CN110742842B - Essence composition for delaying skin aging and preparation method thereof - Google Patents

Essence composition for delaying skin aging and preparation method thereof Download PDF

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CN110742842B
CN110742842B CN201911105273.1A CN201911105273A CN110742842B CN 110742842 B CN110742842 B CN 110742842B CN 201911105273 A CN201911105273 A CN 201911105273A CN 110742842 B CN110742842 B CN 110742842B
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喻敏
王婷婷
欧阳小文
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Yimei Biotech Shanghai Co ltd
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Abstract

The invention discloses an essence composition for delaying skin aging and a preparation method thereof, belonging to the technical field of cosmetics, and the essence composition comprises the following technical key points: an essence composition for delaying skin aging comprises cetyl N-palmitoyl hydroxyproline, p-hydroxyacetophenone, tocopherol, astaxanthin, ginger root extract, acetyl hexapeptide-8, hydrolyzed collagen, carnosine, compound ceramide, thickener, humectant, skin conditioner, emollient, and water. The compound ceramide is selected from one or more of ceramide 3, ceramide 6II, ceramide 1 and ceramide 2. The invention is safe and convenient to operate, can delay skin aging, promote collagen generation, improve skin fullness, increase stratum corneum moisture content, and has good anti-aging effect.

Description

Essence composition for delaying skin aging and preparation method thereof
Technical Field
The invention belongs to the technical field of cosmetics, and particularly relates to an essence composition for delaying skin aging and a preparation method thereof.
Background
With the development of economy and the continuous improvement of living standard of people, the pursuit of the youth of faces is the expectation of the elder people, and the pursuit of women for life is continuous, and the pursuit of women for life is the career for fighting for life.
Facial aging is not a sudden, cumulative process in which the facial skin and structures are constantly changing by extrinsic and intrinsic effects, such as: thickening and aging of epidermis, reduction of water content of epidermis, generation of color spots, drooping of eyelids and cheeks, generation of raised lines, fishtail lines, and stature lines, etc. The manifestation of such facial aging is influenced by several major factors, in addition to the limitation of the life span of stem cells by individual genetic genes.
First, facial muscles are not distributed continuously, but are regionally distributed in a lump. The muscle groups include forehead, eye periphery, nasal wing, cheek, lip periphery, etc. We know that above the muscle is the fat layer, then the dermal collagen layer, the epidermal layer. In the infant period, the whole face is relatively uniform in the process of establishing facial motor muscles, and mainly consists of epidermis, dermis and subcutaneous fat. With age and facial expression, the connective muscles develop gradually. Since muscles are not continuous but massive, discontinuities in the facial contour occur with age. The aging characteristics of the face such as lower eye sagging, cheek bulging, cheek sagging and lip muscle dislocation, facial wrinkle generation and the like gradually appear along with the aging of the face, and the aging is remarkable in that the aging is represented by aging in a block type, and the face loses the smoothness and smoothness.
Second, the second important factor affecting the aging process of the face is ultraviolet rays. The american dermatologist Albert Kligman suggested that "photoaging is a chronic skin disorder" is a high generalization of photoaging. Ultraviolet rays, particularly UVA ultraviolet rays with the wavelength of 320-400nm, can reach the dermis, can activate melanocytes, promote skin blackening and color spot formation, damage Langerhans immune cells, reduce the immunity of the skin, damage fibroblasts, reduce the collagen generation capacity of endoplasmic reticulum of cells, cannot supplement new collagen, influence the fullness and elasticity of the dermis, and cause irreversible wrinkles after long-term development.
Thirdly, the third important influencing factor of the facial aging process is the reduction of the filling degree of the cuticle and the reduction of the water content. The moisture content of the infant cuticle is as high as 60%, and the moisture content of the infant cuticle is reduced to below 30% and even below 10% for adults. In the aging development process, the synthesis of lipid among epidermal cells is reduced, the expression of aquaporin-3 is reduced, the synthesis capacity of hyaluronic acid is reduced, the water content of stratum corneum is reduced, the skin lacks the filling degree, the related cell biological functions of the epidermis are also reduced, the appearance of the skin is rough and not fine, and the generation of fine wrinkles is further initiated.
However, the existing facial essence composition, such as a composition for promoting skin collagen production with publication number CN109260454A, is prepared by a method comprising two components, i.e. a component a and a component b; the component A is an oral preparation and comprises the following raw materials in parts by weight: vitamin C1-2 parts, collagen peptide 4-6 parts, traditional Chinese medicine extract 12-15 parts, sustained-release gel 1-2 parts, and deionized water 10-12 parts; the component B is an injection preparation and comprises calcium hydroxyapatite and physiological saline, and the mass ratio of the calcium hydroxyapatite to the physiological saline is 1: 8-12; the mass ratio of the first component to the second component is 10: 3-4. Said invention uses oral preparation to attain the goal of whitening, moistening skin and resisting senility, and utilizes subcutaneous injection to possess biological potential, attract fibroblast to enter and produce new collagen, and make them supplement each other to promote generation of skin collagen.
The main purpose of the invention is to generate collagen, but the component B needs to meet the requirement of hypodermic injection, so the cost is high, the operation difficulty is high, and an operator can hardly perform hypodermic injection operation by himself; if the subcutaneous injection is performed by self operation, bacteria can be easily infected, and even some accidents such as tetanus occur, so a new technical scheme needs to be proposed to solve the problems.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide the essence composition for delaying skin aging, which is safe and convenient to operate, can delay skin aging, promote the generation of collagen, improve the fullness of skin, increase the moisture content of stratum corneum and has good anti-aging effect.
In order to achieve the purpose, the invention provides the following technical scheme: the essence composition for delaying skin aging comprises the following components in parts by weight:
Figure BDA0002270367160000021
Figure BDA0002270367160000031
the compound ceramide is selected from one or more of ceramide 3, ceramide 6II, ceramide 1 and ceramide 2.
Further, the compound ceramide comprises 0.005-0.05 part of ceramide 3, 0.0025-0.025 part of ceramide 6II, 0.000005-0.00005 part of ceramide 1 and 0.004-0.08 part of ceramide 2.
By adopting the technical scheme, the astaxanthin is one of carotenoids, belongs to a fat-soluble and water-soluble pigment, and is a strong natural antioxidant. The chemical name of the astaxanthin is 3, 3 '-dihydroxy-4, 4' -diketone-beta, and the chemical formula is as follows: c 40 H 52 O 4 . The special molecular structure of astaxanthin can penetrate through the outer wall of human cells, directly remove oxygen free radicals in the cells, enhance the regeneration capacity of the cells, maintain the functional balance of the human body, reduce the accumulation of aged cells and protect the health of the cells and DNA from inside to outside. The strong antioxidant property of astaxanthin makes it a potential photo-protecting agent, effectively scavenging free radicals which cause skin aging, protecting cell membranes and mitochondrial membranes from oxidative damage, and preventing skin photo-aging. Therefore, astaxanthin has effects of preventing ultraviolet radiation, preventing skin photoaging, enhancing body metabolism, and improving immunityHas antiaging effect. The ginger root extract is concentrated solution with biological active components extracted from ginger, and has the functions of enhancing immunity, resisting bacteria, killing pests and diminishing inflammation.
Ceramide naturally exists in the intercellular substance of stratum corneum, plays a key role in the physiological function of stratum corneum, makes the skin smooth and delicate, and prevents the skin from drying due to water loss; meanwhile, ceramide is also involved in various physiological processes such as cell differentiation. The compounded ceramide is a composite product of various ceramides (such as ceramides 1-3), and the cetyl N-palmitoyl hydroxyproline is synthetic ceramide (namely ceramide-like), can overcome the defects of natural ceramide, and has a structure similar to that of the natural ceramide. The cetyl N-palmitoyl hydroxyproline has the effects of moisturizing and removing fine lines, and can effectively repair the skin and play a role in skin barrier when being matched with the compound ceramide.
Moisturizers are hydrophilic skin moisturizing substances that have the ability to bind water in the lower humidity range, moisturize the skin, and they can help maintain the skin in a more than normal equilibrium moisture content by controlling the exchange of moisture between the product and the surrounding air, and thus, reduce skin dryness.
Acetyl hexapeptide-8 is also called as ayurrin, is a neurotransmitter inhibitory peptide, and has high anti-wrinkle activity and small side effect. The anti-wrinkle mechanism is as follows: acetyl hexapeptide-8 is involved in competing for the site of SNAP-25 at the vacuolar complex, thereby affecting complex formation; when the vesicle complex is slightly unstable, the vesicle cannot effectively release neurotransmitters, thereby causing the reduction of muscle contraction and preventing the formation of wrinkles.
The hydrolyzed collagen is small molecular weight collagen (the molecular weight collagen is collagen with the molecular weight of less than 1500 daltons) which is subjected to hydrolysis treatment, is very easy to absorb, can fully meet the requirements of human bodies on repairing skin and connective tissues, and has the effects of inhibiting melanin, whitening skin, delaying aging, improving microcirculation, removing freckles and wrinkles, tightening skin, repairing fine wrinkles and the like.
The p-hydroxyacetophenone is prepared by acetic acid and phenyl vinegar through aluminum trichloride catalytic rearrangement, plays a role of an antioxidant in cosmetics, while the tocopherol is a product obtained after vitamin E hydrolysis and is one of the most main antioxidants, and the antioxidant effect of the tocopherol, the p-hydroxyacetophenone, the astaxanthin and the ginger root extract can be further improved through compound use.
Further, CERAMIDE 3 is known under the English name CERAMIDE 3, and has the CAS number 100403-19-8. Ceramide 3 is a lipid substance, an artificially synthesized component, has a structure similar to that of a substance constituting the horny layer of the skin, can quickly permeate into the skin, helps the renewal of the natural protective layer of the skin, can promote the balance of natural hydration, and is combined with water in the horny layer to form a network structure to lock water. The skin moisturizing and repairing cream has good effects on skin moisturizing and repairing, is an important skin activating component in the horny layer, and can strengthen the skin barrier, rebuild cells and form an effective barrier to prevent water loss and reduce the influence of the external environment. More ceramide is particularly needed in irritated skin and it has been shown that rubbing a product containing a ceramide component reduces redness and swelling and loss of moisture through the skin, acting to enhance the skin barrier and help the damaged skin to relieve dry conditions.
The English name of CERAMIDE 2 is CERAMIDE 2, and the CAS number of the CERAMIDE is 100403-19-8. The ceramide 2 has the functions of serving as a skin conditioner, an antioxidant and a humectant in cosmetics, can improve a sebum membrane and inhibit the secretion of active sebaceous glands, enables the skin to be balanced in water and oil, enhances the self-protection function of the skin, is similar to the ceramide 1, and is more suitable for the young skin which is greasy and has requirements. The composition has good effects in moisturizing and repairing skin, is an important skin-activating component in horny layer, and can enhance skin barrier and rebuild cells. More ceramide is particularly needed in irritated skin, and it has been shown that rubbing products containing ceramide components can reduce redness and swelling and loss of moisture through the skin, and act to increase the skin barrier.
CERAMIDE 1 is known by the English name CERAMIDE 1, and has the CAS number of 100403-19-8. Ceramide 1 is used as skin conditioner and humectant in cosmetic, and can intensively repair natural sebum membrane of skin, strengthen defense function of skin surface barrier, and reduce water evaporation and loss, and is suitable for all skin types.
CERAMIDE 6II has the English name of CERAMIDE 6II and the CAS number of 100403-19-8. Ceramide 6II has effects of skin conditioner, antioxidant and humectant in cosmetics, and can inhibit secretion of active sebaceous gland while improving sebaceous membrane, normalize skin natural exfoliation process by skin scale exfoliation, balance skin water and oil, and enhance skin self-protective function similar to ceramide 1, and is suitable for oily and desired young skin. The composition has good effects in moisturizing and repairing skin, is an important skin-activating component in horny layer, and can enhance skin barrier, rebuild cells, and form an effective barrier to prevent water loss and reduce the influence of external environment. More ceramide is particularly needed in irritated skin, and it has been shown that rubbing a serum composition (i.e., product) containing ceramide components can reduce redness and skin moisture loss, and act to enhance the skin barrier and help the damaged skin to alleviate the dry state.
In conclusion, the added tocopherol, the p-hydroxyacetophenone, the astaxanthin and the ginger root extract provide strong oxidation resistance and effectively delay skin aging. Further, the added compound ceramide, ceramide-like compound and humectant are used in a matching way, so that the skin fullness is improved, and the moisture content of the horny layer is increased. Meanwhile, the added multiple polypeptides and hydrolyzed collagen effectively resist and supplement the loss of collagen, and have good anti-aging effect.
Further, the emollient is selected from one or more of cholesterol, caprylic/capric triglyceride, hexyldecanol, and campesterols.
By adopting the technical scheme, the cholesterol is also called cholesterol and is a derivative of cyclopentane multi-hydrogen phenanthrene. The cholesterol has excellent emulsifying, dispersing and lubricating capabilities. The caprylic/capric triglyceride (GROIL GTCC) is a odorless oil, and belongs to palm oil or coconut oil derivatives. Can be used as base material of moisturizing factor, cosmetic stabilizer, antifreezing agent, and homogenizing agent.
Hexyldecanol, also known as 2-hexyl-1-decanol, is a polyol. Has certain water-holding capacity in cosmetics, and can be used as humectant. And the English name of the rape sterols is: BRASSICA castestis (rapesed) STEROLS, Cas No: 90989-79-0. The campesterol is selected from emollient, skin conditioner, and humectant. The campesterol can be used as humectant with moisture keeping effect and anti-inflammatory effect.
In conclusion, the cholesterol, the caprylic/capric triglyceride, the hexyldecanol and the rape sterol are common emollients, not only can play a role in moisturizing, but also can form a structure similar to an oil film on human skin when the moisturizer is coated on the human skin, and the formed oil film is compounded with four kinds of ceramide to play a good role in skin barrier.
Further, the humectant is selected from one or more of ethylhexyl glycerin, butanediol, glycerin, sodium hyaluronate, 1, 2-pentanediol, 1, 2-hexanediol, and caprylyl glycol.
By adopting the technical scheme, the ethylhexyl glycerin, the butanediol, the glycerin, the sodium hyaluronate, the 1, 2-pentanediol, the 1, 2-hexanediol and the caprylyl glycol are common humectants, and various humectants can be matched with four ceramides and similar ceramides for use, so that the skin fullness is improved, and the moisture content of the horny layer is greatly increased.
Further, the preservative also comprises 0.02-0.2 part of a chelating agent, wherein the chelating agent is disodium EDTA.
By adopting the technical scheme, the EDTA disodium is a common chelating agent, and the EDTA disodium can play a role in chelating heavy metal ions, so that the phenomenon of skin heavy metal poisoning is effectively reduced.
Further, the inulin comprises 0.09-1.8 parts of inulin and 0.01-0.2 parts of brown algae extract.
Further, the main component of the brown algae extract is fucoidan.
By adopting the technical scheme, the inulin is reserve polysaccharide in plants and is water-soluble dietary fiber. Brown algae extract is a common bioactive substance (such as fucoidan sulfate) extracted from marine algae, and can help human cells to improve autophagy function and kill or consume dead cells. Wherein the fucoidan has immunomodulatory activity, and can be used for producing cytokine and chemokine by macrophage and splenocyte; meanwhile, the fucosan sulfate can also inhibit the production of active oxygen free radicals and promote the elimination of the active oxygen free radicals, and has obvious antioxidant activity. In conclusion, the prebiotics such as inulin and brown algae can form a biological film on the surface of skin, so that the skin micro-ecology can be effectively improved, and the skin is healthier.
Further, the thickening agent is selected from one or more of carbomer, xanthan gum, acrylic acid (ester)/C10-30 alkanol acrylate cross-linked polymer and polyacrylic acid.
By adopting the technical scheme, the carbomer is a pharmaceutic adjuvant and has no special side effect. The acrylic crosslinked resin obtained by crosslinking pentaerythritol and acrylic acid has important applications such as thickening and suspending. Xanthan gum is an extracellular microbial multi-pool produced by drunkenness of saccharides by xanthomonas. Due to the special structure and colloid characteristics of macromolecules, the product has multiple functions and can be used as an emulsifier, a stabilizer, a gel thickener and the like.
In addition, the acrylic acid (ester)/C10-30 alkanol acrylate cross-linked polymer is a film forming agent, can replace an emulsifier to be used in cosmetics, not only reduces the irritation effect of the emulsifier on skin, but also has good anti-irritation effect and good safety because the acrylic acid (ester)/C10-30 alkanol acrylate cross-linked polymer has larger molecular weight and can not be absorbed through skin. Polyacrylic acid is used as a binder, an emulsion stabilizer and a film forming agent in cosmetics.
Therefore, carbomer, xanthan gum, acrylic acid (ester)/C10-30 alkanol acrylate cross-linked polymer and polyacrylic acid are all the participating thickening agents, and can play a role in improving and increasing the viscosity of the essence composition.
Further, the skin conditioner is one or more selected from phytosphingosine, 4-tert-butylcyclohexanol, bisabolol, dipotassium glycyrrhizinate, beta-glucan, hydroxyphenylpropionamide benzoic acid, humic acid, and mineral salt.
Further, the beta-glucan can be oat beta-glucan-or highland barley beta-glucan.
By adopting the technical scheme, the phytosphingosine is a precursor of phospholipids (Ceramides), is relatively similar to skin lipids, and is an important component for water retention and barrier function. The phytosphingosine is one of important oil components in human epidermis, the phytosphingosine in the human skin is gradually reduced along with the increase of age and the aging period, so that dry skin and rough skin are caused, and the external phytosphingosine has the effects of efficiently keeping the skin soft and moist and protecting the cortex; the phytosphingosine has antibacterial and antiinflammatory effects, and can be used for preventing and treating skin diseases such as acne. While 4-tert-butylcyclohexanol is white needle-like or powdery crystal. It has patchouli-like fragrance of radix aucklandiae, and the active substance can effectively relieve sensitive skin, thereby inhibiting prickling and burning.
Furthermore, the beta-glucan may be oat beta-glucan-or highland barley beta-glucan. It can be used for keeping moisture, removing wrinkle, relieving inflammation, and promoting stratum corneum regeneration. The bisabolol is extracted from chrysanthemum plants, has the functions of resisting inflammation and inhibiting bacteria, has good stability and good compatibility with skin, reduces skin inflammation, relieves skin acne, prevents acne, improves the anti-irritation capability of the skin, repairs the skin with inflammation injury, and improves the SPF value in a sun-screening product. The bisabolol has obvious anti-inflammatory and antispasmodic effects, and on the function, the natural bisabolol has twice of the effects of a synthetic product, has the functions of relieving pain, alleviating irritation and resisting allergy, and has skin care effect on allergic skin or children skin. The bisabolol has high permeability on the skin cortex, and the action of the bisabolol is dozens of times of that of a common penetrant; can be used as main agent or adjuvant for preventing and treating skin diseases such as acne, and also has skin conditioning effect.
Therefore, the essence composition does not adopt common soothing agents, such as dipotassium glycyrrhizinate or hydroxyphenyl propionamide benzoic acid and the like, and meanwhile, the brown algae extract is extracted from natural plants, so that the raw materials are green and environment-friendly, and have no stimulation to skin and muscle of a human body. Meanwhile, the excellent activities of the brown algae extract and the fucoidan sulfate are combined, the production of active oxygen free radicals can be inhibited, the active oxygen free radicals can be cleared, the inflammation problems of skin allergy, redness and the like can be improved, and the skin can be repaired.
Humic acid is the main component of organic matter in natural water, and is mainly derived from low molecular weight components (for example, less than 1500 daltons) of soil humus and decomposition and lower plankton of aquatic plants, and the basic structure of the humic acid is aromatic ring and alicyclic ring, and the ring is connected with carboxyl, hydroxyl, carbonyl, quinonyl and methoxyl functional group. Due to the influence of various functional groups on the complexity of the molecular structure of the humic acid, the humic acid has a plurality of physical and chemical properties and has good colloid property, solubility, ion exchange property, adsorbability, precipitability, complexation, oxidation-reduction property and thermal stability. Because the water that uses in this application does not contain the halide, the humic acid that adds this moment can promote the good anti-oxidant of essence composition and accuse oily performance on the contrary. The mineral salt is a mineral component containing more than 70 trace elements, such as selenium element, magnesium element, zinc element, silicon element, calcium element, sodium element and the like, can supplement various trace element nutrients required by skin cells of the head, enhance the activity of the cells, improve the tolerance of the cells and improve the skin hydration, thereby being beneficial to prolonging the aging, providing prebiotics for skin microorganisms and maintaining the balance of skin biofilms.
In order to achieve the purpose, the invention provides the following technical scheme: a preparation method of a essence composition for delaying skin aging comprises the following operation steps:
step one, adding water into a water pot according to a ratio, starting stirring, sequentially adding the compound ceramide, the p-hydroxyacetophenone and the tocopherol into the water pot, and heating to 75-80 ℃.
And step two, premixing and dispersing the cross-linking agent, adding the cross-linking agent into a water pot, and homogenizing for 1-3 min.
And step three, sequentially adding the cetyl N-palmitoyl hydroxyproline and the emollient into an oil pan, and heating to 75-80 ℃ to obtain an oil pan mixture.
And step four, adding the oil pot mixture obtained in the step three into a water pot, homogenizing for 2-5min, stirring uniformly at the rotating speed of 3000 plus 5000r/min, and cooling.
And step five, cooling and stirring until the temperature in the water kettle is below 50 ℃, then adding the astaxanthin, the hydrolyzed collagen, the carnosine, the acetyl hexapeptide-8 and the ginger root extract while stirring, and homogenizing for 3-6min after the addition is finished.
And step six, continuously stirring, cooling to below 35 ℃, and detecting and discharging.
The thickening agent is added in two times and is respectively added in the first step and the third step; adding the skin conditioner part for three times, wherein the skin conditioner part is added in the first step, the third step and the fifth step respectively; and (4) adding the humectant in four times, wherein the humectant is added in the first step, the second step, the third step and the fourth step respectively.
Further, 0.02-0.2 parts of disodium EDTA is also added in the step one.
Further, in the fifth step, 0.09-1.8 parts of inulin and 0.01-0.2 parts of brown algae extract are added.
By adopting the technical scheme, the anti-aging cream is convenient to operate, is added according to a similar compatibility principle, increases the stability among the components, accelerates the dissolution of the components, can delay the skin aging, promotes the generation of collagen, improves the skin fullness, increases the moisture content of the stratum corneum and has good anti-aging effect.
In conclusion, the invention has the following beneficial effects:
1. the invention can delay skin aging, promote the generation of collagen, improve the skin fullness, increase the moisture content of the horny layer and has good anti-aging effect;
2. preferably, the cholesterol, the caprylic/capric triglyceride, the hexyldecanol and the brassinosteroids not only can play a role in moisturizing, but also can form a structure similar to an oil film on human skin when the cholesterol and the like are coated on the human skin, and the formed oil film is compounded with the four ceramides for use, so that a good skin barrier effect can be played.
3. The added tocopherol, p-hydroxyacetophenone, astaxanthin and ginger root extract provide strong oxidation resistance and effectively delay skin aging. Further, the added compound ceramide, ceramide-like compound and humectant are used in a matching way, so that the skin fullness is improved, and the moisture content of the horny layer is increased. Meanwhile, the added multiple polypeptides and hydrolyzed collagen effectively resist and supplement the loss of collagen, and have good anti-aging effect.
Drawings
FIG. 1 is a graph showing the change of the moisture content of the stratum corneum of the skin of test sample 4 and control samples 1 to 3 in a serum composition for delaying skin aging;
FIG. 2 is a diagram of the cell morphology observed under an inverted microscope, which is mainly represented by the cell morphology at the volume concentrations of blank control, 0.156%, 0.313%, 0.625%, 1.25%, and 2.5%, in this order;
FIG. 3 is a graph of cell viability for control sample 4 at different concentrations;
FIG. 4 is a bar graph of the measured amounts of collagen in the blank control, solvent control, and test sample 4, prepared according to the data in Table 5;
FIG. 5 is a line graph of the radical scavenging rates for test sample 4 and control samples 1-3, prepared according to the data of Table 7;
fig. 6 is a comparison of fine lines around four weeks in the canthus of two volunteers of test sample 4 in a skin aging delaying essence composition.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings.
First, an embodiment
Example 1: a essence composition for delaying skin aging comprises the components in parts by weight shown in Table 1.
The preparation method comprises the following operation steps:
step one, adding water into a water kettle according to the formula ratio in the table 1, starting stirring, sequentially adding ceramide 3, ceramide 6II, ceramide 1, ceramide 2, phytosphingosine, carbomer, xanthan gum, ethylhexylglycerin, butanediol, cholesterol, p-hydroxyacetophenone and tocopherol into the water kettle, and heating to 75 ℃.
And step two, premixing and dispersing the glycerol, the sodium hyaluronate and the acrylic acid (ester)/C10-30 alkanol acrylate cross-linked polymer, adding the mixture into a water pot, and homogenizing for 1 min.
And thirdly, sequentially adding caprylic/capric triglyceride, 1, 2-pentanediol, 4-tert-butylcyclohexanol, hexyldecanol, bisabolol, N-palmitoyl hydroxyproline cetyl ester, campesterol and polyacrylic acid into an oil pan, and heating to 75 ℃ to obtain an oil pan mixture.
And step four, adding the oil pot mixture obtained in the step three into a water pot, homogenizing for 2min at 5000r/min, and starting cooling.
And step five, cooling and stirring the water kettle to 50 ℃, sequentially adding astaxanthin, hydrolyzed collagen, carnosine, dipotassium glycyrrhizinate, beta-glucan, 1, 2-hexanediol, caprylyl glycol, inulin, brown algae extract, hydroxyphenylpropionamide benzoic acid, humic acid, mineral matter, acetyl hexapeptide-8 and ginger root extract, and homogenizing for 4min after the addition is finished.
And step six, continuously stirring, cooling to 35 ℃, and detecting and discharging.
TABLE 1 essential composition for delaying skin aging comprising the components of examples 1 to 6 in parts by weight
Figure BDA0002270367160000091
Figure BDA0002270367160000101
Example 2: a essence composition for delaying skin aging is different from that of example 1 in that: as shown in Table 1, the components were different in parts by weight.
The preparation method comprises the following operation steps:
step one, adding water into a water kettle according to the formula ratio in the table 1, starting stirring, sequentially adding ceramide 3, ceramide 6II, ceramide 1, ceramide 2, phytosphingosine, carbomer, xanthan gum, ethylhexylglycerin, butanediol, cholesterol, p-hydroxyacetophenone and tocopherol into the water kettle, and heating to 78 ℃.
And step two, premixing and dispersing the glycerol, the sodium hyaluronate and the acrylic acid (ester)/C10-30 alkanol acrylate cross-linked polymer, adding the mixture into a water pot, and homogenizing for 2 min.
And step three, sequentially adding caprylic acid/capric acid triglyceride, 1, 2-pentanediol, 4-tert-butylcyclohexanol, hexyldecanol, bisabolol, N-palmitoyl hydroxyproline cetyl esters, campesterol and polyacrylic acid into an oil pan, and heating to 78 ℃ to obtain an oil pan mixture.
And step four, adding the oil pot mixture obtained in the step three into a water pot, homogenizing for 3.5min at 4000r/min, and starting to cool.
And step five, cooling and stirring the water kettle to 40 ℃, sequentially adding astaxanthin, hydrolyzed collagen, carnosine, dipotassium glycyrrhizinate, beta-glucan, 1, 2-hexanediol, caprylyl glycol, inulin, brown algae extract, hydroxyphenylpropionamide benzoic acid, humic acid, mineral matter, acetyl hexapeptide-8 and ginger root extract, and homogenizing for 3min after the addition is finished.
And step six, continuously stirring, cooling to 30 ℃, detecting and discharging.
Example 3: a essence composition for delaying skin aging is different from that of example 1 in that: as shown in Table 1, the components are different in parts by weight.
The preparation method comprises the following operation steps:
step one, adding water into a water kettle according to the formula ratio in the table 1, starting stirring, sequentially adding ceramide 3, ceramide 6II, ceramide 1, ceramide 2, phytosphingosine, carbomer, xanthan gum, ethylhexylglycerin, butanediol, cholesterol, p-hydroxyacetophenone and tocopherol into the water kettle, and heating to 80 ℃.
And step two, premixing and dispersing the glycerol, the sodium hyaluronate and the acrylic acid (ester)/C10-30 alkanol acrylate cross-linked polymer, adding the mixture into a water pot, and homogenizing for 3 min.
And thirdly, sequentially adding caprylic/capric triglyceride, 1, 2-pentanediol, 4-tert-butylcyclohexanol, hexyldecanol, bisabolol, N-palmitoyl hydroxyproline cetyl wax ester, campesterol and polyacrylic acid into an oil pan, and heating to 80 ℃ to obtain an oil pan mixture.
And step four, adding the mixture in the oil pan in the step three into a water pan, homogenizing for 5min at 3000r/min, and starting to cool.
And step five, cooling and stirring the water kettle to 25 ℃, sequentially adding astaxanthin, hydrolyzed collagen, carnosine, dipotassium glycyrrhizinate, beta-glucan, 1, 2-hexanediol, caprylyl glycol, inulin, brown algae extract, hydroxyphenylpropionamide benzoic acid, humic acid, mineral matter, acetyl hexapeptide-8 and ginger root extract, and homogenizing for 6min after the addition is finished.
And step six, continuing stirring, cooling to 25 ℃, and detecting and discharging.
Example 4: a essence composition for delaying skin aging is different from that of example 1 in that: as shown in Table 1, the components are different in parts by weight, the preparation method is different, and 0.02 part of disodium EDTA is also added in the step one. 0.09 part of inulin and 0.01 part of brown algae extract are also added in the step five.
Example 5: a essence composition for delaying skin aging is different from that of example 1 in that: as shown in Table 1, the components in parts by weight are different, the preparation method is also different, and 0.1 part of disodium EDTA is also added in the first step. In the fifth step, 1.1 parts of inulin and 0.12 parts of brown algae extract are also added.
Example 6: the essence composition for delaying skin aging is different from the essence composition in example 1 in that: as shown in Table 1, the components in parts by weight are different, the preparation method is also different, and 0.2 part of disodium EDTA is also added in the first step. In the fifth step, 1.8 parts of inulin and 0.2 parts of brown algae extract are also added.
Second, comparative example
Comparative example 1: the essence composition for delaying skin aging adopts commercially available Yashilandai moisturizing skin-care essence lotion.
Comparative example 2: an essence composition for delaying skin aging adopts Olay water-feeling transparent white light plastic essence available on the market.
Comparative example 3: the essence composition for delaying skin aging adopts commercially available feloca NCTF serum regeneration essence.
Third, test data inspection
Test one: stratum corneum water change
Test subjects: the purification compositions obtained in examples 1 to 6 were used as test samples 1 to 6, and the purification compositions obtained in comparative examples 1 to 3 were used as control samples 1 to 3.
The test method comprises the following steps: randomly selected 45 persons of 18-40 years old in the same area, each group having 5 test samples. Firstly, facial cleanser (commercially available Nivea condensed water is used for collecting 150g of foam facial cleanser actively) is adopted, then the test samples 1-6 and the control samples 1-3 are respectively smeared on the skin after facial moisture is wiped off, after complete absorption, the moisture content of the stratum corneum of the skin at the position of nonuse, 0.5h, 1h, 2h, 3h and 4h is respectively tested by adopting a skin moisture content tester (Hengda technology), and real-time moisture loss data statistics is respectively carried out.
And (3) test results: as is clear from Table 2 and FIG. 1, the water content of the stratum corneum of each of the samples 1 to 6 was higher than that of the control sample 1. The stratum corneum water loss was greatest with test sample 4 within 1 hour, and the test sample 4 was relatively steep. Whereas the moisture content of the stratum corneum of the skin using test sample 4 decreased slowly over a period of 1-4 hours, the curve of test sample 4 was relatively flat.
As is apparent from fig. 1, the water content curves of control sample 1 and control sample 2 are significantly lower than those of test sample 4 and control sample 3. The curves for test sample 4 and control sample 3 show that: the water content of control sample 3 was higher than that of test sample 4 before 1.5h, and the water content of control sample 3 was significantly lower than that of test sample 4 after 1.5h, indicating that the water-holding capacity of test sample 4 was higher than that of control sample 3.
It can be seen from the combination of table 2 and fig. 1 of this experiment that the moisturizing capabilities of the sample samples 1-6 are generally higher than those of the control samples 1-3. Thus, samples 1-6 can significantly increase the water content of the stratum corneum as seen from the curve.
TABLE 2 test results of the stratum corneum moisture content of test samples 1 to 6 and control samples 1 to 3
Figure BDA0002270367160000131
And (2) test II: ability to resist photoaging
Test subjects: the test was conducted using a blank control and a solvent control, and the purified composition obtained in example 4 was used as test sample 4.
The test method comprises the following steps:
1. the test system comprises: the cells used in the test are fibroblasts, and are obtained by cell primary culture and subculture of Guangdong Boxi Biotech limited company.
2. Reagent: Low-DMEM (GIBCO), PBS (Dr. Germany), MTT (Sigma), DMSO (Sigma), Collagen IELISA kit (Abcam).
3. The main equipment is as follows: CO 2 2 Incubator (Thermo), clean bench (Sujing Antai), inverted microscope (Olympus), micro-oscillator (Linbel), enzyme labeling instrument (BioTek), and incubator (Tester).
4. Cytotoxicity test:
(1) cell inoculation: cells were seeded at a seeding density of 1E 4/well in 96-well plates in incubators (37 ℃ C., 5% CO) 2 、95%RH)。
(2) Preparing a first solution: in sample 4, 8 concentration gradients were set, and 3 replicate wells were set under each concentration gradient.
(3) Preparing a second solution: preparing a working solution (i) to (i) of a tested object according to a cytotoxicity test concentration gradient setting table (see table 3).
(4) Administration: to be plated in 96-well platesThe administration is carried out when the rate reaches 40-60%. Adding 200 mu L of cell culture solution into each hole of the blank control group, and adding 200 mu L of culture solution containing the corresponding concentration of the test object into each hole of the test sample 4; wells were zeroed for cell-free seeding and only 200 μ L of cell culture medium was added. After completion of the administration, the 96-well plate was placed in an incubator (37 ℃ C., 5% CO) 2 95% RH).
(5) And (3) testing: after 24h of cell culture, the supernatant was discarded, MTT working solution (0.5mg/mL, ready for use) was added, and incubated at 37 ℃ for 4h at 37 ℃ in the dark. After incubation, the supernatant was discarded and 150. mu.L DMSO was added to each well and the OD read at 490 nm.
(6) Calculating relative activity of cells:
Figure BDA0002270367160000141
5. cytotoxicity test:
(1) cell inoculation: cells were seeded at a density of 4E 4/well in 24-well plates and cultured in an incubator (37 ℃ C., 5% CO) 2 95% RH) overnight.
(2) Preparing a liquid: according to the result of cytotoxicity test, 5 concentrations around CV90 were selected for each sample, and morphological test was performed.
(3) Administration: and when the cell plating rate of the 24-well plate reaches 40-60%, the administration is carried out. The test sample 4 was added to the cell culture medium containing the test substance at the corresponding concentration, and the blank control group was added to the cell culture medium in an incubator (37 ℃ C., 5% CO) 2 95% RH) for 24 h.
(4) And (3) morphological observation: after the end of the culture, the cell morphology was observed under an inverted microscope and photographed (20 ×), see fig. 3.
6. Anti-photoaging efficacy test
(1) Cell inoculation: cells were seeded at a density of 2.5E 5/well in 6-well plates in incubators (37 ℃ C., 5% CO) 2 95% RH) overnight.
(2) Preparing a liquid: the preparation of the working solution of the test object was carried out according to the test groups (see Table 4).
(3) Administration according to the specific design of the experiment in Table 4, the cells in the 6-well plate are platedWhen the rate reaches 40-50%, the medicine is administered in groups, the dosage of each hole is 2ml, and each group is provided with 3 multiple holes. During the culture period (37 ℃ C., 5% CO) 2 95% RH) for 24 h.
(4) Radiation: culturing for 24 hr, irradiating with UVA, replacing fresh culture medium, and culturing in incubator (37 deg.C, 5% CO) 2 95% RH) for 24 h.
(5) Collecting cell supernatant, culturing for 24 hr, collecting cell culture supernatant in 1.5ml of LEP tube, and storing at-80 deg.C in refrigerator for freezing.
(6) ELISA test: cllagen detection was performed according to Cllagen 1ELISA reagents.
And (3) test results: as can be seen from table 3, fig. 2 and fig. 3, the cytotoxicity test result and the morphology test result finally determined that the maximum safe concentration of the test sample 4 was 1.25%.
As can be seen from table 4, table 5 and fig. 4, when the test sample 4 is irradiated by UVA, the collagen content of the test sample 4 is reduced from 81.85ng/ml (blank control) to 76.76ng/ml, and when the solvent control group is irradiated by UVA, the collagen content of the test sample 4 is reduced from 81.85ng/ml (blank control) to 55.51ng/ml, compared with the solvent control group (UVA +), so it is obvious that the collagen content of the control sample 4 of the present application can be significantly increased (P < 0.05), and the test sample 4 has a certain anti-aging effect.
TABLE 3 8 concentration gradients in sample 4
Figure BDA0002270367160000151
TABLE 4
Test object Concentration of sample Treatment method Detecting the index Detection method
Blank control group / UVA- Collagen ELISA
Solvent control group / UVA+ Collagen ELISA
Test sample No. 4 1.25% UVA+ Collagen ELISA
TABLE 5
Figure BDA0002270367160000152
And (3) test III: radical scavenging test
Test subjects: the cleaning composition obtained in example 4 was used as test sample 4; the cleaning compositions prepared in comparative examples 1-3 were used as control samples 1-3.
The test method comprises the following steps:
the experiment is based on the characteristic that DPPH free radical has single electron, strong absorption is generated at 517nm, and alcoholic solution is purple. In the presence of a free radical scavenger, its absorption gradually disappears by pairing with its single electron, and its degree of discoloration is quantitatively related to the number of electrons it receives, so that a rapid quantitative analysis can be performed with a spectrophotometer.
Preparing the tested test sample 1 and the control samples 1-3 into solutions with mass concentrations of 0.1mg/ml, 0.2mg/ml, 0.4mg/ml, 0.6mg/ml and 0.8mg/ml by using distilled water respectively, adding 2ml of diluent and 2ml of 0.2mg/ml DPPH 50% ethanol solution into the same test tube, shaking uniformly, standing for 30min in a closed manner at room temperature, measuring absorbance at a wavelength of 517nm, and calculating the removal rate, thereby evaluating and discussing the antioxidant capacity of the refined carving, namely the face moistening essence milk and other products.
Clearance rate ═ 1- (A) 1 -A 2 )/A 0 ]×100%
In the formula, A 1 The absorbance of the sample solution + DPPH.50% ethanol solution;
A 2 the absorbance of the sample solution plus 50% ethanol solution;
A 0 the absorbance was DPPH.50% ethanol solution + distilled water.
TABLE 6
Figure BDA0002270367160000161
TABLE 7 measurement results of radical scavenging rates of test sample 4 and control sample 1
Figure BDA0002270367160000162
And (3) test results: as can be seen in table 6, table 7 and fig. 5, the ability to scavenge free radicals becomes stronger with increasing concentration. The curves for control sample 1 and control sample 2 mostly coincide, with clearance for control sample 1 being less than control sample 2 between concentrations of 0.1mg/ml and 0.2 mg/ml. The curve of the control sample 3 is relatively zigzag, the clearance rate of the control sample 3 is greater than that of the control sample 1 within the concentration range of 0.1mg/ml to 0.3 mg/ml; between 0.4mg/ml and 0.8mg/ml, the clearance of control sample 3 was less than that of test sample 4. The clearance curve for test sample 4 is much higher than the clearance curves for control samples 1-3.
Compared with the control samples 1-3, the highest clearance is the test sample 4, the second is the control sample 3 and the control sample 2, and the lowest clearance is the control sample 1 between the concentrations of 0.2mg/ml and 0.4 mg/ml. The greater the clearance, the greater the antioxidant capacity, so the antioxidant capacity is in turn test sample 4 > control sample 3 > control sample 2 > control sample 1. At higher concentrations, the highest clearance was found in test sample 4, the worst was found in control sample 3, and the clearance was not much different between control samples 1 and 2.
From this, it can be seen that the antioxidant ability of the test sample 4 of the present application is far stronger than that of the control samples 1 to 3.
And (4) testing: variation of canthus wrinkle
Test subjects: the cleaning compositions obtained in example 4 were each used as test sample 4.
The test method comprises the following steps: two women with significant wrinkles in the canthus of 40-50 years old were randomly selected as volunteers in the same area, and the results of fine lines in the canthus at 0 week and 4 weeks (photographed) were recorded after the test sample 4 was continuously applied for 4 weeks, and are shown in fig. 6.
And (3) test results: as shown in the photograph of fig. 6, the canthus wrinkles of both volunteers were significantly improved after four weeks of the test sample 4, the wrinkles were shallow in depth and short in length.
The specific embodiments are only for explaining the present invention, and the present invention is not limited thereto, and those skilled in the art can make modifications without inventive contribution to the present embodiments as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present invention.

Claims (1)

1. The essence composition for delaying skin aging is characterized by comprising the following components in parts by mass:
82.44 parts of water;
0.02 part of EDTA disodium;
0.75 part of p-hydroxyacetophenone;
30.033 parts of ceramide;
0.018 portion of ceramide 6 II;
10.00003 parts of ceramide;
0.018 parts of phytosphingosine;
0.0087 parts of carbomer;
0.009 parts of xanthan gum;
0.0089 part of ethylhexyl glycerol;
6.81 parts of butanediol;
20.065 parts of ceramide;
0.047 parts of cholesterol;
0.012 part of tocopherol;
11.12 parts of glycerol;
0.7 part of sodium hyaluronate;
0.69 part of acrylic acid (ester)/C10-30 alkanol acrylate crosslinked polymer;
3.2 parts of caprylic/capric triglyceride;
2.7 parts of 1, 2-pentanediol;
0.16 part of 4-tert-butylcyclohexanol;
2.11 parts of hexyldecanol;
0.14 part of bisabolol;
0.13 part of N-palmitoyl hydroxyproline cetyl ester;
0.025 parts of rape sterols;
0.18 part of polyacrylic acid;
0.031 portion of astaxanthin
0.31 part of hydrolyzed collagen;
0.75 part of carnosine;
0.3 part of dipotassium glycyrrhizinate;
0.032 part of beta-glucan;
0.736 part of 1, 2-hexanediol;
0.016 part of caprylyl glycol;
0.09 part of inulin;
0.01 part of brown algae extract;
0.033 parts of hydroxyphenylpropionamide benzoic acid;
0.014 parts of humic acid;
0.025 parts of mineral;
80.007 parts of acetyl hexapeptide;
ginger root extract 0.058 parts.
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