Lifting, tightening and exfoliating composition as well as microcrystal and preparation method thereof

By buried tire tightness and exfoliating compositions in the soluble microcrystalline needle of hyaluronic acid in oxidized hyaluronic acid, using cross -linking to generate Sifine, it solves the problem of being difficult to effectively deliver active ingredients to the dermis layer. High -efficiency, security firmness and exfoliating effects.

CN119345093APending Publication Date: 2025-01-24GUANGDONG UNIV OF TECH
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Patent Information

Application Number
CN202311114274.9
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2023-08-30
Publication Date
2025-01-24

AI Technical Summary

Technical Problem

Existing firming and exfoliating products are difficult to effectively deliver active ingredients to the dermis, resulting in low absorption rates and frequent injection methods, high treatment costs, and complex operation.

Method used

Develop a soluble microcrystalline composition for lifting, firming, and exfoliation. By embedding it in oxidized hyaluronic acid soluble microcrystalline needles, the oxidized hyaluronic acid is cross-linked with collagen to generate Schiff base, thereby improving the active composition. Excellent transdermal absorption and sustained release to reduce irritation.

Benefits of technology

It improves the transparent absorption and slow release of the active component, reduces the irritation, significantly improves the effects of tensioning and exfoliating, delaying the skin's thinning time, which has the characteristics of safe and efficient and convenient operation.

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Abstract

The invention discloses a lifting, tightening and exfoliating composition as well as a soluble microcrystal and a preparation method thereof. According to the technical scheme, the skin care product is prepared from 0.2 to 1.2 parts of fructus perillae extract, 0.2 to 1.2 parts of rhizoma curcumae longae extract, 0.2 to 4 parts of XVII type collagen, 0.1 to 0.5 part of vitriol, 0.2 to 1.2 parts of gardenia extract, 5 to 20 parts of oxidized hyaluronic acid, 3 to 10 parts of algal polysaccharide, 3 to 10 parts of glycerol and 51.9 to 88.1 parts of ultrapure water. According to the microcrystal provided by the invention, the lifting, tightening and exfoliating composition is embedded in the oxidized hyaluronic acid soluble microcrystal needle body, so that the effects of improving the transdermal absorbability and slow release property of active components and reducing irritation are achieved, and the lifting, tightening and exfoliating effects are further improved; belongs to the technical field of daily chemicals.
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Description

Technical Field

[0001] The invention relates to a skin care product and a preparation method thereof, in particular to a lifting, firming and exfoliating composition and a preparation method thereof; and belongs to the technical field of daily chemical products. Background Art

[0002] As people's aesthetic level improves, "Q elastic and smooth" skin has become one of the hot topics that beauty lovers pay attention to. The skin is composed of three parts: epidermis, dermis and subcutaneous tissue. When the human dermis undergoes asymmetrical division due to external or internal factors such as light radiation or aging, the thickness of the dermis decreases, the epidermal cells cannot be fully and timely replenished, and the stratum corneum lacks "fresh" keratin replenishment, and the skin is no longer "Q elastic". Healthy keratin is dense and elastic, while aging keratin is fragile, dull and dull, and loses the adhesion between cells and the ability to protect the skin. If the stratum corneum is too thick, too many keratin cells will block the pores, which may cause the accumulation of sebum and provide conditions for the formation of acne. In addition, an overly thick stratum corneum will affect the absorption of nutrients by the skin and may also cause skin problems such as enlarged pores. Although self-aging and external light radiation are inevitable, we can alleviate the negative effects of both in other ways to maintain skin elasticity, and firming and exfoliating cosmetics came into being.

[0003] Collagen is an indispensable component of hemidesmosomes in basal daughter cells. When this protein is lacking, basal daughter cells divide asymmetrically, and the number of basal daughter cells gradually decreases, eventually leading to a weakening of the ability of dermal cells to divide and differentiate, and thinning of the skin thickness. When this protein is present, it can induce basal daughter cells to divide symmetrically, maintain the high ability of dermal cells to divide and differentiate, and slow down the rate of skin thinning, which is the cause of wrinkles and a sign of skin aging. The stratum corneum is the protective barrier of the skin, but the aging stratum corneum will not only clog the pores, thereby affecting the skin's oil secretion and nutrient absorption, but also lose its barrier effect.

[0004] There are two main forms of firming and exfoliating products today: 1. Topical cosmetics, which mainly add active ingredients that soften the stratum corneum and promote collagen secretion or cell regeneration to improve the thickness of the skin's stratum corneum. However, due to the existence of the skin barrier, macromolecules such as proteins and water-soluble active ingredients are difficult to break through the blockade of the stratum corneum and epidermal cells, and cannot effectively deliver active ingredients to the dermis, resulting in a low absorption rate. 2. Epidermal filling, by injecting collagen, hyaluronic acid or botulinum toxin-like substances into the skin. However, this method not only has a short effective period of the active ingredients, but also only treats the symptoms but not the root cause, resulting in frequent injections and high treatment costs; and this method requires professional operation, the process is very painful, may be accompanied by adverse reactions, and the operation is cumbersome.

[0005] Therefore, it is very necessary to develop a safe, efficient, low-irritation, easy-to-operate, effective and stable lifting, firming and exfoliating product. Summary of the invention

[0006] In order to overcome the problems existing in the above-mentioned prior art, the purpose of the present invention is to provide a soluble microcrystalline composition for lifting, firming and exfoliating the stratum corneum, which shortens the keratin replacement cycle by promoting the division and differentiation of basal daughter cells, and maintains elasticity and smoothness of the skin by continuously producing dense and elastic new keratin.

[0007] The second purpose of the present invention is to embed the lifting, firming and stratum corneum exfoliating composition into the oxidized hyaluronic acid soluble microcrystalline needle body, and the oxidized hyaluronic acid and the effective ingredient collagen are cross-linked to form a Schiff base, which not only has the effect of improving the transdermal absorption, sustained release and reducing irritation of the active component, but also can effectively inhibit bacterial growth, further enhancing the skin firming and stratum corneum exfoliating effects.

[0008] Another object of the present invention is to provide a method for preparing the above-mentioned lifting, firming and stratum corneum-exfoliating soluble microcrystalline composition, which has simple operation, low production energy consumption, low cost, and is easy to realize continuous mass production.

[0009] The present invention adopts the following technical scheme to achieve the first purpose.

[0010] A lifting, firming and exfoliating composition comprises the following components by weight: 0.2-1.2 parts of perilla fruit extract, 0.2-1.2 parts of turmeric extract, 0.2-4 parts of type XVII collagen, 0.1-0.5 parts of bosacein and 0.2-1.2 parts of gardenia extract.

[0011] Furthermore, the above-mentioned lifting, firming and exfoliating composition also includes 5-20 parts of oxidized hyaluronic acid, 3-10 parts of seaweed polysaccharide, and 3-10 parts of glycerol.

[0012] The second technical solution provided by the present invention is as follows:

[0013] A lifting, firming and exfoliating microcrystal comprises a base and a needle body located on the base, wherein the lifting, firming and exfoliating composition described in the first technical solution is embedded in the needle body.

[0014] Furthermore, in the above-mentioned lifting, firming and exfoliating microcrystals, the needle body is an oxidized hyaluronic acid microcrystal pillar.

[0015] The third technical solution provided by the present invention is a method for preparing the above-mentioned lifting, firming and exfoliating microcrystals, which comprises the following steps in sequence:

[0016] 1) Weigh each component;

[0017] 2) adding the perilla fruit extract, turmeric extract, type XVII collagen, bosacein, and gardenia extract weighed in step 1) to the remaining amount of ultrapure water and stirring to dissolve, then adding oxidized hyaluronic acid, seaweed polysaccharide, and glycerol, stirring to dissolve to make it swell evenly, and centrifuging to remove bubbles to obtain a viscous liquid;

[0018] 3) injecting the viscous liquid prepared in step 2) into the microcrystal mold by vacuuming, and recovering the excess viscous liquid to obtain a soluble microcrystal needle tip;

[0019] 4) dissolving 3-10% chitosan and 15-20% hyaluronic acid in the remaining water, stirring evenly and centrifuging to remove bubbles to obtain a base solution;

[0020] 5) adding the base solution prepared in step 4) into the mold containing the microcrystal needle tip solution in step 3), and preparing the soluble microcrystals with self-lifting, tightening and exfoliating properties by constant temperature drying.

[0021] Furthermore, in the preparation method of the above-mentioned lifting, firming and exfoliating microcrystals, the oxidized hyaluronic acid described in step 2) is prepared by oxidizing hyaluronic acid and sodium periodate for 1-2 hours in a dark environment, at room temperature of 25-30°C, with a stirring speed of 350-600 rpm / min, and stirring for 10-15 minutes, and then dialyzing through a dialysis bag with a pore size of 8000-14000KDa to remove unreacted sodium periodate and its acid radicals, and then freeze-drying at -60°C for 60-80 hours.

[0022] Furthermore, in the above-mentioned method for preparing lifting, firming and exfoliating microcrystals, the stirring rate in step 2) is 300-700 rpm / min, and the stirring time is 15-45 min.

[0023] Furthermore, in the above-mentioned method for preparing lifting, firming and exfoliating microcrystals, the vacuuming temperature in step 3) is 25-40° C., the vacuum degree is 0.5-0.9 MPa, and the vacuum time is 40-70 min.

[0024] Furthermore, in the above-mentioned method for preparing lifting, firming and exfoliating microcrystals, the stirring rate in step 4) is 300-700 rpm / min, and the stirring time is 15-45 min; the centrifugal rate is 3200-4800 rpm / min, the centrifugal time is 5-15 min, and the temperature is 2-8°C.

[0025] Furthermore, in the preparation method of the above-mentioned lifting, firming and exfoliating composition, in step 5), the constant temperature drying temperature is 35-40° C., and the drying time is 12-24 hours.

[0026] The present invention has the following beneficial technical effects:

[0027] 1) The composition of the present invention uses oxidized hyaluronic acid cross-linked collagen as the microcrystal needle tip viscous liquid to produce Schiff base with antibacterial effect, reducing the probability of bacteria infecting the human body through the traces left by the microcrystals; at the same time, the added collagen can promote the homolysis and proliferation of basal daughter cells, and other additives can stimulate collagen synthesis, inhibit the activity of collagenase that degrades collagen, and prevent collagen loss, thereby increasing the thickness of the dermis to delay the thinning time of the skin, and having a certain anti-aging effect while playing a role in skin firming.

[0028] 2) The present invention embeds the lifting, firming and exfoliating composition in the oxidized hyaluronic acid soluble microcrystalline needle body, which has the effects of improving the transdermal absorbability and sustained release of the active components and reducing irritation, further enhancing the lifting, firming and exfoliating effects.

[0029] 3) The technical solution provided by the present invention adopts perilla fruit extract, turmeric extract, type XVII collagen, bosaiin, and gardenia extract to form a formula with each other, and the synergistic effect is achieved by inhibiting collagen degradation, promoting cell proliferation, and increasing cell adhesion to maintain the elasticity of the dermis and increase the firmness of cells and skin. Among them, gardenia extract and perilla fruit extract can effectively inhibit the activity of MMP1 enzyme and slow down the degradation of collagen; by adding type XVII collagen to induce symmetrical division of matrix daughter cells, increase the number of dermal cells, shorten the replacement cycle of stratum corneum, and effectively solve the problem of aging and thinning of stratum corneum; the added bosaiin and turmeric extract can promote the generation and construction of proteoglycans in the extracellular matrix and improve the adhesion between dermis and epidermis;

[0030] 4) The technical solution provided by the present invention adopts perilla fruit extract, turmeric extract, type XVII collagen, bosin, gardenia extract and oxidized hyaluronic acid, seaweed polysaccharide, and glycerin to better break through the skin barrier, effectively exert the efficacy of the composition, stably maintain skin elasticity, increase cell and skin firmness, and coordinate skin water balance, further enhancing the lifting, firming and exfoliating effects. BRIEF DESCRIPTION OF THE DRAWINGS

[0031] Figure 1 The present invention provides a structural diagram of a lifting, firming and exfoliating soluble beauty microcrystal.

[0032] Figure 2 It is a graph of Hacat cell proliferation. DETAILED DESCRIPTION

[0033] The technical solution of the present invention is further specifically described below through specific preferred embodiments. It should be understood that the specific embodiments described herein are only used to explain the present invention and are not used to limit the present invention.

[0034] The bosogenin used in the present invention was purchased from Shanghai Macklin Biochemical Technology Co., Ltd.; the perilla fruit extract was obtained by petroleum ether reflux extraction and methanol reduced pressure evaporation extraction; the turmeric extract was obtained by ultrasonic extraction; type XVII collagen was purchased from Beijing Bioson Biotechnology Co., Ltd.; and the gardenia extract was purchased from Shanghai Macklin Biochemical Technology Co., Ltd.

[0035] Perilla fruit extract is prepared by the following method:

[0036] (1) Accurately weigh 620 g of perilla fruit, fully crush it using a grinder, and pass it through a 60-mesh sieve;

[0037] (2) Reflux extraction with 1250 ml of petroleum ether (60-90°C) for 2 h;

[0038] (3) Reflux extraction with 2000 mL of 80% methanol aqueous solution for 2.5 h;

[0039] (4) Methanol was evaporated under reduced pressure at 50°C.

[0040] Turmeric extract was prepared by the following method:

[0041] (1) Accurately weigh 100 g of turmeric plant, grind it and pass it through an 80-mesh sieve;

[0042] (2) Dissolve in 85% ethanol and sonicate for 30 min;

[0043] (3) Centrifuge at 12000 r / min for 4 min, repeat extraction three times, and then filter through a 0.45 μm microporous membrane.

[0044] Example 1

[0045] The present invention provides a lifting, firming and exfoliating composition, which consists of the following components: 0.2g of perilla fruit extract, 0.2g of turmeric extract, 0.2g of type XVII collagen, 0.1g of bosogenin, 0.2g of gardenia extract, 15g of oxidized hyaluronic acid, 4g of seaweed polysaccharide and 8g of glycerol.

[0046] Example 2

[0047] The present invention provides a lifting, firming and exfoliating composition, which consists of the following components: 0.4g of perilla fruit extract, 0.4g of turmeric extract, 1g of type XVII collagen, 0.2g of bosogenin, 0.4g of gardenia extract, 15g of oxidized hyaluronic acid, 4g of seaweed polysaccharide and 8g of glycerol.

[0048] Example 3

[0049] The present invention provides a lifting, firming and exfoliating composition, which consists of the following components: 0.6g of perilla fruit extract, 0.6g of turmeric extract, 2g of type XVII collagen, 0.3g of bosogenin, 0.6g of gardenia extract, 15g of oxidized hyaluronic acid, 4g of seaweed polysaccharide and 8g of glycerol.

[0050] Example 4

[0051] The present invention provides a lifting, firming and exfoliating composition, which consists of the following components: 0.8g of perilla fruit extract, 0.8g of turmeric extract, 3g of type XVII collagen, 0.4g of bosogenin, 0.8g of gardenia extract, 15g of oxidized hyaluronic acid, 4g of seaweed polysaccharide and 8g of glycerol.

[0052] Example 5

[0053] The present invention provides a lifting, firming and exfoliating composition, which consists of the following components: 1.2g of perilla fruit extract, 1.2g of turmeric extract, 4g of type XVII collagen, 0.5g of bosogenin, 1.2g of gardenia extract, 15g of oxidized hyaluronic acid, 4g of seaweed polysaccharide and 8g of glycerol.

[0054] Example 6

[0055] The present embodiment provides a lifting, firming and exfoliating microcrystal, comprising a base and a needle body located on the base, wherein the microcrystal is conical and the needle head length is 450-850 μm. The lifting, firming and exfoliating composition provided in embodiment 1 is embedded in the needle body.

[0056] The specific preparation method is as follows:

[0057] 1) Add 0.2 g of perilla fruit extract, 0.2 g of turmeric extract, 0.2 g of type XVII collagen, 0.1 g of bosaicin, and 0.2 g of gardenia extract to 72.08 g of water, stir and dissolve at a stirring speed of 300-700 rpm / min for 15-45 minutes, then add 15 g of oxidized hyaluronic acid, 4 g of seaweed polysaccharide, and 8 g of glycerol, continue stirring to make it swell evenly, centrifuge to remove bubbles, and obtain a viscous liquid.

[0058] 2) Preparation of soluble microcrystalline needle tip:

[0059] The above viscous liquid is injected into a square microcrystal mold, and the vacuum is drawn at a temperature of 25-40 degrees Celsius for 40-70 minutes at a vacuum degree of 0.5-0.9 MPa, and the excess needle tip solution on the mold surface is recovered to obtain a soluble microcrystal needle tip.

[0060] 3) Preparation of the base:

[0061] Dissolve 4 g of chitosan and 15 g of hyaluronic acid in 81 g of water, stir at 650 rpm / min for 40 min until uniform, and then centrifuge at 4°C, 4000 rpm / min, for 10 min to remove bubbles to obtain a base solution.

[0062] 4) Preparation of soluble microcrystals

[0063] The base solution prepared in step 3) is added to the mold containing the microcrystal needle tip solution in step 2), and dried at 35-40°C for 12-24 hours to obtain soluble microcrystals with self-lifting, tightening and exfoliating properties, such as Figure 1 As shown in the structure diagram.

[0064] The oxidized hyaluronic acid is prepared by subjecting hyaluronic acid to an oxidation reaction with sodium periodate for 1 hour in a dark environment, at room temperature of 25-30°C, with a stirring speed of 500 rpm / min, and stirring for 15 minutes, dialyzing through a dialysis bag with a pore size of 8000-14000 KDa to remove unreacted sodium periodate and its acid radicals, and then freeze-drying at -60°C for 60-80 hours.

[0065] Example 7

[0066] The present embodiment provides a lifting, firming and exfoliating microcrystal, comprising a base and a needle body located on the base, wherein the microcrystal is conical and the needle head length is 450-850 μm. The lifting, firming and exfoliating composition provided in embodiment 2 is embedded in the needle body.

[0067] The specific preparation method is as follows:

[0068] 1) Preparation of viscous liquid:

[0069] Add 0.4g of perilla fruit extract, 0.4g of turmeric extract, 1g of type XVII collagen, 0.2g of bosacein and 0.4g of gardenia extract to 70.58g of water, stir to dissolve, then add 15g of oxidized hyaluronic acid, 4g of seaweed polysaccharide and 8g of glycerol, continue stirring to make it swell evenly, centrifuge to remove bubbles, and obtain a viscous liquid.

[0070] 2) Preparation of soluble microcrystalline needle tip solution:

[0071] Same as Example 6.

[0072] 3) Preparation of the base:

[0073] Same as Example 6.

[0074] 4) Preparation of soluble microcrystals:

[0075] Same as Example 6.

[0076] Example 8

[0077] The present embodiment provides a lifting, firming and exfoliating microcrystal, comprising a base and a needle body located on the base, wherein the microcrystal is conical and the needle head length is 450-850 μm. The lifting, firming and exfoliating composition provided in embodiment 3 is embedded in the needle body.

[0078] The specific preparation method is as follows:

[0079] The following steps are involved:

[0080] 1) Preparation of viscous liquid:

[0081] Add 0.6g of perilla fruit extract, 0.6g of turmeric extract, 2g of type XVII collagen, 0.3g of bosacein and 0.6g of gardenia extract to 68.9g of water, stir to dissolve, then add 15g of oxidized hyaluronic acid, 4g of seaweed polysaccharide and 8g of glycerol, continue stirring to make it swell evenly, centrifuge to remove bubbles, and obtain a viscous liquid.

[0082] 2) Preparation of soluble microcrystalline needle tip:

[0083] Same as Example 6.

[0084] 3) Preparation of the base:

[0085] Same as Example 6.

[0086] 4) Preparation of soluble microcrystals:

[0087] Same as Example 6.

[0088] The preparation method is similar to that of Example 6.

[0089] Example 9

[0090] The present embodiment provides a lifting, firming and exfoliating microcrystal, comprising a base and a needle body located on the base. The microcrystal is conical, and the needle head length is 450-850 μm.

[0091] The needle body is embedded with the lifting, firming and exfoliating composition provided in Example 4.

[0092] The specific preparation method is as follows:

[0093] 1) Preparation of viscous liquid:

[0094] Add 0.8g of perilla fruit extract, 0.8g of turmeric extract, 3g of type XVII collagen, 0.4g of bosacein, and 0.8g of gardenia extract to 67.2g of water, stir to dissolve, then add 15g of oxidized hyaluronic acid, 4g of seaweed polysaccharide, and 8g of glycerol, continue stirring to make it swell evenly, centrifuge to remove bubbles, and obtain a viscous liquid.

[0095] 2) Preparation of soluble microcrystalline needle tip:

[0096] Same as Example 6.

[0097] 3) Preparation of the base:

[0098] Same as Example 6.

[0099] 4) Preparation of soluble microcrystals:

[0100] Same as Example 6.

[0101] Example 10

[0102] The present embodiment provides a lifting, firming and exfoliating microcrystal, comprising a base and a needle body located on the base. The microcrystal is conical, and the needle head length is 450-850 μm.

[0103] The needle body is embedded with the lifting, firming and exfoliating composition provided in Example 5.

[0104] The specific preparation method is as follows:

[0105] Add 1.2g of perilla fruit extract, 1.2g of turmeric extract, 4g of type XVII collagen, 0.5g of bosacein, and 1.2g of gardenia extract to 64.9g of water, stir to dissolve, then add 15g of oxidized hyaluronic acid, 4g of seaweed polysaccharide, and 8g of glycerol, continue stirring to make it swell evenly, centrifuge to remove bubbles, and obtain a viscous liquid.

[0106] 2) Preparation of soluble microcrystalline needle tip:

[0107] Same as Example 6.

[0108] 3) Preparation of the base:

[0109] Same as Example 6.

[0110] 4) Preparation of soluble microcrystals:

[0111] Same as Example 6.

[0112] Embodiment 11

[0113] This embodiment provides a lifting, firming and exfoliating microcrystal, comprising a base and a needle body located on the base, wherein the microcrystal is conical and the needle head length is 450-850 μm.

[0114] The needle body is embedded with the lifting, firming and exfoliating composition provided in Example 5; and an experiment is designed to optimize the needle body matrix formula.

[0115] The specific preparation method is as follows:

[0116] 1.2 g of perilla fruit extract, 1.2 g of turmeric extract, 4 g of type XVII collagen, 0.5 g of bosacein, and 1.2 g of gardenia extract were added into the ultrapure water of the corresponding formula and stirred to dissolve; then, the needle tip matrix solutions of each formula in Table 1 were added and continued to be stirred to make it swell evenly, and centrifuged to remove bubbles to obtain a viscous liquid.

[0117] Table 1 Test plan for needle tip matrix formulation

[0118]

[0119]

[0120] 2) Preparation of soluble microcrystalline needle tip:

[0121] Same as Example 6.

[0122] 3) Preparation of the base:

[0123] Same as Example 6.

[0124] 4) Preparation of soluble microcrystals:

[0125] Same as Example 6.

[0126] The soluble microcrystals prepared by the formulas in Table 1 were subjected to a pig skin puncture test to detect the puncture rate, and the results are shown in Table 2 below:

[0127] Table 2 Pig skin puncture test puncture rate

[0128]

[0129]

[0130] The mechanical strength of the microcrystalline needle tip is positively correlated with its puncture ability. The mechanical strength of the needle tip can be increased by increasing the concentration of the supporting material in the formula. Table 2 shows the results of the pig skin puncture test puncture rate. Oxidized hyaluronic acid is the main supporting material for mechanical strength. As the concentration increases from 1-25%, the puncture rate first increases to a peak and then gradually decreases. Seaweed polysaccharide also plays a role in increasing mechanical strength. As the concentration increases, the needle tip puncture rate also increases. Comprehensive analysis of the entire Table 2 shows that the puncture rate is high when the concentration of oxidized hyaluronic acid is 5-20%, seaweed polysaccharide is 3-10%, and glycerol is 3-10%. Among them, the puncture rate of the formula with 15% oxidized hyaluronic acid, 4% seaweed polysaccharide and 8% glycerol is the highest, up to 98.4%.

[0131] Comparative Example 1 Preparation method of soluble microcrystalline composition without adding perilla fruit extract

[0132] 1) Preparation of viscous liquid:

[0133] 1.2g of turmeric extract, 4g of type XVII collagen, 0.5g of bosacein and 2.4g of gardenia extract are added into 64.9g of water and stirred to dissolve. Then 15g of oxidized hyaluronic acid, 4g of seaweed polysaccharide and 8g of glycerol are added and stirred continuously to make the mixture swell evenly. Centrifuge to remove bubbles to obtain a viscous liquid.

[0134] 2) Preparation of soluble microcrystalline needle tip:

[0135] Same as Example 6.

[0136] 3) Preparation of the base:

[0137] Same as Example 6.

[0138] 4) Preparation of soluble microcrystals:

[0139] Same as Example 6.

[0140] Comparative Example 2 Preparation method of soluble microcrystalline composition without adding turmeric extract

[0141] 1) Preparation of viscous liquid:

[0142] Add 2.4g of perilla fruit extract, 4g of type XVII collagen, 0.5g of bosacein and 1.2g of gardenia extract into 64.9g of water and stir to dissolve. Then add 15g of oxidized hyaluronic acid, 4g of seaweed polysaccharide and 8g of glycerol and continue stirring to make it swell evenly. Centrifuge to remove bubbles to obtain a viscous liquid.

[0143] 2) Preparation of soluble microcrystalline needle tip:

[0144] Same as Example 6.

[0145] 3) Preparation of the base:

[0146] Same as Example 6.

[0147] 4) Preparation of soluble microcrystals:

[0148] Same as Example 6.

[0149] Comparative Example 3 Preparation method of collagen-free soluble microcrystalline composition

[0150] 1) Preparation of viscous liquid:

[0151] Add 1.2g of perilla fruit extract, 1.2g of turmeric extract, 0.5g of bosacein and 1.2g of gardenia extract to 68.9g of water and stir to dissolve. Then add 15g of oxidized hyaluronic acid, 4g of seaweed polysaccharide and 8g of glycerol and continue stirring to make it swell evenly. Centrifuge to remove bubbles to obtain a viscous liquid.

[0152] 2) Preparation of soluble microcrystalline needle tip:

[0153] Same as Example 6.

[0154] 3) Preparation of the base:

[0155] Same as Example 6.

[0156] 4) Preparation of soluble microcrystals:

[0157] Same as Example 6.

[0158] Comparative Example 4 Preparation method of soluble microcrystalline composition without adding bosine

[0159] 1) Preparation of viscous liquid:

[0160] Add 1.2g of perilla fruit extract, 1.2g of turmeric extract, 4g of type XVII collagen and 1.2g of gardenia extract to 65.4g of water and stir to dissolve. Then add 15g of oxidized hyaluronic acid, 4g of seaweed polysaccharide and 8g of glycerol and continue stirring to make it swell evenly. Centrifuge to remove bubbles to obtain a viscous liquid.

[0161] 2) Preparation of soluble microcrystalline needle tip:

[0162] Same as Example 6.

[0163] 3) Preparation of the base:

[0164] Same as Example 6.

[0165] 4) Preparation of soluble microcrystals:

[0166] Same as Example 6.

[0167] Comparative Example 5 Preparation method of soluble microcrystalline composition without adding gardenia extract

[0168] 1) Preparation of viscous liquid:

[0169] Add 1.2g of perilla fruit extract, 2.4g of turmeric extract, 4g of type XVII collagen, and 0.5g of bosaicin to 64.9g of water, stir to dissolve, then add 15g of oxidized hyaluronic acid, 4g of seaweed polysaccharide, and 8g of glycerol, continue stirring to make it swell evenly, centrifuge to remove bubbles, and obtain a viscous liquid.

[0170] 2) Preparation of soluble microcrystalline needle tip:

[0171] Same as Example 6.

[0172] 3) Preparation of the base:

[0173] Same as Example 6.

[0174] 4) Preparation of soluble microcrystals:

[0175] Same as Example 6.

[0176] Comparative Example 6 (Blank Comparative Example)

[0177] Preparation method of lifting, firming and exfoliating composition

[0178] The following steps are involved:

[0179] 1) Preparation of viscous liquid:

[0180] Add 15 g of oxidized hyaluronic acid, 4 g of seaweed polysaccharide, 8 g of glycerol and 73 g of ultrapure water, stir to make it swell evenly, and centrifuge to remove bubbles to obtain a viscous liquid.

[0181] 2) Preparation of soluble microcrystalline needle tip:

[0182] Same as Example 6.

[0183] 3) Preparation of the base:

[0184] Same as Example 6.

[0185] 4) Preparation of soluble microcrystals:

[0186] Same as Example 6.

[0187] Comparative Example 7 (Positive Drug Comparative Example)

[0188] Hyaluronic acid is a firming positive drug1; fruit acid is a peeling positive drug2

[0189] In order to demonstrate the advantages of the technical solution provided by the present application, experimental tests of the technical solution provided by the present application are given below.

[0190] Experimental Example 1 DPPH free radical scavenging test

[0191] Test samples: a lifting, firming and exfoliating composition prepared in Examples 6-10, Comparative Examples 1-5 and a blank comparative example.

[0192] Experimental method: The in vitro antioxidant performance of the sample was evaluated by scavenging DPPH free radicals. Its ethanol solution has maximum absorption at a wavelength of 517nm and is purple. When a free radical scavenger is present, it pairs with its electrons, causing the ultraviolet absorption intensity to weaken or even disappear, and the degree of fading is proportional to the number of electrons it accepts. Therefore, the antioxidant activity of the sample can be evaluated by measuring the change in absorbance.

[0193] The specific steps are as follows:

[0194] Take three PE tubes, add 4 mL of deionized water to one tube, and add 4 mL of the viscous liquid of the above examples and blank examples to the other two tubes, respectively, and mark them as 1, 2, and 3. Add 4 mL of DPPH solution to tubes 1 and 2 in turn, and add 4 mL of anhydrous ethanol to tube 3. Mix well, keep it away from light for 30 minutes, and measure its absorbance at a wavelength of 517 nm with an ultraviolet spectrophotometer in turn.

[0195] The scavenging rate calculation formula is: scavenging rate (%) = [1-(A2-A3) / A1] × 100%, where: A1 is the absorbance of DPPH ethanol solution; A2 is the absorbance of the test solution scavenging free radicals; A3 is the absorbance of the test solution.

[0196] The calculated results are shown in Table 3 below:

[0197] Table 3 DPPH free radical scavenging test results

[0198] Grouping DPPH free radical scavenging rate of test samples % Example 6 62.3 Example 7 65.4 Example 8 72.3 Example 9 79.2 Example 10 84.3 Comparative Example 1 49.2 Comparative Example 2 51.3 Comparative Example 3 41.2 Comparative Example 4 48.7 Comparative Example 5 50.1 Blank comparison 0.5

[0199] Experimental results: It can be seen from Table 3 that the scavenging rates of Examples 6-10 on DPPH free radicals are much higher than those of the blank comparative examples, and the scavenging rates gradually increase with the increase of concentration; Comparative Examples 1-5 are viscous liquids containing only four functional ingredients, among which Comparative Example 3 has the worst free radical scavenging ability, and this comparative example is a group without adding collagen; The effect of the comparative examples in scavenging DPPH free radicals is far inferior to that of the embodiments, which indicates that the five functional ingredients synergistically scavenges free radicals, can effectively resist oxidation, and stably delay the aging of keratinocytes.

[0200] Experimental Example 2: Effect of lifting, firming and exfoliating composition on keratinocyte proliferation

[0201] Test samples: Examples 6 to 10 and comparative examples 1 to 5 viscous liquid were used as the experimental group, and hyaluronic acid was used as the positive drug control group 1.

[0202] Experimental methods:

[0203] (1) Recovery culture of keratinocytes (Hacat):

[0204] Take out the cells from the liquid nitrogen tank, thaw them quickly in a 37℃ water bath with constant stirring, and melt the cryopreservation solution in the cryopreservation tube within 1 minute; wipe and disinfect the cryopreservation tube with 75% alcohol, and transfer the cell suspension into a 15mL centrifuge tube on a sterile operating table; centrifuge at 1000rpm for 5 minutes, and discard the supernatant; add 5mL of complete culture medium to the centrifuge tube, blow and mix evenly, and transfer it into a 25cm 2 Culture flask: Place the cell culture flask in a 37°C, 5% CO2 cell culture incubator for culture.

[0205] (2) Subculture of keratinocytes (Hacat):

[0206] When the cells in the culture flask grow and fuse into a sheet of 70-80%, subculture is performed; the original culture medium in the culture flask is discarded on the clean bench, and the cells are washed twice with preheated PBS (preheated in a 37°C cell culture incubator), the PBS is discarded, 0.5 mL of preheated 0.25% Trypsin-0.02% EDTA is added, and the cells are digested at 37°C for 5-10 minutes. During the cell digestion process, the culture flask is gently tapped to accelerate the degree of cell digestion; when observed under an inverted phase contrast microscope, after most of the cells become round and suspended, an equal volume of DMEM high-glucose complete medium is added, and the cells are gently shaken to neutralize the activity of trypsin; the cell suspension is transferred to a 15 mL centrifuge tube, centrifuged at 1000 rpm for 5 minutes, the supernatant is discarded, DMEM high-glucose complete medium is added, the cells are gently blown with a pipette to mix, and then inoculated into a new culture flask, and the cell culture flask is placed in a cell culture incubator at 37°C and 5% CO2 for culture. The growth is observed on the second day and the culture medium is replaced.

[0207] (3) Effects of the experimental group and the positive drug control group on the growth of Hacat cells

[0208] Prepare 11 equal amounts of DMEM high-glucose complete culture medium, add 10 ml of the viscous liquid of Examples 6 to 10, the viscous liquid of Comparative Examples 1 to 5 (experimental group), the positive drug (control group) and 10 ml of distilled water (blank control group) respectively. Inoculate the culture medium with equal amounts of bacterial seed liquid of the same density.

[0209] (4) Cell growth curve determination

[0210] The cells after inoculation were made into a single cell suspension with DMEM high-glucose medium, and the cell density was adjusted to 1×104 / mL and inoculated in a 96-well plate, with an initial number of 1000 cells per well. After 24 hours of inoculation and culture (recorded as day 0), the culture medium was replaced at the same time on days 0, 2, 4, 6, 8, 10, and 12, and the cell proliferation was determined by the MTT method. During the determination, the culture medium of each well was carefully aspirated, 90 ml of DMEM high-glucose basal medium and 10 μL of 5 mg / mL MTT solution were added, and the culture was continued for 4 hours in a cell culture incubator at 37°C. Then the supernatant of each well was aspirated, 110 μL of formazan solution was added, and the shaker was placed on a low-speed shaker for 10 minutes to fully dissolve the crystals. The absorbance of each well was measured at 490 nm using an enzyme-linked immunosorbent assay.

[0211] The results of the effects of the experimental group and the control group on the proliferation of Hacat cells are shown below Figure 2 :

[0212] Experimental results: The stratum corneum is mainly composed of keratin, which is composed of dead anucleated epidermal cells. The newly formed keratin is dense and elastic, while the aged keratin is fragile, dull and lusterless, and loses the adhesion between cells and the ability to protect the skin, and then forms a desquamated tissue. The dermis undergoes symmetrical division to produce matrix daughter cells with the ability to redifferentiate and divide, maintaining the vitality of the dermis cells and the thickness of the dermis. By adding the effective ingredients in Examples 6-10, Comparative Examples 1-5 and Positive Drug Control 1, the dermis cells are prompted to continuously divide symmetrically to form keratinocytes, and the dermis cells secrete collagen, which can not only shorten the keratin renewal cycle, but also produce full and elastic collagen filling, so that the skin remains tight and elastic.

[0213] Hacat cells were in the latent period from 0 to 2 days with a low proliferation rate. They entered the logarithmic growth phase on the 4th day. The cell number reached the maximum on the 10th day, then gradually decreased and entered the senescence phase. When in the latent period, there was no significant difference in the effect of each experimental group and the control group on the proliferation of Hacat cells; when in the logarithmic growth period, the cells began to proliferate in large quantities, among which Examples 6-10 gradually increased the promoting effect of cell proliferation with the increase of the concentration of the effective components, and Example 10 had the greatest effect on the proliferation of Hacat cells, while the positive drug control group 1 and the comparative example 3 without the addition of collagen had the least promoting effect on the proliferation of Hacat cells, but were still significantly higher than the blank control group; when the number of cell proliferation reached a peak on the tenth day, Example 10 also had the best effect, while the positive drug control group and the comparative example 3 without the addition of collagen had the least promoting effect on the proliferation of Hacat cells; Compared with Comparative Examples 1-5, Example 10 added five effective components, while the comparative examples added one less effective component each, and the remaining effective components were the same as the examples, but it can be seen from the result diagram that the promoting effect of Example 10 on the proliferation of Hacat cells far exceeded that of Comparative Examples 1-5, which indicates that the five effective components synergistically promote the proliferation of keratinocytes, can effectively increase the thickness of the epidermis, and stably achieve the effect of skin firming and shortening the stratum corneum renewal cycle.

[0214] Experimental Example 3 Anti-aging test of human skin using lifting, firming and exfoliating composition

[0215] Test samples: Examples 6 to 10 were used to prepare lifting, firming and exfoliating compositions as the experimental group, and Comparative Examples 1-5 and hyaluronic acid (positive comparative example 1), fruit acid (positive comparative example 2), and a blank comparative example were used as the control group.

[0216] Experimental methods:

[0217] (1) 130 healthy women aged 25 to 30 years were selected and divided into 13 groups, with 10 women in each group. Each group used the same formula product;

[0218] (2) Test area: subject’s face;

[0219] (3) Usage: once a day, 1-2 hours each time, for 1 month;

[0220] (4) Effect indicators: Skin wrinkles were measured using the skin elasticity tester MPA580 produced by German CK Company and the Reviscometer RV600 probe.

[0221] The test results are shown in Table 4:

[0222] Table 4 Test results

[0223] Group Wrinkle area reduction (%) Example 6 33.6 Example 7 35.6 Example 8 40.1 Example 9 42.3 Example 10 46.4 Comparative Example 1 32.2 Comparative Example 2 31.8 Comparative Example 3 22.1 Comparative Example 4 33.2 Comparative Example 5 30.1 Positive drug comparative example 1 31.2 Positive drug comparative example 2 28.4 Blank comparison 1.2

[0224] Experimental results: From the test data in Table 4, it can be concluded that the wrinkle removal and skin tightening effects are ranked as Example 10 > Example 9 > Example 8 > Example 7 > Example 6 > Comparative Example 4 > Comparative Example 1 > Comparative Example 2 > Positive drug comparative example 1 > Comparative Example 5 > Positive drug comparative example 2 > Comparative Example 3 > Blank control group, which proves that the lifting, firming and exfoliating composition has better anti-aging effect than a simple combination of one, two or three ingredients through the synergistic effect between the components.

[0225] In summary, the composition of the present invention uses oxidized hyaluronic acid cross-linked collagen as a microcrystalline needle tip viscous liquid to produce a Schiff base with antibacterial effect, reducing the probability of bacteria infecting the human body through traces left by microcrystalline; at the same time, the added collagen can promote the homolysis and proliferation of basal daughter cells, thereby increasing the thickness of the dermis to delay the thinning time of the skin, and other additives can stimulate collagen synthesis, inhibit the collagenase activity of degrading collagen, prevent collagen loss and fill the gap between skin cells, and play a role in skin firming while also playing a certain anti-aging effect. The present invention embeds the lifting and firming, exfoliating composition in the oxidized hyaluronic acid soluble microcrystalline needle body, which has the effect of improving the transdermal absorbability, sustained release and irritation reduction of the active component, and further enhances the lifting and firming, exfoliating efficacy.

[0226] The present invention embeds the lifting, firming and exfoliating composition in the hyaluronic acid soluble microcrystalline needle body, which has the effects of improving the transdermal absorbability and sustained release of the active components and reducing irritation, and further improving the lifting, firming and exfoliating effects.

[0227] The above description is only a preferred embodiment of the present invention and does not limit the present invention in any form. There are other variations and modifications without exceeding the technical solutions described in the claims.

Claims

1. A lifting, firming and exfoliating composition, characterized in that: The invention comprises the following components in parts by weight: 0.2-1.2 parts of perilla fruit extract, 0.2-1.2 parts of turmeric extract, 0.2-4 parts of type XVII collagen, 0.1-0.5 parts of bosacein and 0.2-1.2 parts of gardenia extract.

2. A lifting, firming and exfoliating composition according to claim 1, characterized in that: It also includes 5-20 parts of oxidized hyaluronic acid, 3-10 parts of seaweed polysaccharide, 3-10 parts of glycerol and 51.9-88.1 parts of ultrapure water.

3. A microcrystal for lifting, firming and exfoliating, characterized in that: The invention comprises a base and a needle body located on the base, wherein the lifting, firming and exfoliating composition according to claims 1 and 2 is embedded in the needle body.

4. The microcrystal for lifting, firming and exfoliating according to claim 3, characterized in that: The needle body is an oxidized hyaluronic acid microcrystalline pillar.

5. The method for preparing the lifting, firming and exfoliating microcrystals according to claim 3, characterized in that: The steps are as follows: 1) Weigh each component according to the weight portion described in claim 1 or 2; 2) adding 51.9-88.1 parts of ultrapure water to the perilla fruit extract, turmeric extract, type XVII collagen, bosin, and gardenia extract weighed in step 1) and stirring; then adding the oxidized hyaluronic acid, seaweed polysaccharide, and glycerol described in claim 2), stirring and dissolving to make it swell evenly, and centrifuging to remove bubbles to obtain a viscous liquid; 3) injecting the viscous liquid prepared in step 2) into the microcrystal mold by vacuuming, and recovering the excess viscous liquid to obtain a soluble microcrystal needle tip; 4) dissolving 3-10% chitosan and 15-20% hyaluronic acid in the remaining water, stirring evenly and centrifuging to remove bubbles to obtain a base solution; 5) adding the base solution prepared in step 4) into the mold containing the microcrystal needle tip solution in step 3) and preparing microcrystals with lifting, tightening and exfoliating properties by constant temperature drying.

6. The method for preparing lifting, firming and exfoliating microcrystals according to claim 5, characterized in that: The oxidized hyaluronic acid described in step 2) is prepared by subjecting hyaluronic acid to an oxidation reaction with sodium periodate for 1-2 hours in a dark environment at room temperature of 25-30°C, with a stirring speed of 350-600 rpm / min, and stirring for 10-15 minutes, dialyzing through a dialysis bag with a pore size of 8000-14000 KDa to remove unreacted sodium periodate and its acid radicals, and then freeze-drying at -60°C for 60-80 hours.

7. The method for preparing lifting, firming and exfoliating microcrystals according to claim 5, characterized in that: In step 2), the stirring rate is 300-700 rpm / min, and the stirring time is 15-45 min.

8. The method for preparing lifting, firming and exfoliating microcrystals according to claim 5, characterized in that: The vacuuming temperature in step 3) is 25-40°C, the vacuum degree is 0.5-0.9Mpa, and the vacuum time is 40-70min.

9. The method for preparing lifting, firming and exfoliating microcrystals according to claim 5, characterized in that: In step 4), the stirring rate is 300-700 rpm / min, and the stirring time is 15-45 min; the centrifugal rate is 3200-4800 rpm / min, the centrifugal time is 5-15 min, and the temperature is 2-8°C.

10. The method for preparing the lifting, firming and exfoliating composition according to claim 5, characterized in that: In step 5), the constant temperature drying temperature is 35-40° C., and the drying time is 12-24 hours.