CN113116762B - Tightening cream, preparation method thereof and collagenase inhibitor - Google Patents
Tightening cream, preparation method thereof and collagenase inhibitor Download PDFInfo
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- CN113116762B CN113116762B CN201911396221.4A CN201911396221A CN113116762B CN 113116762 B CN113116762 B CN 113116762B CN 201911396221 A CN201911396221 A CN 201911396221A CN 113116762 B CN113116762 B CN 113116762B
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- extract
- addition amount
- skin
- tightening
- collagenase
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- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
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- A61K2800/782—Enzyme inhibitors; Enzyme antagonists
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Abstract
The application provides a tightening cream, a preparation method thereof and a collagenase inhibitor. The tightening cream comprises a collagenase inhibitor and a penetration enhancer, wherein the addition amount of the collagenase inhibitor is 0.01-10% based on the total mass of the tightening cream; the addition amount of the penetration enhancer is 0.01-10%; the collagenase inhibitor comprises extract of pericarpium Granati and extract of grapefruit; the addition amount of the pomegranate rind extract is 15-65% and the addition amount of the grapefruit extract is 35-85% based on the total mass of the collagenase inhibitor. The tightening cream disclosed by the application is mild in formula, and can effectively improve skin elasticity, so that an anti-aging effect is achieved.
Description
Technical Field
The application relates to a tightening cream, a preparation method thereof and a collagenase inhibitor, belonging to the field of cosmetics.
Background
Collagen is mainly produced by fibroblasts of the dermis layer, is a main component of the dermis layer, can maintain the structure of the skin, and imparts toughness and elasticity to the skin. The collagen content and distribution determine whether the skin is youthful. However, abnormal decrease of collagen content causes thinning of dermis, slackening of skin, loss of elasticity, occurrence of wrinkles, and influence of life quality of people. With the continued intensive research on collagen, researchers have found that collagenase plays an important role in the dynamic balance of skin collagen, and that its overexpression and abnormal activation are one of the main causes of skin aging. Therefore, inhibiting collagenase activity can block skin collagen degradation, increase collagen content, and realize anti-aging effect.
For factors affecting skin collagen content, the main approaches to skin anti-aging and skin care include the following: (1) Increasing collagen synthesis by stimulating proliferation of dermal fibroblasts; (2) The collagen synthesis speed of the fibroblast is stimulated by the active factors, so that the total amount of the collagen in the dermis layer is increased; (3) The catalytic activity of a key enzyme-collagenase for inhibiting collagen degradation in the dermis is used for slowing down the degradation speed of the collagen, so as to achieve the purpose of resisting aging; (4) The sun protection is adopted to prevent ultraviolet rays in sunlight from damaging collagen in skin and slow down photoaging of the skin; (5) The antioxidant is used for removing excessive oxygen free radicals in the skin, so that the induced expression of collagenase and abnormal cross-linking of biomacromolecules are slowed down.
In the prior art, in order to prevent skin from sagging, losing elasticity, wrinkling and the like, and keep skin youthful, anti-aging products mixed with various components such as hydrolyzed collagen, hyaluronic acid, polypeptide, retinol and derivatives thereof have been proposed. However, if these ingredients are used in large amounts, there are problems in terms of anti-aging effects, skin feel in use, and safety. If the molecular weight of the hydrolyzed collagen is too large, the hydrolyzed collagen is not easy to penetrate through the skin barrier of the human body to reach the dermis layer; hyaluronic acid cannot substantially slow down the loss of collagen; polypeptides and retinol present a certain irritation and safety risk to the skin, etc.
Along with the increase of the attention of people to skin health, the development of the natural anti-aging agent with safety, stability, obvious effect and high cost performance becomes one of the main research directions of the current medicine and cosmetic industry, and has very good development prospect.
Disclosure of Invention
Problems to be solved by the application
In view of the prior art, the hydrolyzed collagen has excessive molecular weight, and is not easy to penetrate through the skin barrier of the human body to reach the dermis; hyaluronic acid cannot substantially slow down the loss of collagen; the polypeptide and the retinol have certain irritation to skin, safety risk and other problems, and the application firstly provides the tightening cream containing the collagenase inhibitor, and the tightening cream has excellent anti-aging performance.
Further, the application also provides a collagenase inhibitor capable of inhibiting collagenase activity.
Furthermore, the application also provides a preparation method of the tightening cream, which is simple to operate and easy to obtain raw materials.
Solution for solving the problem
The application provides a tightening cream, which comprises a collagenase inhibitor and a penetration enhancer, wherein the addition amount of the collagenase inhibitor is 0.01-10% based on the total mass of the tightening cream; the addition amount of the penetration enhancer is 0.01-10%;
the collagenase inhibitor comprises extract of pericarpium Granati and extract of grapefruit; the addition amount of the pomegranate rind extract is 15-65% and the addition amount of the grapefruit extract is 35-85% based on the total mass of the collagenase inhibitor.
The tightening cream according to the present application, wherein the collagenase is interstitial collagenase.
The tightening cream according to the present application, wherein the mass ratio of the pomegranate rind extract to the grapefruit extract is 1:0.6-5.5, preferably 1:0.8-5, more preferably 1:1-4.5, still more preferably 1:1.2-4, still more preferably 1:1.5-3.5, still more preferably 1:1.8-3.
The tightening cream according to the present application, wherein the penetration enhancer comprises one or a combination of two or more of propylene glycol, bis-diethoxydiglycol cyclohexane 1, 4-dicarboxylate, and chitosan.
The tightening cream according to the present application, wherein the tightening cream further comprises one or a combination of two or more of a humectant, a thickener, a pH adjuster, a fat, a preservative, a skin conditioner, an emulsifier, a sensitivity-soothing agent, a chelating agent, a fragrance, and an antioxidant; wherein,,
the addition amount of the humectant is 0.01-20%; the addition amount of the thickener is 0.02-5%; the addition amount of the pH regulator is 0.01-1%; the addition amount of the grease is 10-30%; the addition amount of the preservative is 0.01-1.5%; the addition amount of the skin conditioning agent is 0.01-5%; the addition amount of the emulsifier is 0.01-5%; the addition amount of the sensitivity-relieving agent is 0.01-5%; the addition amount of the antioxidant is 0.01-2%; the addition amount of the aromatic is 0.01-1%; the chelating agent is added in an amount of 0-2%.
The tightening cream according to the present application, wherein the skin conditioning agent comprises one or a combination of two or more of manganese chloride, tapioca starch, ceramide 2, lactobacillus/soybean fermentation product extract, palmitoyl tripeptide-5, acetyl hexapeptide-8, palmitoyl oligopeptide, colloidal oat flour, hydrolyzed collagen, hydrolyzed wheat protein, kelp extract, allantoin, pansy extract, and chlorella fermentation product.
The tightening cream of the application, wherein the sensitivity-relieving agent comprises one or more of Hamamelis virginiana flower water, stearyl glycyrrhetinate, bisabolol, ginger root extract and aloe extract.
The application also provides a preparation method of the tightening cream, which comprises the step of mixing the components of the tightening cream.
The present application also provides a collagenase inhibitor comprising: the addition amount of the pomegranate rind extract is 15-65% and the addition amount of the grapefruit extract is 35-85% based on the total mass of the collagenase inhibitor.
The collagenase inhibitor according to the present application, wherein the mass ratio of the pomegranate rind extract to the grapefruit extract is 1:0.6 to 5.5, preferably 1:0.8 to 5, more preferably 1:1 to 4.5, still more preferably 1:1.2 to 4, still more preferably 1:1.5 to 3.5, still more preferably 1:1.8 to 3.
ADVANTAGEOUS EFFECTS OF INVENTION
The tightening cream disclosed by the application is mild in formula, and can effectively improve skin elasticity, so that an anti-aging effect is achieved.
The collagenase inhibitor of the present application has excellent inhibitory effect on collagenase activity and no side effect on human body.
The preparation method of the tightening cream is simple to operate, raw materials are easy to obtain, and batch production can be realized.
Drawings
FIG. 1 is a graph showing the relationship between the logarithmic mass concentration and the collagenase activity inhibition rate of the extract of the red pomegranate rind of comparative examples 1 to 5 of the present application;
FIG. 2 is a graph showing the relationship between the logarithmic mass concentration and the collagenase activity inhibition rate of the grapefruit extract of comparative examples 6-10 of the present application;
FIG. 3 is a graph showing the relationship between the logarithmic mass concentration of collagenase inhibitor and the inhibition rate of collagenase activity in examples 1 to 5 of the present application;
FIG. 4 shows a graph of the content of extract of guava skin in relation to the interaction coefficient in the collagenase inhibitors of examples 1 to 5 of the present application.
Fig. 5 shows a comparative graph of skin elasticity change rates of application examples 1 to 5 of the present application and application comparative examples 1 to 8.
Detailed Description
Various exemplary embodiments, features and aspects of the application are described in detail below. The word "exemplary" is used herein to mean "serving as an example, embodiment, or illustration. Any embodiment described herein as "exemplary" is not necessarily to be construed as preferred or advantageous over other embodiments.
Furthermore, in the following detailed description, numerous specific details are set forth in order to provide a better illustration of the application. It will be understood by those skilled in the art that the present application may be practiced without some of these specific details. In other instances, well known methods, procedures, means, equipment and steps have not been described in detail so as not to obscure the present application.
It should be noted that:
in the present specification, the use of the meaning of "can" or "can" includes both the meaning of performing a certain process and the meaning of not performing a certain process.
In the present specification, the numerical range indicated by the term "numerical value a to numerical value B" means a range including the end point numerical value A, B.
Unless otherwise indicated, all units used in the present application are international standard units, and numerical values, ranges of values, appearing in the present application should be understood to include errors permitted in industrial production.
Reference throughout this specification to "some specific/preferred embodiments," "other specific/preferred embodiments," "an embodiment," and so forth, means that a particular element (e.g., feature, property, and/or characteristic) described in connection with the embodiment is included in at least one embodiment described herein, and may or may not be present in other embodiments. In addition, it is to be understood that the elements may be combined in any suitable manner in the various embodiments.
<First aspect>
In a first aspect, the present application provides a collagenase inhibitor comprising: the addition amount of the pomegranate rind extract is 15-65% and the addition amount of the grapefruit extract is 35-85% based on the total mass of the collagenase inhibitor.
The inventors of the present application found that using a combination of the extract of guava skin and the extract of grapefruit can produce excellent synergistic effects, so that collagenase activity can be suppressed to achieve an anti-aging effect.
Specifically, in the present application, the mass ratio of the pomegranate rind extract to the grapefruit extract is 1:0.6 to 5.5, preferably 1:0.8 to 5, more preferably 1:1 to 4.5, still more preferably 1:1.2 to 4, still more preferably 1:1.5 to 3.5, still more preferably 1:1.8 to 3. When the mass ratio of the pomegranate rind extract to the grapefruit extract is within the above range, a synergistic effect can be further obtained, and the effect of suppressing collagenase activity is excellent.
The method for producing the collagenase inhibitor of the present application is not particularly limited, and may be a method commonly used in the art, for example, a method of mixing the extract of pericarpium Granati and the extract of grapefruit uniformly.
Collagenase enzyme
Collagenases belong to the class of matrix metalloproteinases (Matrix Metalloproteinase, MMPs). Matrix metalloproteinases are a family of endopeptidases whose biological activity depends on zinc ions and which have the ability to degrade the extracellular Matrix (ECM). The main function of collagenase is to degrade collagen and elastin in dermis, and its tissue type inhibitor (Tissue Inhibitors of Metalloproteinase, TIMPs) specifically inhibits collagenase activity by covalent binding to its highly conserved zinc binding site, and together regulate matrix metabolism, maintaining the structure of dermis.
Collagenases include interstitial collagenase (MMP-1), polymorphonuclear collagenase (MMP-8) and collagenase 3 (MMP-13). Wherein, the interstitial collagenase is also called collagenase-1, has multiple functions and can act on different substrates. The matrix collagenase is capable of degrading several matrix molecules such as aggrecan, multipolycan, decorin, casein, entactin, serine protein inhibitors and mucin-C. Thus, the interstitial collagenase plays a key role in the physiological repair of the extracellular matrix. The application is mainly based on the important role of the interstitial collagenase in the skin aging process, and can inhibit the activity of the interstitial collagenase, thereby reducing skin inflammatory reaction and wrinkles, and being used as a way for delaying aging so as to realize the anti-aging effect.
It should be noted that the purpose of the collagenase inhibitor of the present application is to inhibit collagenase activity, not collagenase expression, for example: inhibiting the activity of interstitial collagenase.
Extract of pomegranate rind
Punica granatum (Punica granatum l.) is Punica granatum (Punica) deciduous shrubs or arbors. The baldry peninsula to iran and its neighboring areas are planted in temperate and tropical regions worldwide. The cultivation is carried out in both north and south China, and the planting area is large in Jiangsu, henan and other places. The pomegranate is one of the pomegranates.
The red pomegranate rind has rich chemical substances, such as tannins, alkaloid compounds, flavonoids, amino acids, organic acids and the like, which have pharmacological and health-care effects on human bodies, and can be used for treating insect expelling, hemostasis, dysentery, toothache and the like. The pericarpium Granati extract is rich in pericarpium Granati polyphenols, including ellagitannin, ellagic acid catechol, chlorogenic acid, etc. These substances have antioxidant, free radical scavenging, sun screening, and skin whitening effects.
In the present application, the addition amount of the extract of guava skin is 15-65% based on the total mass of the collagenase inhibitor. When the addition amount of the pomegranate rind extract is 15-65%, collagenase activity can be effectively inhibited.
Grapefruit extract
Grapefruit, also known as grapefruit (Citrus paradisi macf.), is a small tree of Citrus (Citrus) genus of the family Rutaceae (Rutaceae). The grapefruit extract can nourish tissue cells, induce diuresis to alleviate edema, resist bacteria and infection, treat large pores, and condition mixed and oily skin which is easy to grow acnes; deep purifying oily acne and hyperemic skin, compacting skin and heel tissue, and its component naringin has effects of blocking free radical chain reaction of pyrogallol autoxidation, i.e. naringin has antioxidant effect.
In the present application, the grapefruit extract is added in an amount of 35-85% by weight based on the total mass of the collagenase inhibitor. When the content of the grapefruit extract is 35-85%, collagenase activity can be effectively inhibited.
<Second aspect>
In a second aspect the present application provides a tightening cream comprising a collagenase inhibitor according to the first aspect of the application and a penetration enhancer; by adding a proper amount of collagenase inhibitor, the application can inhibit the activity of collagenase, especially the activity of interstitial collagenase, so that the tightening cream has excellent anti-aging effect and can improve skin elasticity. In order to promote the absorption of collagenase inhibitors by the skin, the tightening cream of the present application also uses a penetration enhancer. The collagenase inhibitors of the present application can be used to a greater extent by using a permeation enhancer.
Wherein the collagenase inhibitor is added in an amount of 0.01 to 10% based on the total mass of the tightening cream, for example: 0.5%,1%, 2%, 3%, 5%, 6%, 7%, 8%, etc. When the collagenase inhibitor is added in an amount of between 0.01 and 10%, the skin elasticity after the use of the collagenase inhibitor increases. When the addition amount of the collagenase inhibitor is less than 0.01%, the anti-aging effect cannot be achieved; when the addition amount of the collagenase inhibitor is more than 10%, the content of the collagenase inhibitor is too high, the cost is too high, and the corresponding anti-aging effect is not obviously improved.
The penetration enhancer is added in an amount of 0.01-10% based on the total mass of the tightening cream. When the addition amount of the permeation enhancer is less than 0.01%, the permeation enhancer effect is not obvious. When the addition amount of the permeation enhancer is more than 10%, the permeation enhancer cannot further act.
In the present application, the permeation enhancer includes one or a combination of two or more of propylene glycol, bis-diethoxydiglycol cyclohexane 1, 4-dicarboxylate and chitosan. The present application preferably uses a combination of propylene glycol and bis-diethoxydiglycol cyclohexane 1, 4-dicarboxylate, and the propylene glycol and the bis-diethoxydiglycol cyclohexane 1, 4-dicarboxylate have a synergistic effect, which can make the absorption effect of the collagenase inhibitor more excellent.
When a combination of propylene glycol and bis-diethoxydiglycol cyclohexane 1, 4-dicarboxylate is used as a penetration enhancer, the amount of propylene glycol added is 0.01 to 5% and the amount of bis-diethoxydiglycol cyclohexane 1, 4-dicarboxylate added is 0.01 to 5% based on the total mass of the tightening cream. When the propylene glycol is added in an amount of 0.01 to 5% and the bis-diethoxydiglycol cyclohexane 1, 4-dicarboxylate is added in an amount of 0.01 to 5%, the absorption effect of the collagenase inhibitor can be effectively improved. For example: the amount of propylene glycol added was 0.1%, 0.5%,1%, 1.5%, 2.5%, 3.5%, 4.5%, etc., and the amount of bis-diethoxydiglycol cyclohexane 1, 4-dicarboxylate added was 0.1%, 0.5%,1%, 1.5%, 2.5%, 3.5%, 4.5%.
The tightening cream of the present application may further comprise one or a combination of two or more of moisturizers, thickeners, pH adjusters, oils, preservatives, skin conditioners, emulsifiers, sensitivity-soothing agents, chelating agents, fragrances, and antioxidants. The formula of the tightening cream disclosed by the application is mild in composition, and the efficacy of the collagenase inhibitor disclosed by the application can be fully exerted. Specifically:
the humectant is added in an amount of 0.01-20% based on the total mass of the tightening cream. When the addition amount of the humectant is 0.01-20%, the moisturizing agent can play a role in moisturizing and supplementing water. In order to further exert the effect of the humectant, the humectant of the present application may be preferably added in an amount of 1 to 18%, 2 to 16%, 3 to 14%, 4 to 13%, 5 to 12%, etc. When the content of the humectant is less than 0.01%, the moisturizing effect is not obvious; when the content of the humectant is higher than 20%, the tightening cream is sticky.
In the application, the humectant comprises one or more than two of dipropylene glycol, butanediol, glycerol, panthenol, glycerol polyacrylate, glycerol polyether-26, sodium hyaluronate, betaine and trehalose.
The addition amount of the grease is 10-30% based on the total mass of the tightening cream. For example: the amount of the grease may be 12%, 14%, 16%, 18%, 20%, 22%, 24%, 28%, etc. When the content of the grease is 10-30%, not only can a hydrophobic film be formed on the skin surface to prevent invasion of external harmful substances, but also evaporation of moisture on the skin surface can be inhibited to prevent skin chapping. When the addition amount of the grease is less than 10%, invasion of harmful substances cannot be effectively prevented; when the amount of the oil added is more than 30%, the tightening cream becomes too greasy, and the feeling of use is lowered.
In the application, the grease comprises one or more than two of isopropyl myristate, polydimethylsiloxane, cyclomethicone, cyclopentadimethicone, caprylic/capric triglyceride, oleyl erucate, hydrogenated polyisobutene, shea butter, ethylhexyl palmitate, olive oil unsaponifiable matter, hydrogenated polydecene, cyclohexasiloxane, C20-24 alkyl dimethicone, C13-14 isoparaffin and C12-15 alcohol benzoate.
The addition amount of the emulsifier is 0.01-5% based on the total mass of the tightening cream. Preferably 0.1-4%, for example: 0.5%,1%,1.2%,1.5%,2%,2.5%, 3%, 3.5%, 4%, etc. When the dosage of the emulsifier is less than 0.01%, insufficient emulsification is caused, so that the system is unstable; when the dosage of the emulsifier is more than 5%, the irritation of the product can be increased, and meanwhile, the stability of the product can be influenced to a certain extent.
In the present application, the emulsifier includes one or a combination of two or more of polyglycerol-3 methyl glucose distearate, a complex of PEG-100 stearate and glycerol stearate, cetyl polyether-20, polysorbate-60, a complex of polyacrylamide and laureth-7 and C13-14 isoparaffin, sorbitan sesquioleate.
The emulsifying system of the present application is a non-water-in-oil system, and therefore, when propylene glycol and bis-diethoxydiglycol cyclohexane 1, 4-dicarboxylate are used as the permeation enhancer, the synergistic effect is not affected even if they are not added at the same time.
The thickener is added in an amount of 0.02 to 5% based on the total mass of the tightening cream. By adding the thickener, the consistency of the tightening cream of the present application can be made suitable and the stability is excellent. Preferably, the thickener of the present application may be added in an amount of 0.05 to 4%, 0.1 to 3%, 1 to 3%, etc.
The thickener comprises one or more than two of xanthan gum, behenyl alcohol, polyacrylamide, carbomer, polyethylene glycol-90M, ammonium acryloyldimethyl taurate/VP copolymer and hydroxyethyl acrylate/sodium acryloyldimethyl taurate copolymer.
In order to further improve the efficacy of the tightening cream of the present application, the tightening cream of the present application further comprises the skin conditioning agent. By adding skin conditioning agents, the occurrence of wrinkles can be reduced. The effective components in the skin conditioner can penetrate deep into skin and be absorbed by skin, so as to improve skin state.
The skin conditioning agent is added in an amount of 0.01-5% based on the total mass of the tightening cream. Preferably, the skin conditioning agent may be added in an amount of 0.1 to 4%, 0.5 to 3%, 0.6 to 2.5%, etc. When the addition amount of the skin conditioning agent is less than 0.01%, the corresponding effect cannot be achieved; when the amount of the skin conditioner added is more than 5%, the cost is too high.
The skin conditioner comprises one or more than two of manganese chloride, tapioca starch, ceramide 2, lactobacillus/soybean fermentation product extract, palmitoyl tripeptide-5, acetyl hexapeptide-8, palmitoyl oligopeptide, colloidal oat flour, hydrolyzed collagen, hydrolyzed wheat protein, giant alga extract, allantoin, pansy extract and chlorella fermentation product.
The colloidal oat flour can reduce the irritation of tightening cream, can relieve the itching symptom of skin, and is used for diminishing inflammation, relieving itching and relieving erythema.
Wherein, allantoin can reduce the adhesion of keratinocytes, accelerate the renewal of epidermal cells, enhance the repair ability of skin, and has high safety.
Wherein, manganese chloride can imitate superoxide dismutase in vivo, can remove superoxide anions and other oxidation molecule precursors, and can delay skin aging and improve skin health state when used for the tightening cream.
In order to further improve the efficacy of the tightening cream, the tightening cream also comprises a sensitivity-relieving agent. The skin can be calmed by adding the sensitivity-soothing agent, so that the face skin injury red swelling can be relieved to a certain extent. The addition amount of the sensitivity-relieving agent is 0.01-5% based on the total mass of the tightening cream. Specifically, the addition amount of the sensitivity-relieving agent can be 0.1-4%, can be 0.2-3%, can be 0.3-2% and the like. When the addition amount of the sensitivity-relieving agent is less than 0.01%, the corresponding effect cannot be achieved; when the addition amount of the sensitivity-relieving agent is more than 5%, the cost is excessively high.
In the application, the sensitivity-relieving agent comprises one or more than two of Hamamelis virginiana water, stearyl glycyrrhetinate, bisabolol, ginger root extract and aloe extract.
The antioxidant is added in an amount of 0.01 to 2% by weight based on the total mass of the tightening cream, for example: the antioxidant may be added in an amount of 0.1%, 0.3%, 0.5%, 0.8%, 1.0%, 1.2%,1.5%, 1.8%, etc. The application can remove free radical by adding proper amount of antioxidant, protect skin, reduce skin injury caused by ultraviolet rays, promote wound healing, prevent inflammation and prevent rough skin from chapping. The antioxidant may be one or more of tocopherol acetate, butylhydroxytoluene, lycopene, etc.
The adding amount of the pH regulator is 0.01-1% based on the total mass of the tightening cream; the chelating agent is added in an amount of 0-1%. The pH regulator comprises one or more than two of aminomethylpropanol, arginine, citric acid, sodium citrate, sodium hydroxide and the like. The chelating agent may be EDTA-2Na and/or EDTA-4Na, etc.
In addition, the preservative in the tightening cream of the application is added in an amount of 0.01-1.5% based on the total mass of the tightening cream; the addition amount of the aromatic is 0.01-1%. The preservative may include one or a combination of two or more of phenoxyethanol, methylparaben, propylparaben, benzoic acid, and salts thereof. The aromatic may be essence, etc.
<Third aspect of the application>
A third aspect of the present application provides a method of preparing the tightening cream of the second aspect. The method includes the step of mixing the components of the tightening cream.
Specifically, the preparation method of the tightening cream comprises the following steps:
1. adding oil, part of thickener, emulsifier, part of humectant, sensitivity-relieving agent, antioxidant, part of antiseptic, and aromatic into oil phase pot, stirring and heating to 75-85deg.C to dissolve thoroughly;
2. adding part of humectant, part of penetration enhancer, optionally chelating agent, pH regulator, part of skin conditioner, and part of thickener into emulsifying pot, stirring and heating to 75-85deg.C to dissolve thoroughly;
3. slowly pumping the oil phase substances in the oil phase pot to an emulsifying pot, stirring, homogenizing, emulsifying in vacuum, and keeping the temperature of the emulsifying pot at 75-85 ℃;
4. cooling to 40-50deg.C, adding the rest humectant, rest penetration enhancer, rest thickener, collagenase inhibitor, rest skin conditioner and rest antiseptic, and stirring;
5. cooling to 30-40deg.C, discharging, and standing for 12-48 hr;
6. and after the inspection is qualified, sub-packaging and packaging, inspecting again, and warehousing the finished product.
Examples
Embodiments of the present application will be described in detail below with reference to examples, but it will be understood by those skilled in the art that the following examples are only for illustrating the present application and should not be construed as limiting the scope of the present application. The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
Extract of red pomegranate rind: to the state market exhibition macro biotechnology limited company;
grapefruit extract: and is available from the state market exhibition macro biotechnology limited company.
Comparative examples 1 to 5
Providing extract of pericarpium Granati as collagenase inhibitor. The pomegranate rind extract was dissolved in 5 groups of deionized water of different volumes to obtain 5 groups of test solutions, the concentrations of the 5 groups of test solutions being 4000 μg/mL, 3200 μg/mL, 2400 μg/mL, 1600 μg/mL, 800 μg/mL, respectively. The logarithmic mass concentration of the extract of guava skin is shown in table 2 and fig. 1 below.
Comparative examples 6 to 10
A grapefruit extract is provided as collagenase inhibitor. The grapefruit extract was dissolved in 5 deionized water groups of a volume corresponding to comparative examples 1-5 to obtain 5 test solutions, and the concentrations of the 5 test solutions were 4000. Mu.g/mL, 3200. Mu.g/mL, 2400. Mu.g/mL, 1600. Mu.g/mL, 800. Mu.g/mL, respectively. The logarithmic mass concentrations of grapefruit extract are shown in table 2 and fig. 2 below.
Examples 1 to 5
Providing extract of pericarpium Granati and extract of grapefruit as collagenase inhibitor. The collagenase inhibitor is obtained by mixing the extract of pericarpium Granati and the extract of grapefruit in a mass ratio of 3:1 (example 1), 2:1 (example 2), 1:1 (example 3), 1:2 (example 4), and 1:3 (example 5). The collagenase inhibitors of examples 1-5 were dissolved in 5 sets of deionized water corresponding to comparative examples 1-5, respectively. Examples 1 to 5 can give 5 sets of test solutions of corresponding concentrations to comparative examples 1 to 5. Wherein the content (mass%) of the guava skin extract and the grapefruit extract in the collagenase inhibitor is shown in table 1 below, and the logarithmic mass concentration of the collagenase inhibitor is shown in table 3 below.
TABLE 1
Assay for inhibition of collagenase Activity
The Fu Lin Fen reagent can be reduced to blue by phenols (molybdenum blue and tungsten blue mixture) under alkaline condition, and the protein and its hydrolysate can be reacted due to amino acids containing phenol group (such as tyrosine, tryptophan, etc.) in protein molecule, so that the principle can be used for measuring proteaseVitality. In general, casein is used as substrate, under the condition of a certain pH value and temperature, the casein is hydrolyzed by collagenase, after a period of time, the enzymolysis reaction is stopped by trichloroacetic acid, after the casein precipitate is removed by centrifugation or filtration, the supernatant is taken, and Na is used 2 CO 3 Alkalizing, adding Fu Lin Fen reagent to develop color, and measuring the blue color in proportion to the tyrosine amount of the product in the filtrate at 650nm wavelength by a spectrophotometer to calculate the activity of collagenase.
In the test, collagenase was used as matrix collagenase (MMP-1), purchased from: shanghai ze Biotechnology Co., ltd.
Collagenase activity is measured as collagenase activity that catalyzes the production of tyrosine from casein. The method comprises the following steps:
(1) taking 1 test tube, respectively adding 0.25mL of deionized water and 0.25mL of collagenase (32U/mL), then adding 0.5mL (1.0 percent, w/v) of substrate casein solution, immediately mixing, carrying out water bath heat preservation for 10min at 37 ℃, then adding 1mL (6.5 percent, w/v) of trichloroacetic acid solution, mixing uniformly, standing for 10min, centrifuging at 10000rpm for 5min, taking 0.5mL of supernatant sample in the test tube in another test tube, respectively adding 0.5mL (mass concentration: 10 percent) of sodium bicarbonate test solution, and shaking uniformly. After 10 minutes, 0.5ml of Fu Lin Fen test solution (diluted 2 times of Fu Lin Fen test solution with 1mol/L acid concentration) is added respectively, and the mixture is immediately mixed and left at room temperature for 30 minutes; the supernatant 1 of the test group was obtained, and absorbance was measured at a wavelength of 650nm and designated as A1.
(2) Taking 1 test tube, adding deionized water 0.25mL and collagenase 0.25mL (32U/mL) respectively, then adding trichloroacetic acid solution 1mL (6.5%, w/v) and immediately mixing uniformly, carrying out water bath heat preservation for 10min at 37 ℃, then adding substrate casein solution 0.5mL (1.0%, w/v) and mixing uniformly, standing for 10min, centrifuging at 10000rpm for 5min, taking supernatant sample 0.5mL in the test tube into another test tube, adding sodium bicarbonate test solution 0.5mL (mass concentration: 10%) respectively, and shaking uniformly. After 10 minutes, 0.5ml of Fu Lin Fen test solution (diluted 2 times of Fu Lin Fen test solution with 1mol/L acid concentration) is added respectively, and the mixture is immediately mixed and left at room temperature for 30 minutes; control supernatant 2 was obtained, and absorbance was measured at a wavelength of 650nm and designated as A2.
(3) 0.25mL (32U/mL) of collagenase is added into 35 test tubes respectively, then 0.25mL of the test solutions of comparative examples 1-10 and examples 1-5 are added respectively and mixed evenly, then 0.5mL (1.0 percent, w/v) of substrate casein solution is added and mixed evenly immediately, after water bath heat preservation is carried out for 10min at 37 ℃, 1mL (6.5 percent, w/v) of trichloroacetic acid solution is added and mixed evenly, after standing for 10min, centrifugation is carried out for 5min at 10000rpm, 0.5mL of supernatant fluid sample in 35 test tubes is taken into 35 other test tubes respectively, and 0.5mL (mass concentration: 10 percent) of sodium bicarbonate test solution is added respectively and mixed evenly. After 10 minutes, 0.5ml of Fu Lin Fen test solution (diluted 2 times of Fu Lin Fen test solution with 1mol/L acid concentration) is added respectively, and the mixture is immediately mixed and left at room temperature for 30 minutes; 35 experimental group supernatants 3 were obtained, each absorbance was measured at a wavelength of 650nm and designated A3.
(4) 0.25mL (32U/mL) of collagenase is added into 35 test tubes respectively, then 0.25mL of the test solutions of comparative examples 1-10 and examples 1-5 are added respectively and mixed evenly, then 1mL (6.5%, w/v) of trichloroacetic acid solution is added and mixed evenly immediately, after water bath heat preservation is carried out for 10min at 37 ℃, 0.5mL (1.0%, w/v) of substrate casein solution is added and mixed evenly, after 10min standing, centrifugation is carried out for 5min at 10000rpm, 0.5mL of supernatant fluid samples in 35 test tubes are taken into 35 other test tubes respectively, and 0.5mL (mass concentration: 10%) of sodium bicarbonate test solution is added respectively and shaken evenly. After 10 minutes, 0.5ml of Fu Lin Fen test solution (diluted 2 times of Fu Lin Fen test solution with 1mol/L acid concentration) is added respectively, and the mixture is immediately mixed and left at room temperature for 30 minutes; 35 control supernatants 4 were obtained, each absorbance detected at a wavelength of 650nm, designated A4.
Inhibition ratio = [1- (A3-A4)/(A1-A2) ] ×100%
Wherein: a1 is absorbance of supernatant 1 of the experimental group without collagenase inhibitor;
a2 is absorbance of supernatant 2 of control group without collagenase inhibitor;
a3 is absorbance of supernatant 3 of the experimental group containing collagenase inhibitor;
a4 is absorbance of supernatant 4 of control group containing collagenase inhibitor.
The inhibition ratios of collagenase activities by each of the extract of guava (comparative examples 1 to 5) and the extract of grapefruit (comparative examples 6 to 10) were calculated. And combining logarithmic mass concentration-collagenThe relation of enzyme activity inhibition ratio (FIG. 1 and FIG. 2) was calculated to obtain the corresponding mass concentration (IC) when the inhibition ratio of the extract of guava skin was 50% 50A ) And the mass concentration (IC) corresponding to 50% inhibition rate of grapefruit extract 50B ) The results are shown in Table 2.
TABLE 2
The collagenase activity inhibition rate of the collagenase inhibitors of examples 1 to 5 was then measured. And combining the relationship graph (figure 3) of logarithmic mass concentration and collagenase activity inhibition ratio, and obtaining the equivalent inhibition ratio (50%) by the combined action of the pericarpium Granati extract and the grapefruit extract by conversion, wherein the mass concentration (IC) 50a ) The mass concentration of the grapefruit extract ((IC) when the combination of the pomegranate rind extract and the grapefruit extract produces an equivalent inhibition rate (50%) 50b ) The results are shown in Table 3.
The effect of the complex action of the extract of pericarpium Granati and the extract of grapefruit can be evaluated by the interaction coefficient γ, and the specific results are shown in table 3.
γ=IC 50a /IC 50A +IC 50b /IC 50B
Wherein the IC 50A Representing the corresponding mass concentration when the inhibition rate of the pomegranate rind extract is 50%;
IC 50B represents the corresponding mass concentration when the inhibition rate of the grapefruit extract is 50%;
IC 50a representing the mass concentration of the pomegranate rind extract when the equivalent inhibition rate (50%) is generated by the combination of the pomegranate rind extract and the grapefruit extract;
IC 50b the mass concentration of the grapefruit extract is shown when the combination of the pomegranate rind extract and the grapefruit extract produces an equivalent inhibition rate (50%).
Wherein γ=1, representing that the extract of pericarpium Granati and the extract of grapefruit exhibit a simple additive effect; gamma < 1 is that the extract of the red pomegranate rind and the extract of the grapefruit show a synergistic effect, and the smaller the gamma value is, the stronger the synergistic effect is; gamma > 1 is that the extract of pericarpium Granati and the extract of grapefruit show antagonistic effect, and the larger the gamma value is, the larger the antagonistic effect is.
TABLE 3 Table 3
Note that: in Table 3, examples 1 and 2 are presented in the present application as reference examples 1 and 2, which can be contrasted with examples 3-5.
As can be seen from table 3, the interaction coefficient in the collagenase inhibitor of the present application is less than 1, and the interaction coefficient thereof may be 0.8 or less, and even 0.7 or less, so that the extract of pericarpium Granati and the extract of grapefruit may exhibit excellent synergistic effects.
Application examples 1 to 5
The contents (mass percent) of the components in the formulations of the tightening creams of application examples 1 to 5 in the following Table 4 were prepared according to the following production process steps. The production process comprises the following steps:
1. adding the phase A raw material into an oil phase pot, stirring and heating to 80-85 ℃ to fully dissolve the phase A raw material;
2. adding phase B into emulsifying pot, stirring and heating to 80-85deg.C to dissolve thoroughly;
3. slowly pumping the oil phase substances in the oil phase pot to an emulsifying pot, stirring, homogenizing, emulsifying in vacuum, and keeping the temperature of the emulsifying pot at 80-85 ℃;
4. cooling to 42 ℃, adding the phase C and the phase D, and uniformly stirring;
5. cooling to 37 ℃, discharging, and standing for 24 hours;
6. and after the inspection is qualified, sub-packaging and packaging, inspecting again, and warehousing the finished product.
Note that: a, B, C, D phases in the process are respectively
Phase A: isopropyl myristate, cyclomethicone, caprylic/capric triglyceride, oleyl erucate, cyclohexasiloxane, polyglycerol-3 methyl glucose distearate, shea butter, dimethicone, a complex of polyacrylamide and laureth-7 and C13-14 isoparaffins, C12-15 alcohol benzoate, a complex of PEG-100 stearate and glyceryl stearate, ceramide 2, tocopheryl acetate, olive oil unsaponifiables, glyceryl polyacrylate, ammonium acryloyldimethyl taurate/VP copolymer, stearyl glycyrrhetinate, butylhydroxytoluene, methylparaben, propylparaben, perfume;
and B phase: water, glycerol, propylene glycol, panthenol, betaine, aminomethylpropanol, colloidal oat flour, allantoin, carbomer, and manganese chloride;
and C phase: polyethylene glycol-90M, butylene glycol;
and D phase: pomegranate rind extract, grapefruit extract, phenoxyethanol, lactobacillus/soybean fermentation product extract, bis-diethoxydiglycol cyclohexane 1, 4-dicarboxylate.
Wherein glycerol, panthenol, betaine, glycerol polyacrylate and butanediol are humectant;
isopropyl myristate, cyclomethicone, caprylic/capric triglyceride, oleyl erucate, cyclohexasiloxane, butter fruit, dimethicone, C12-15 alcohol benzoate, olive oil unsaponifiable matter is oil;
polyethylene glycol-90M, ammonium acryloyldimethyl taurate/VP copolymer, carbomer are thickeners;
the extract of pericarpium Granati and the extract of grapefruit are collagenase inhibitor;
the complex of polyglycerol-3 methyl glucose distearate, polyacrylamide and laureth-7 and C13-14 isoparaffin, PEG-100 stearate and glyceryl stearate are emulsifiers;
ceramide 2, lactobacillus/soybean fermentation product extract, colloidal oat flour, allantoin, manganese chloride are skin conditioners;
propylene glycol, bis-diethoxydiglycol cyclohexane 1, 4-dicarboxylate are permeation promoters;
stearyl glycyrrhetinate is a allergy-relieving agent; butylated hydroxytoluene, tocopheryl acetate are antioxidants;
phenoxyethanol, methylparaben and propylparaben are preservatives;
aminomethylpropanol is a pH adjuster; the essence is a fragrance.
PEG-100 stearate and glyceryl stearate, manufacturer, heda, trade name: arlael 165;
the manufacturer of the composite of polyacrylamide and laureth-7 and C13-14 isoparaffin is Sepick under the trademark Sepigel 305.
Comparative examples 1 to 8 were used
The contents (mass percent) of each component in the formulations of the tightening creams of comparative examples 1 to 8 were prepared according to the application in the following table 5, and the tightening creams were prepared in the same manner as in application examples 1 to 5.
TABLE 4 Table 4
TABLE 5
Skin elasticity test
Skin elasticity test method: the test principle is based on suction and stretching, and the suction pressure generated on the surface of the tested skin sucks the skin into a specific test probe, and the depth of the skin sucked into the test probe is measured by a non-contact optical test system. The test probe includes a light emitter and a light receiver, and the ratio of light (the ratio of emitted light to received light) is proportional to the depth of skin drawn into the probe, thus obtaining a plot of the length of skin stretched versus time.
Measuring skin elasticity of a subject by using a probe PVM600 of German CK company and a skin elasticity measuring instrument MPA580, selecting a parameter R2 as a comparison index (R2: the ratio of the skin rebound amount without negative pressure to the maximum stretching amount with negative pressure is closer to 1, the better the skin elasticity is), measuring 3 times in total, and taking an average value; the improvement of skin elasticity in the test area by the product was evaluated by measuring the change in skin elasticity value R2 before and after use of the product.
The number of subjects was 33, the test period was 8 weeks, the application of the tightening creams of examples 1 to 5 and the application of the tightening creams of comparative examples 1 to 8 were selected as test samples, 13 different areas were divided in the forearm of the subjects, the tightening creams of examples 1 to 5 and the application of the tightening creams of comparative examples 1 to 8 were applied to different areas on the inner side of the forearm every morning and evening, and the application amount was about 2mg/cm 2 The application position of each test sample in the test period was kept unchanged, and the skin elasticity of the test area before the test and 8 weeks of use was measured, so as to characterize the change rate of the skin elasticity, and the results of specific elasticity change rate (averaged) are shown in table 6 and fig. 5.
TABLE 6
As can be seen from table 6 and fig. 5, the application examples 1 to 5 of the present application have a large rate of change in elasticity, i.e., skin elasticity is enhanced, and thus, the use of the extract of guava skin and the extract of grapefruit can effectively improve skin aging.
The skin elasticity change rate of the present application was small in the application comparative examples 1 to 8, and thus the anti-aging effect of the application comparative examples 1 to 8 was relatively poor.
The above examples of the present application are merely illustrative of the present application and are not intended to limit the embodiments of the present application. Other variations or modifications of the above teachings will be apparent to those of ordinary skill in the art. It is not necessary here nor is it exhaustive of all embodiments. Any modification, equivalent replacement, improvement, etc. which come within the spirit and principles of the application are desired to be protected by the following claims.
Claims (11)
1. A tightening cream, characterized by comprising a collagenase inhibitor and a penetration enhancer, wherein the addition amount of the collagenase inhibitor is 0.01-10% based on the total mass of the tightening cream; the addition amount of the penetration enhancer is 0.01-10%;
the collagenase inhibitor comprises extract of pericarpium Granati and extract of grapefruit; the addition amount of the pomegranate rind extract is 15-65% by weight of the total mass of the collagenase inhibitor, and the addition amount of the grapefruit extract is 35-85%;
the mass ratio of the pomegranate rind extract to the grapefruit extract is 1:0.6-3;
the penetration enhancer comprises one or more of propylene glycol, bis-diethoxydiglycol cyclohexane 1, 4-dicarboxylic acid ester and chitosan.
2. The tightening cream of claim 1, wherein the collagenase is interstitial collagenase.
3. The tightening cream according to claim 1 or 2, characterized in that the mass ratio of the extract of the peel of red pomegranates to the extract of grapefruits is 1:0.8-3.
4. The tightening cream according to claim 3, wherein the mass ratio of the extract of guava skin to the extract of grapefruit is 1:1-3.
5. The tightening cream according to claim 4, wherein the mass ratio of the extract of guava skin to the extract of grapefruit is 1:1.2-3.
6. The tightening cream according to claim 5, wherein the mass ratio of the extract of guava skin to the extract of grapefruit is 1:1.5-3.
7. The tightening cream according to claim 6, wherein the mass ratio of the extract of guava skin to the extract of grapefruit is 1:1.8-3.
8. The tightening cream according to claim 1 or 2, further comprising one or a combination of two or more of a humectant, a thickener, a pH adjuster, a grease, a preservative, a skin conditioner, an emulsifier, a sensitivity-soothing agent, a chelating agent, a fragrance, and an antioxidant; wherein,,
the addition amount of the humectant is 0.01-20%; the addition amount of the thickener is 0.02-5%; the addition amount of the pH regulator is 0.01-1%; the addition amount of the grease is 10-30%; the addition amount of the preservative is 0.01-1.5%; the addition amount of the skin conditioning agent is 0.01-5%; the addition amount of the emulsifier is 0.01-5%; the addition amount of the sensitivity-relieving agent is 0.01-5%; the addition amount of the antioxidant is 0.01-2%; the addition amount of the aromatic is 0.01-1%; the chelating agent is added in an amount of 0-2%.
9. The tightening cream of claim 8, wherein the skin conditioning agent comprises one or more of manganese chloride, tapioca starch, ceramide 2, lactobacillus/soybean fermentation product extract, palmitoyl tripeptide-5, acetyl hexapeptide-8, palmitoyl oligopeptide, colloidal oat flour, hydrolyzed collagen, hydrolyzed wheat protein, kelp extract, allantoin, pansy extract, and chlorella fermentation product.
10. The tightening cream of claim 8, wherein the sensitivity-relieving agent comprises one or a combination of more than two of hamamelis water, stearyl glycyrrhetinate, bisabolol, ginger root extract, aloe vera extract.
11. A method of preparing a tightening cream according to any one of claims 1 to 10, comprising the step of mixing the components of the tightening cream.
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CN107951769A (en) * | 2017-12-08 | 2018-04-24 | 广州赛莱拉干细胞科技股份有限公司 | Anti-aging face cream and preparation method and application thereof |
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JPH09110710A (en) * | 1995-10-24 | 1997-04-28 | Ichimaru Pharcos Co Ltd | Dermal preparation for external use and bathing agent |
JPH11137224A (en) * | 1997-11-13 | 1999-05-25 | Ogawa Koryo Co Ltd | Agent for inhibiting deterioration of flavor and taste |
CN102448434A (en) * | 2009-08-17 | 2012-05-09 | 沈宝美 | Composition for preventing and treating different types of wrinkles depending on physical morphology |
CN105963182A (en) * | 2016-05-30 | 2016-09-28 | 李建东 | Clear nourishing skin-softening mask solution and preparing method thereof |
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