CN116270392B - Composition with moisturizing effect and application thereof - Google Patents
Composition with moisturizing effect and application thereof Download PDFInfo
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Abstract
The invention relates to the technical field of cosmetics, in particular to a composition with a moisturizing effect and application thereof. The composition with the moisturizing effect consists of the following substances: plant extract, composite hydrolyzed collagen and water. The composite hydrolyzed collagen prepared by the invention can be effectively absorbed by human skin, has very good moisture absorption and retention properties and relatively good antioxidant activity, can penetrate the skin more slowly, can supplement skin moisture better, maintain skin elasticity and repair skin barriers, and is particularly suitable for being used in various cosmetics. The composition with the moisturizing effect prepared by the invention has good moisturizing effect and antioxidation effect, and can be effectively applied to moisturizing cosmetics.
Description
Technical Field
The invention relates to the technical field of cosmetics, in particular to a composition with a moisturizing effect and application thereof.
Background
In recent years, skin moisturization has become one of the important concerns for cosmetic skin care. Moisturizers are a class of compounds that increase the moisture content of the skin and improve the dryness of the skin. Many people face skin dryness problems, whether caused by weather, environmental factors, or personal factors. Therefore, research and development of a composition with moisturizing effect is of great significance. Studies have shown that moisturizers are very important for maintaining skin health and aesthetics. Dry skin is prone to desquamation, roughness, wrinkles, etc., and in severe cases may cause inflammation and itching. Thus, by increasing the moisture content and retaining moisture in the skin, these problems can be ameliorated, making the skin smoother, softer and more elastic.
First, moisturizers are an important functional ingredient for the cosmetic and skin care industries. Consumer demand for moisturizing products continues to increase, allowing various moisturizers and formulations to appear on the market. Accordingly, researchers are continually striving to find new moisturizers and compositions that meet consumer needs. Second, the skin is a complex biological barrier that prevents the ingress of external harmful substances and prevents the loss of moisture. However, the skin barrier function may be impaired due to the influence of several internal and external factors, resulting in loss of moisture. Therefore, by studying moisturizers and their mechanism of action, effective methods can be found to improve the moisturization function of the skin, strengthen the skin barrier, and thereby reduce water loss and dryness problems.
In studying moisturizing compositions, researchers often choose to combine multiple ingredients to achieve better moisturizing results. For example, certain moisturizers can increase the moisture content of the skin by absorbing moisture, while other ingredients with a water-blocking function can prevent the loss of moisture. In addition, some components with repairing and nourishing effects can improve the barrier function of the skin and enhance the resistance of the skin to the external environment.
The Chinese patent (application number: 201510505365.4) discloses a moisturizing composition, and a preparation method and application thereof, wherein the moisturizing composition mainly comprises 10-25 parts of plant extract liposome, 3-10 parts of dendrobium candidum extract, 3-10 parts of aloe extract, 0-3 parts of natural moisturizing factor and 0-3 parts of ceramide, and the plant extract is dendrobium candidum extract and grape seed extract. Although the invention can effectively improve the moisturizing and repairing effects of the skin and solve the problem of skin dryness, the invention still has a problem, but does not solve the problems of oxidization resistance and aging, and the prepared moisturizing composition has single efficacy, so that the multiple efficacy of the moisturizing composition needs to be further improved, and the market application is enlarged.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention provides a composition with moisturizing effect and application thereof.
In order to solve the technical problems, the invention adopts the following technical scheme:
a composition with moisturizing effect is prepared by mixing the following substances in percentage by mass: 3-8% of plant extract, 0.5-4% of composite hydrolyzed collagen and the balance of water.
The plant extract is prepared from at least two of aloe, rose, liquorice, clove and dendrobium, and preferably comprises the following raw materials in percentage by mass (4-6): (2-4): (3-5): (0.5-2): (0.5-2); further, the plant extract is prepared from aloe, rose, liquorice, clove and dendrobium according to the mass ratio of 5:3:4:1:1.
The preparation method of the plant extract comprises the following steps:
n1 mixing aloe, rose, licorice, clove and dendrobium, crushing and sieving to obtain mixed powder;
Mixing the mixed powder with ethanol water solution, placing in a reflux device with nitrogen protection for reflux, cooling to room temperature, filtering, retaining filtrate A, and drying filter cake; adding ethanol water solution into the filter cake, performing ultrasonic extraction, filtering, retaining filtrate B, combining filtrate A and filtrate B, concentrating under reduced pressure, and freeze-drying to obtain plant extract.
Aloe extract: aloe contains abundant polysaccharide and amino acid, and can absorb moisture and retain water, and provide deep moisture and relieving effects for skin. Water retention capacity: the aloe extract contains polysaccharide substances, has excellent water-retaining capacity, and can adsorb and lock water to form a protective film to prevent water loss and keep skin moist. Osmotic force: the natural moisturizing factors in aloe have smaller molecular size, can quickly permeate into deep layers of skin, supplement moisture storage of skin, and enhance moisturizing ability of skin. And (3) relieving and repairing: aloe has effects of tranquilizing and relieving skin, and can be used for relieving discomfort and inflammatory reaction caused by dryness, and promoting skin repair and regeneration.
Rose extract: the rose has good moisturizing and nourishing properties, can increase the moisture content of skin, and improve the softness and luster of skin. Moisturizing and water locking: the rose extract contains various natural active ingredients such as polysaccharide and vitamins, and has excellent moisture keeping and water locking capabilities. They are capable of forming protective films, preventing moisture loss, and maintaining skin moisturization. Moisturizing and nourishing: the rose extract is rich in polysaccharide and organic acid, and can provide additional moisture supply, increase skin moisture content, and improve dry and rough skin condition. Antioxidant effect: the anthocyanin and the vitamin C in the rose extract have strong antioxidant activity, can neutralize free radicals, reduce oxidative damage of environmental factors to skin, and maintain the health state of the skin.
Licorice extract: the Glycyrrhrizae radix extract generally comprises Glycyrrhrizae radix root component, wherein the main active ingredient is glycyrrhizic acid. Anti-inflammatory action: the Glycyrrhrizae radix extract has antiinflammatory effect, and can relieve skin inflammation and sensitive reaction, and reduce skin water loss caused by inflammation. Moisturizing effect: the Glycyrrhrizae radix extract has moisturizing effect, and can enhance skin water retention capacity, form protective barrier, and prevent water evaporation, so as to keep skin moist. Antioxidant effect: the antioxidant component in the licorice extract can neutralize free radicals, reduce damage to skin caused by environmental factors, provide additional protection, and help maintain the health of skin.
Flos Caryophylli extract: the flos Caryophylli extract generally comprises components of flos Caryophylli bud, wherein the main active component is eugenol. The flos Caryophylli extract has effects of keeping moisture and retaining water, and can enhance skin water retention capacity, form a film, reduce water loss, and keep skin moist. The flos Caryophylli extract can also regulate sebum secretion, make skin reach water-oil balance state, and improve dry and greasy skin condition. Eugenol in the clove extract has strong antibacterial capability, can effectively inhibit bacterial growth, and reduces skin problems caused by bacteria.
Dendrobe extract: the herba Dendrobii extract contains abundant polysaccharide and flavonoid compounds, and has good moisture keeping effect. Moisturizing and water locking effects: they can form a protective film, reduce the loss of moisture and effectively lock the moisture of the skin. This helps to maintain skin moisture and reduces skin problems caused by dryness and evaporation of water. Promoting hydration of the stratum corneum: the polysaccharide component of herba Dendrobii extract can promote hydration of skin horny layer. They can absorb moisture, provide additional moisture replenishment, increase the moisture content of the stratum corneum, and make the skin softer and smoother. Antioxidant effect: the herba Dendrobii extract is rich in flavonoids, and has strong antioxidant activity. The antioxidant component can neutralize free radical and reduce oxidation damage caused by environmental factors. This helps to protect the skin from ultraviolet light, pollutants and other harmful substances, and to maintain the healthy state of the skin. Soothing sedation: some components in herba Dendrobii extract have skin soothing and calming effects. They can reduce skin sensitivity and inflammatory response, and alleviate skin discomfort. By soothing the skin, the dendrobium extract helps to improve dry, sensitive and inflamed skin conditions.
In a word, the invention adopts aloe, rose, liquorice, clove and dendrobium extracts to play a synergistic role in the moisturizing cosmetics. They each have unique moisturizing effects, and meanwhile, have a plurality of complementary action mechanisms: (1) combined moisturizing and water locking effects: the polysaccharide component in the extract has good moisture keeping and water locking capacity. The polysaccharides in aloe, rose, licorice, clove and dendrobium extracts can form protective films, reduce water loss, and thus enhance the moisturizing effect of the skin. When they are used in combination, the polysaccharide components can be mutually overlapped to form a more stable moisture-retaining barrier, and the moisture-retaining and water-locking effects are synergistically exerted. (2) promote hydration of the stratum corneum: the active ingredients in these extracts can promote hydration of the stratum corneum. The polysaccharides and other active ingredients in aloe, rose, licorice, clove and dendrobium extracts have the ability to adsorb moisture, can increase the moisture content of the stratum corneum, and improve the softness and smoothness of the skin. The combination of the components can provide more water supply, synergistically promote the hydration of the stratum corneum and enhance the moisturizing effect of the skin. (3) antioxidant and soothing actions:
The antioxidant component and soothing component in the extract can act together to improve skin moisture. The antioxidant component in the aloe, rose, licorice, clove and dendrobium extracts can neutralize free radicals, reduce the oxidative damage of environmental factors to skin and maintain the health state of the skin. Meanwhile, the soothing components in the composition can reduce the sensibility and inflammatory response of the skin and relieve the discomfort caused by dryness. Through the synergistic exertion of the antioxidant and soothing effects, the moisturizing condition of the skin can be improved, so that the skin is healthier and smoother.
Preferably, the preparation method of the plant extract comprises the following steps:
N1 mixing aloe, rose, licorice, clove and dendrobium, crushing, and sieving with a 10-40 mesh sieve to obtain mixed powder; the plant extract is prepared from aloe, rose, liquorice, clove and dendrobium according to the mass ratio of (4-6): (2-4): (3-5): (0.5-2): (0.5-2);
Mixing 70-120 parts by weight of the mixed powder with 400-700 parts by weight of 60-80wt% ethanol water solution, placing in a reflux device with nitrogen protection, refluxing for 4-6h at 75-90 ℃, cooling to room temperature, filtering, retaining filtrate A, and drying to obtain a filter cake; adding 300-500 parts by weight of 40-60wt% ethanol water solution into the filter cake, extracting at 30-50deg.C, ultrasonic power of 200-400W and ultrasonic frequency of 40-60kHz for 50-80min, standing for 20-50min after finishing, filtering, retaining filtrate B, mixing filtrate A and filtrate B, concentrating under reduced pressure to 10-30% of the original volume, and freeze drying to obtain plant extract.
The preparation method of the composite hydrolyzed collagen comprises the following steps:
S1, adding a cleaning agent into fresh fish scales, stirring, filtering, washing to be neutral, and drying to obtain pretreated fish scale powder; adding water for ultrasonic treatment; repeatedly cleaning, drying, pulverizing, and sieving to obtain fish scale powder;
S2, adding citric acid aqueous solution into the fish scale powder, stirring, performing ultrasonic treatment, and adding trypsin for enzymolysis; adding hydrochloric acid to regulate pH, and adding flavourzyme for enzymolysis; inactivating enzyme, centrifuging, and retaining supernatant to obtain collagen stock solution;
S3, dissolving chitosan in an acetic acid aqueous solution, adding methoxy polyethylene glycol ethylene oxide for reaction, adjusting pH with an HCl solution, dialyzing, and freeze-drying to obtain hydroxyethyl chitin; adding PBS buffer solution of arginine, 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide and N-hydroxysuccinimide, stirring in ice water bath, reacting again, dialyzing, and freeze-drying to obtain amino acid modified chitosan;
And S4, adding the amino acid modified chitosan into the collagen stock solution, stirring to obtain an enzymolysis solution, and performing enzymolysis and freeze drying to obtain the composite hydrolyzed collagen.
The collagen has good beautifying effect, and good water-retaining ability, so that the skin is moist and bright, the skin tightness can be increased, the skin tension is generated, pores are reduced, and the skin is rich in elasticity. The collagen is similar to protein of human skin, has strong permeability to skin, can be combined with skin epithelial cells through stratum corneum, participates in and improves metabolism of the skin cells, enhances collagen activity in the skin, oxidizes cells to generate free radicals, promotes further aging of the skin, and has an antioxidant effect, so that the collagen can also play a certain role in protection. And the collagen is a small molecular polypeptide formed after the collagen is treated by artificial protease, and can be effectively absorbed and utilized; can effectively supplement collagen components relative to other polypeptides; and the collagen peptide has high activity, and can be efficiently targeted and absorbed by human body.
Because the collagen and the hydrolysate thereof have similar structures with human skin collagen, the collagen and the hydrolysate thereof have good compatibility, can enter into the deep layer of human skin, have good nutrition effect on the skin, have amino acids such as hydroxyproline, hydroxylysine and the like with a large number of carboxyl groups and hydroxyl groups in the collagen, and have a large number of natural moisturizing factors such as glycine and the like, can improve the water storage capacity of tissue cells, have good moisturizing effect on the skin, have a plurality of collagen polypeptides related to the growth, division, proliferation, migration and differentiation of skin cells, can provide nutrients for the skin, delay the aging of the skin and promote the wound repair of the skin.
In order to improve the utilization rate of the collagen, the collagen peptide is hydrolyzed to generate the collagen peptide, compared with the collagen, the collagen peptide has the advantages of increased polar groups and further enhanced solubility, obviously increased water absorption and water retention, and simultaneously has a plurality of biological activities such as the influence of antioxidant activity besides the general functional characteristics of the protein. Compared with high molecular weight natural collagen, small molecular weight collagen peptide penetrates deep into skin more easily through stratum corneum, and can play important roles in growth of fibroblast, collagen expression and formation of strong collagen fibers in epidermis, and can maintain skin homeostasis and repair damaged skin layers by increasing water content of stratum corneum. In order to maximize the skin permeability of the collagen peptide. Firstly, S1, cleaning, drying and crushing the abandoned fish scales, and then adding a cleaning agent to remove and dissolve grease on the surfaces of the fish scales, including the lipid on the surfaces of the fish scales and the fish oil, so that the surfaces of the fish scales are cleaner, and meanwhile, the adhesive force and the adhesive force of the fish scales can be effectively reduced, convenience is brought to the following treatment by adopting citric acid, and the extraction efficiency of the collagen is improved; s2, adding citric acid aqueous solution for treatment can effectively increase the solubility of collagen, promote the hydrolysis of collagen, and accelerate the hydrolysis process of collagen, so that the collagen is easier to be absorbed and utilized by human bodies. In addition, the citric acid water treatment is added to promote the reduction of collagen and improve the functional activity of collagen. S3, preparing chitin with different molecular weights through oxidative degradation, and modifying hydroxyethyl on the surface of the chitin, so that the compatibility of the chitin with lipid in a skin cuticle is improved; finally, the positive charge quantity of the chitosan is increased by modifying amino acid on the chitosan, so that the charge content of the chitosan is increased, and the amino acid modified chitosan is further obtained. And S4, grafting the amino and carboxyl in the collagen stock solution with the carboxyl, amino and hydroxyl in the amino acid modified chitosan to obtain the composite hydrolyzed collagen.
Preferably, the preparation method of the composite hydrolyzed collagen comprises the following steps:
S1, adding a cleaning agent with the mass 3-6 times that of the fish scale powder into fresh fish scales, stirring for 1-4 hours at the temperature of 30-50 ℃ and at the speed of 600-1000rpm, filtering, washing to be neutral, and drying to obtain pretreated fish scale powder; adding 5-10 times of water, and cleaning at room temperature and ultrasonic power of 200-400W and ultrasonic frequency of 45-70kHz for 20-50min; repeatedly cleaning for 2-5 times, drying, pulverizing, and sieving with 50-80 mesh sieve to obtain fish scale powder; the cleaning agent is a mixture of 8-15wt% of glycerol aqueous solution and laurinol polyoxyethylene ether according to the mass ratio of (30-50): 1;
S2, adding 3-6 times of citric acid aqueous solution with the mass concentration of 5-8wt% into the fish scale powder, stirring for 3-8min at 600-1000rpm, placing the fish scale powder at 50-70 ℃ and ultrasonic power of 200-400W and ultrasonic frequency of 45-70kHz for 60-120min, adjusting pH to 7.5-8.5, adding 0.1-0.3 part by weight of trypsin, and carrying out enzymolysis for 1-3h at 35-40 ℃; adding 0.5-2mol/L hydrochloric acid to adjust pH=6-7, adding 0.3-0.7 weight part of flavourzyme, and performing enzymolysis at 50-60 ℃ for 2-5 h; inactivating enzyme at 85-100deg.C for 10-30min, centrifuging, and retaining supernatant to obtain collagen stock solution;
s3, dissolving 4-8 parts by weight of chitosan in 160-300 parts by weight of 3-8wt% acetic acid aqueous solution, adding 0.3-0.8 part by weight of methoxy polyethylene glycol ethylene oxide, reacting for 6-10 hours at 40-60 ℃ and 300-500rpm, adjusting pH=1.5-2.5, dialyzing, and freeze-drying to obtain hydroxyethyl chitin; adding 4-6 parts by weight of 8-12wt% arginine PBS buffer solution (pH=5.0, 0.1M), 0.2-0.8 parts by weight of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide and 0.1-0.5 parts by weight of N-hydroxysuccinimide, stirring for 1-3 hours in an ice-water bath at 300-500rpm, reacting for 4-8 hours at 25-35 ℃, dialyzing, and freeze-drying to obtain amino acid modified chitosan;
S4, adding 2-5 parts by weight of the amino acid modified chitosan into 40-60 parts by weight of the collagen stock solution, stirring for 10-20min at 500-700rpm, and freeze-drying to obtain the composite hydrolyzed collagen.
The composite hydrolyzed collagen prepared by the invention can be effectively absorbed by human skin, has very good moisture absorption and retention properties and relatively good antioxidant activity, can penetrate the skin more slowly, supplements skin moisture better, maintains skin elasticity, repairs skin barrier, has excellent beautifying effect, and is particularly suitable for being used in various cosmetics.
The preparation method of the composition with the moisturizing effect comprises the step of uniformly mixing plant extracts, composite hydrolyzed collagen and water according to a proportion.
The composition with the moisturizing effect is applied to the preparation of moisturizing cosmetics and hair care products.
The invention has the beneficial effects that: the composition with the moisturizing effect is mild in raw materials, free of stimulation, natural, green and environment-friendly, and simple in preparation method, can greatly maintain the stability of active ingredients, and is high in percutaneous absorption rate, obvious in moisturizing effect and good in antioxidation effect.
Detailed Description
The above summary of the present invention is described in further detail below in conjunction with the detailed description, but it should not be understood that the scope of the above-described subject matter of the present invention is limited to the following examples.
Introduction of partial raw materials in the application:
Chitosan was purchased from su-state jia leaf biotechnology limited, degree of deacetylation: 90%, viscosity: 50-200 mPa.s.
Trypsin was purchased from Guangdong Eusman Biotechnology Co., ltd., enzyme activity: 20 ten thousand U/g.
Flavourzyme is purchased from Nanning Donghenghua biological technology Limited liability company and has a specific activity of about 24000U/g.
Commercially available hydrolyzed collagen is purchased from western safety austochyta, inc, mesh: 80 mesh, cargo number: QAD-053.
Commercial plant extracts are purchased from Jining Malus asiatica chemical industry Co., ltd, and the main components are as follows: aloe vera extract.
Example 1
A composition with moisturizing effect is prepared by mixing the following substances in percentage by mass: 5% of commercial plant extract, 3% of commercial hydrolyzed collagen and the balance of water.
Example 2
A composition with moisturizing effect is prepared by mixing the following substances in percentage by mass: 5% of plant extract, 3% of hydrolyzed collagen and the balance of water.
The preparation method of the plant extract comprises the following steps:
n1 mixing aloe, rose, licorice, clove and dendrobium, crushing, and sieving with a 20-mesh sieve to obtain mixed powder; the aloe, the rose, the liquorice, the clove and the dendrobium are prepared from the following components in percentage by mass: 3:4:1:1, a step of;
Mixing 100 parts by weight of the mixed powder with 500 parts by weight of 70wt% ethanol water solution, placing in a reflux device with nitrogen protection, refluxing for 5 hours at 80 ℃, cooling to room temperature, filtering, retaining filtrate A, and drying to obtain a filter cake; adding 400 parts by weight of 50wt% ethanol water solution into the filter cake, extracting at 40 ℃ under the ultrasonic power of 300W and the ultrasonic frequency of 45kHz for 60min, standing for 30min after the completion, filtering, retaining filtrate B, combining filtrate A and filtrate B, concentrating under reduced pressure to 20% of the original volume, and freeze-drying to obtain the plant extract.
The preparation method of the hydrolyzed collagen comprises the following steps:
S1, adding a cleaning agent with the mass of 4 times of that of the fish scale powder into fresh fish scales, stirring for 2 hours at 40 ℃ and 800rpm, filtering, washing to be neutral, and drying to obtain pretreated fish scale powder; adding 7 times of water into the pretreated fish scale powder, and cleaning for 30min at room temperature and ultrasonic power of 300W and ultrasonic frequency of 60 kHz; repeatedly cleaning for 3 times, drying, pulverizing, and sieving with 60 mesh sieve to obtain fish scale powder; the cleaning agent is a mixture of 10wt% of glycerol aqueous solution and laurinol polyoxyethylene ether according to a mass ratio of 40:1;
S2, adding 5 times of 5wt% citric acid aqueous solution into the fish scale powder, stirring for 5min at 800rpm, placing at 60 ℃ and ultrasonic power 300W and ultrasonic frequency 60kHz for 90min, adjusting pH to 8, adding 0.2 part by weight of trypsin, and carrying out enzymolysis for 2h at 37 ℃; adjusting the pH to be 6.5, adding 0.5 part by weight of flavourzyme, and carrying out enzymolysis for 3 hours at 55 ℃; inactivating enzyme at 90deg.C for 15min, centrifuging, and retaining supernatant to obtain collagen stock solution;
and S3, freeze-drying the 50 parts by weight of collagen stock solution to obtain hydrolyzed collagen.
Example 3
A composition with moisturizing effect is prepared by mixing the following substances in percentage by mass: 5% of plant extract, 3% of composite hydrolyzed collagen and the balance of water.
The preparation method of the plant extract comprises the following steps:
n1 mixing aloe, rose, licorice, clove and dendrobium, crushing, and sieving with a 20-mesh sieve to obtain mixed powder; the aloe, the rose, the liquorice, the clove and the dendrobium are prepared from the following components in percentage by mass: 3:4:1:1, a step of;
Mixing 100 parts by weight of the mixed powder with 500 parts by weight of 70wt% ethanol water solution, placing in a reflux device with nitrogen protection, refluxing for 5 hours at 80 ℃, cooling to room temperature, filtering, retaining filtrate A, and drying to obtain a filter cake; adding 400 parts by weight of 50wt% ethanol water solution into the filter cake, extracting at 40 ℃ under the ultrasonic power of 300W and the ultrasonic frequency of 45kHz for 60min, standing for 30min after the completion, filtering, retaining filtrate B, combining filtrate A and filtrate B, concentrating under reduced pressure to 20% of the original volume, and freeze-drying to obtain the plant extract.
The preparation method of the composite hydrolyzed collagen comprises the following steps:
S1, adding a cleaning agent with the mass of 4 times of that of the fish scale powder into fresh fish scales, stirring for 2 hours at 40 ℃ and 800rpm, filtering, washing to be neutral, and drying to obtain pretreated fish scale powder; adding 7 times of water into the pretreated fish scale powder, and cleaning for 30min at room temperature and ultrasonic power of 300W and ultrasonic frequency of 60 kHz; repeatedly cleaning for 3 times, drying, pulverizing, and sieving with 60 mesh sieve to obtain fish scale powder; the cleaning agent is a mixture of 10wt% of glycerol aqueous solution and laurinol polyoxyethylene ether according to a mass ratio of 40:1;
S2, adding 5 times of 5wt% citric acid aqueous solution into the fish scale powder, stirring for 5min at 800rpm, placing at 60 ℃ and ultrasonic power 300W and ultrasonic frequency 60kHz for 90min, adjusting pH to 8, adding 0.2 part by weight of trypsin, and carrying out enzymolysis for 2h at 37 ℃; adjusting the pH to be 6.5, adding 0.5 part by weight of flavourzyme, and carrying out enzymolysis for 3 hours at 55 ℃; inactivating enzyme at 90deg.C for 15min, centrifuging, and retaining supernatant to obtain collagen stock solution;
s3, adding 3 parts by weight of chitosan into the 50 parts by weight of collagen stock solution, stirring for 15min at 600rpm, and freeze-drying to obtain the composite hydrolyzed collagen.
Example 4
A composition with moisturizing effect is prepared by mixing the following substances in percentage by mass: 5% of plant extract, 3% of composite hydrolyzed collagen and the balance of water.
The preparation method of the plant extract comprises the following steps:
n1 mixing aloe, rose, licorice, clove and dendrobium, crushing, and sieving with a 20-mesh sieve to obtain mixed powder; the aloe, the rose, the liquorice, the clove and the dendrobium are prepared from the following components in percentage by mass: 3:4:1:1, a step of;
Mixing 100 parts by weight of the mixed powder with 500 parts by weight of 70wt% ethanol water solution, placing in a reflux device with nitrogen protection, refluxing for 5 hours at 80 ℃, cooling to room temperature, filtering, retaining filtrate A, and drying to obtain a filter cake; adding 400 parts by weight of 50wt% ethanol water solution into the filter cake, extracting at 40 ℃ under the ultrasonic power of 300W and the ultrasonic frequency of 45kHz for 60min, standing for 30min after the completion, filtering, retaining filtrate B, combining filtrate A and filtrate B, concentrating under reduced pressure to 20% of the original volume, and freeze-drying to obtain the plant extract.
The preparation method of the composite hydrolyzed collagen comprises the following steps:
S1, adding a cleaning agent with the mass of 4 times of that of the fish scale powder into fresh fish scales, stirring for 2 hours at 40 ℃ and 800rpm, filtering, washing to be neutral, and drying to obtain pretreated fish scale powder; adding 7 times of water into the pretreated fish scale powder, and cleaning for 30min at room temperature and ultrasonic power of 300W and ultrasonic frequency of 60 kHz; repeatedly cleaning for 3 times, drying, pulverizing, and sieving with 60 mesh sieve to obtain fish scale powder; the cleaning agent is a mixture of 10wt% of glycerol aqueous solution and laurinol polyoxyethylene ether according to a mass ratio of 40:1;
S2, adding 5 times of 5wt% citric acid aqueous solution into the fish scale powder, stirring for 5min at 800rpm, placing at 60 ℃ and ultrasonic power 300W and ultrasonic frequency 60kHz for 90min, adjusting pH to 8, adding 0.2 part by weight of trypsin, and carrying out enzymolysis for 2h at 37 ℃; adjusting the pH to be 6.5, adding 0.5 part by weight of flavourzyme, and carrying out enzymolysis for 3 hours at 55 ℃; inactivating enzyme at 90deg.C for 15min, centrifuging, and retaining supernatant to obtain collagen stock solution;
S3, dissolving 5 parts by weight of chitosan in 200 parts by weight of 5wt% acetic acid aqueous solution, adding 0.5 part by weight of methoxypolyethylene glycol ethylene oxide, reacting for 8 hours at 50 ℃ and 400rpm, adjusting pH to be 2, dialyzing, and freeze-drying to obtain hydroxyethyl chitin;
s4, adding 3 parts by weight of the hydroxyethyl chitin into 50 parts by weight of the collagen stock solution, stirring for 15min at 600rpm, and freeze-drying to obtain the composite hydrolyzed collagen.
Example 5
A composition with moisturizing effect is prepared by mixing the following substances in percentage by mass: 5% of plant extract, 3% of composite hydrolyzed collagen and the balance of water.
The preparation method of the plant extract comprises the following steps:
n1 mixing aloe, rose, licorice, clove and dendrobium, crushing, and sieving with a 20-mesh sieve to obtain mixed powder; the aloe, the rose, the liquorice, the clove and the dendrobium are prepared from the following components in percentage by mass: 3:4:1:1, a step of;
Mixing 100 parts by weight of the mixed powder with 500 parts by weight of 70wt% ethanol water solution, placing in a reflux device with nitrogen protection, refluxing for 5 hours at 80 ℃, cooling to room temperature, filtering, retaining filtrate A, and drying to obtain a filter cake; adding 400 parts by weight of 50wt% ethanol water solution into the filter cake, extracting at 40 ℃ under the ultrasonic power of 300W and the ultrasonic frequency of 45kHz for 60min, standing for 30min after the completion, filtering, retaining filtrate B, combining filtrate A and filtrate B, concentrating under reduced pressure to 20% of the original volume, and freeze-drying to obtain the plant extract.
The preparation method of the composite hydrolyzed collagen comprises the following steps:
S1, adding a cleaning agent with the mass of 4 times of that of the fish scale powder into fresh fish scales, stirring for 2 hours at 40 ℃ and 800rpm, filtering, washing to be neutral, and drying to obtain pretreated fish scale powder; adding 7 times of water into the pretreated fish scale powder, and cleaning for 30min at room temperature and ultrasonic power of 300W and ultrasonic frequency of 60 kHz; repeatedly cleaning for 3 times, drying, pulverizing, and sieving with 60 mesh sieve to obtain fish scale powder; the cleaning agent is a mixture of 10wt% of glycerol aqueous solution and laurinol polyoxyethylene ether according to a mass ratio of 40:1;
S2, adding 5 times of 5wt% citric acid aqueous solution into the fish scale powder, stirring for 5min at 800rpm, placing at 60 ℃ and ultrasonic power 300W and ultrasonic frequency 60kHz for 90min, adjusting pH to 8, adding 0.2 part by weight of trypsin, and carrying out enzymolysis for 2h at 37 ℃; adjusting the pH to be 6.5, adding 0.5 part by weight of flavourzyme, and carrying out enzymolysis for 3 hours at 55 ℃; inactivating enzyme at 90deg.C for 15min, centrifuging, and retaining supernatant to obtain collagen stock solution;
S3, dissolving 5 parts by weight of chitosan into 200 parts by weight of 5wt% acetic acid aqueous solution, adding 0.5 part by weight of methoxy polyethylene glycol ethylene oxide, reacting for 8 hours at 50 ℃ and 400rpm, adjusting pH=2, and dialyzing to obtain hydroxyethyl chitin; adding 5 parts by weight of 10wt% arginine PBS buffer solution (pH=5.0, 0.1M), 0.5 parts by weight of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide and 0.3 parts by weight of N-hydroxysuccinimide, stirring in an ice water bath at 400rpm for 1.5 hours, reacting at 30 ℃ for 6 hours, dialyzing, and freeze-drying to obtain amino acid modified chitosan;
S4, adding 3 parts by weight of the amino acid modified chitosan into 50 parts by weight of the collagen stock solution, stirring for 15min at 600rpm, and freeze-drying to obtain the composite hydrolyzed collagen.
Test example 1
Assessment of moisturizing Properties: a cosmetic was prepared from 0.5% by weight of carbomer, 1.0% by weight of nicotinamide, 1% by weight of sorbitan monostearate, 2% by weight of cetostearyl glucoside, 2% by weight of glyceryl monostearate, 1% by weight of polydimethylsiloxane, 10% by weight of the moisturizing composition prepared in examples 1 to 5, and the balance deionized water, and the skin of 30 to 40 years old was dried or persons believed to have dry skin were randomly divided into 5 groups of 10 persons each. The compositions with moisturizing effect prepared in examples 1 to 5 were prepared to prepare cosmetics to be applied to the face of a subject, respectively. The subjects uniformly cleaned the facial skin and wiped clean with a dry face towel, after 30min, the facial moisture of the subjects was measured and recorded using a HONKON-TC02s skin tester, and before application was started, the skin moisture content of each subject was measured using a skin tester under constant temperature and constant humidity (24 ℃ and 40% humidity) and used as a reference value. Skin moisture levels were measured at 0.5h, 2h, 6h after application and averaged. The measurement results are shown in table 1 below.
Principle of measurement method using skin moisture tester: the moisturizing performance was determined by measuring the water ion degree in the epidermis of the skin using a sensor, the measurement result was represented numerically, and the water content was calculated.
Table 1 results of moisturizing effect test of compositions having moisturizing efficacy
Test example 2
Hydroxyl radical scavenging test: the compositions with moisturizing effect prepared in example 1, example 2 and example 5 were subjected to hydroxyl radical scavenging test:
4 groups were set up as positive control groups (Vc groups), examples 1, 2 and 5. Vc is selected as a positive control group, absolute ethyl alcohol is selected as a solvent, and Vc is prepared into a solution to be detected with the concentration of 100 mug/mL. In this manner, the compositions having moisturizing effect obtained in example 1, example 2 and example 5 were prepared into test solutions having a concentration of 100. Mu.g/mL in the test group by weight.
Fresh 0.15mmol/L DPPH in ethanol was prepared. Uniformly mixing the solution to be detected (1.5 mL) +DPPH ethanol solution (7.5 mL), incubating for 30min at 37 ℃ in a dark place, and measuring absorbance (A1) at 517 nm; uniformly mixing the solution to be detected (1.5 mL) +absolute ethyl alcohol (7.5 mL), and incubating at 37 ℃ for 30min in a dark place to measure absorbance (A2); the blank was absolute ethanol (1.5 mL) +DPPH ethanol (7.5 mL) and absorbance was recorded as A0 by incubation at 37℃for 30min in the absence of light. The relative clearance (R) of the samples to DPPH radicals was calculated as follows, with greater clearance indicating greater antioxidant capacity, and 5 times per set of replicates, with the results shown in table 2.
DPPH radical scavenging Ra= [ A0- (A1-A2) ]/A0.times.100%
Table 2 results of hydroxyl radical scavenging test of compositions with moisturizing efficacy
Radical scavenging rate of hydroxyl (%) | |
Example 1 | 70.6 |
Example 2 | 78.3 |
Example 5 | 90.5 |
From the above results, the composition with moisturizing effect prepared by the invention has good moisturizing effect and antioxidant effect. The invention adopts aloe, rose, liquorice, clove and dendrobium extracts to play a synergistic role in the moisturizing cosmetics. They utilize each having unique moisturizing effects while also having complementary effects to each other to collectively enhance the moisturizing and water-retaining effects, the stratum corneum hydration promoting, antioxidant and soothing effects of the moisturizing composition: the antioxidant component and soothing component in the extract can act together to improve skin moisture. The antioxidant component in the aloe, rose, licorice, clove and dendrobium extracts can neutralize free radicals, reduce the oxidative damage of environmental factors to skin and maintain the health state of the skin. As can be seen from examples 1-2, the composite hydrolyzed collagen prepared by the present invention has significantly better moisturizing and antioxidant effects than commercially available hydrolyzed collagen, because the present invention hydrolyzes the same to produce collagen peptide, which has significantly increased water absorption and water holding capacity due to its smaller molecular weight, increased polar groups and thus increased solubility, and also has many biological activities such as the influence of antioxidant activity in addition to the general functional characteristics of protein, and the small molecular weight collagen peptide penetrates deeper into the skin through the stratum corneum more easily, which can play an important role not only in the growth of ciliated cells, the expression of collagen and the formation of strong collagen fibers in the epidermis, but also maintain the skin steady state and repair damaged skin layers by increasing the water content of the stratum corneum. In order to maximize the skin permeability of the collagen peptide. It can be seen from examples 2-5 that modification of hydroxyethyl groups on chitin surface increases its compatibility with lipids in the stratum corneum; finally, the positive charge quantity of the chitosan is increased by modifying amino acid on the chitosan, so that the charge content of the chitosan is increased, and the amino acid modified chitosan is further obtained.
The composite hydrolyzed collagen prepared by the invention can be effectively absorbed by human skin, has very good moisture absorption and retention properties and relatively good antioxidant activity, can penetrate the skin more slowly, supplements skin moisture better, maintains skin elasticity, repairs skin barrier, has excellent beautifying effect, and is particularly suitable for being used in various cosmetics.
Claims (5)
1. The composition with the moisturizing effect is characterized by being prepared by mixing the following substances in percentage by mass: 3-8% of plant extract, 0.5-4% of composite hydrolyzed collagen and the balance of water;
the preparation method of the plant extract comprises the following steps:
N1 mixing aloe, rose, licorice, clove and dendrobium, crushing, and sieving with a 10-40 mesh sieve to obtain mixed powder; wherein the mass ratio of aloe, rose, liquorice, clove and dendrobium is (4-6): (2-4): (3-5): (0.5-2): (0.5-2);
mixing 70-120 parts by weight of the mixed powder with 400-700 parts by weight of 60-80wt% ethanol water solution, placing in a reflux device with nitrogen protection, refluxing for 4-6h at 75-90 ℃, cooling to room temperature, filtering, retaining filtrate A, and drying to obtain a filter cake; adding 300-500 parts by weight of 40-60wt% ethanol water solution into the filter cake, extracting for 50-80min at 30-50 ℃ under ultrasonic power of 200-400W and ultrasonic frequency of 40-60kHz, standing for 20-50min after finishing, filtering, retaining filtrate B, mixing filtrate A and filtrate B, concentrating under reduced pressure to 10-30% of the original volume, and freeze-drying to obtain plant extract;
The preparation method of the composite hydrolyzed collagen comprises the following steps: s1, adding a cleaning agent with the mass 3-6 times that of the fish scale powder into fresh fish scales, stirring for 1-4 hours at the temperature of 30-50 ℃ and at the speed of 600-1000rpm, filtering, washing to be neutral, and drying to obtain pretreated fish scale powder; adding 5-10 times of water, and cleaning at room temperature and ultrasonic power of 200-400W and ultrasonic frequency of 45-70kHz for 20-50min; repeatedly cleaning for 2-5 times, drying, pulverizing, and sieving with 50-80 mesh sieve to obtain fish scale powder; the cleaning agent is a mixture of 8-15wt% of glycerol aqueous solution and laurinol polyoxyethylene ether according to the mass ratio of (30-50): 1;
s2, adding 3-6 times of citric acid aqueous solution with the mass concentration of 5-8wt% into the fish scale powder, stirring for 3-8min at 600-1000rpm, placing the fish scale powder at 50-70 ℃ and ultrasonic power of 200-400W and ultrasonic frequency of 45-70kHz for 60-120min, adjusting pH to 7.5-8.5, adding 0.1-0.3 part by weight of trypsin, and carrying out enzymolysis for 1-3h at 35-40 ℃; adding 0.5-2mol/L hydrochloric acid to adjust pH=6-7, adding 0.3-0.7 weight part of flavourzyme, and performing enzymolysis at 50-60 ℃ for 2-5 h; inactivating enzyme at 85-100deg.C for 10-30min, centrifuging, and retaining supernatant to obtain collagen stock solution;
S3, dissolving 4-8 parts by weight of chitosan in 160-300 parts by weight of 3-8wt% acetic acid aqueous solution, adding 0.3-0.8 part by weight of methoxy polyethylene glycol ethylene oxide, reacting for 6-10 hours at 40-60 ℃ and 300-500rpm, adjusting pH=1.5-2.5, dialyzing, and freeze-drying to obtain hydroxyethyl chitin; adding 4-6 parts by weight of 8-12wt% arginine PBS buffer solution, wherein the pH=5.0, the concentration is 0.1M,0.2-0.8 parts by weight of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide and 0.1-0.5 parts by weight of N-hydroxysuccinimide, stirring for 1-3 hours in an ice water bath at 300-500rpm, reacting for 4-8 hours at 25-35 ℃, dialyzing, and freeze-drying to obtain amino acid modified chitosan;
S4, adding 2-5 parts by weight of the amino acid modified chitosan into 40-60 parts by weight of the collagen stock solution, stirring for 10-20min at 500-700rpm, and freeze-drying to obtain the composite hydrolyzed collagen.
2. The method for preparing a moisturizing composition according to claim 1, wherein the composition is prepared by uniformly mixing plant extracts, composite hydrolyzed collagen and water according to a certain proportion.
3. The preparation method of the composite hydrolyzed collagen is characterized by comprising the following steps of: s1, adding a cleaning agent with the mass 3-6 times that of the fish scale powder into fresh fish scales, stirring for 1-4 hours at the temperature of 30-50 ℃ and at the speed of 600-1000rpm, filtering, washing to be neutral, and drying to obtain pretreated fish scale powder; adding 5-10 times of water, and cleaning at room temperature and ultrasonic power of 200-400W and ultrasonic frequency of 45-70kHz for 20-50min; repeatedly cleaning for 2-5 times, drying, pulverizing, and sieving with 50-80 mesh sieve to obtain fish scale powder; the cleaning agent is a mixture of 8-15wt% of glycerol aqueous solution and laurinol polyoxyethylene ether according to the mass ratio of (30-50): 1;
s2, adding 3-6 times of citric acid aqueous solution with the mass concentration of 5-8wt% into the fish scale powder, stirring for 3-8min at 600-1000rpm, placing the fish scale powder at 50-70 ℃ and ultrasonic power of 200-400W and ultrasonic frequency of 45-70kHz for 60-120min, adjusting pH to 7.5-8.5, adding 0.1-0.3 part by weight of trypsin, and carrying out enzymolysis for 1-3h at 35-40 ℃; adding 0.5-2mol/L hydrochloric acid to adjust pH=6-7, adding 0.3-0.7 weight part of flavourzyme, and performing enzymolysis at 50-60 ℃ for 2-5 h; inactivating enzyme at 85-100deg.C for 10-30min, centrifuging, and retaining supernatant to obtain collagen stock solution;
S3, dissolving 4-8 parts by weight of chitosan in 160-300 parts by weight of 3-8wt% acetic acid aqueous solution, adding 0.3-0.8 part by weight of methoxy polyethylene glycol ethylene oxide, reacting for 6-10 hours at 40-60 ℃ and 300-500rpm, adjusting pH=1.5-2.5, dialyzing, and freeze-drying to obtain hydroxyethyl chitin; adding 4-6 parts by weight of 8-12wt% arginine PBS buffer solution, wherein the pH=5.0, the concentration is 0.1M,0.2-0.8 parts by weight of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide and 0.1-0.5 parts by weight of N-hydroxysuccinimide, stirring for 1-3 hours in an ice water bath at 300-500rpm, reacting for 4-8 hours at 25-35 ℃, dialyzing, and freeze-drying to obtain amino acid modified chitosan;
S4, adding 2-5 parts by weight of the amino acid modified chitosan into 40-60 parts by weight of the collagen stock solution, stirring for 10-20min at 500-700rpm, and freeze-drying to obtain the composite hydrolyzed collagen.
4. Use of the complex hydrolyzed collagen protein according to claim 3 for the preparation of a composition having moisturizing effect.
5. Use of the composition having moisturizing effect as in claim 1 for preparing a moisturizing cosmetic.
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CN107522781A (en) * | 2017-09-01 | 2017-12-29 | 浦江县欧立生物技术有限公司 | The method that collagen peptide is extracted from grass carp scales |
CN109771322A (en) * | 2019-03-19 | 2019-05-21 | 上海联衡生物科技有限公司 | Human stem cell factor skin repair composition and its application in skin care item |
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JP2000191499A (en) * | 1998-12-25 | 2000-07-11 | Henkel Japan Ltd | Moisturizing skin cosmetics |
CN107522781A (en) * | 2017-09-01 | 2017-12-29 | 浦江县欧立生物技术有限公司 | The method that collagen peptide is extracted from grass carp scales |
CN109771322A (en) * | 2019-03-19 | 2019-05-21 | 上海联衡生物科技有限公司 | Human stem cell factor skin repair composition and its application in skin care item |
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