whitening mask rich in marine extract |
| CN113384642A (en) * | 2021-07-15 | 2021-09-14 | 忧立舒医药科技(广东)有限公司 | Natural extraction compound with acne removing effect and preparation method and application thereof |
| CN116270367A (en) * | 2023-05-12 | 2023-06-23 | 广州俏姿颜化妆品有限公司 | Face-cleaning acne-removing essence and preparation method thereof |
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