Repair composition, preparation method thereof and repair preparation

Abstract

The invention provides a repairing composition, a preparation method thereof and a repairing preparation, and belongs to the technical field of repairing product preparation. The repairing composition is prepared from the following raw materials in parts by weight: 5-20 parts of Chinese wolfberry fruits, 2-10 parts of scutellaria baicalensis roots, 1.5-9 parts of licorice roots and 4.5-20 parts of calamine. The repairing composition disclosed by the invention has an obvious inhibiting effect on hyaluronidase, so that the repairing composition has soothing and anti-allergy effects. Elastase can be effectively inhibited, completeness and elasticity of the skin structure can be maintained, skin laxity can be improved, wrinkles can be reduced, and the skin can be tight, elastic and moist.

Description

Technical Field

[0001] The invention belongs to the technical field of preparation of repair products, and specifically relates to a repair composition and a preparation method thereof and a repair preparation. Background Art

[0002] When the skin is stimulated by external stimuli, such as excessive sunlight, contact with certain substances, or dry and dehydrated skin, it often shows inflammatory manifestations such as itching, blisters, redness, and swelling. Skin inflammation is the result of a complex interaction between multiple inflammatory mediators. During the inflammatory process, on the one hand, the cells and tissues of the body are directly or indirectly damaged. On the other hand, through inflammatory bleeding and inflammatory exudation, harmful substances from the outside world can be diluted, killed, and besieged. The body repairs and heals damaged tissues through the regeneration of parenchymal and interstitial cells. Inflammatory damage, anti-damage, and repair are a dynamic process of trinity. Ways that can help reduce skin inflammation include topical application of anti-inflammatory drugs, use of topical preparations with soothing and repairing effects, hydrotherapy, oral prescription or over-the-counter drugs, etc. The most acceptable way is to use topical preparations with few side effects and soothing and repairing effects.

[0003] According to TCM theory, sunlight is warm and its nature belongs to fire. The evil of fire and heat can easily cause swelling and ulcers, and the evil of fire can easily generate wind and move blood, which can cause skin erythema, swelling and itching. Ancient medical books believe that sunburn is caused by "heat", so heat-clearing and detoxifying drugs can be used to achieve the effect of clearing heat and detoxifying heat. Clinical studies have shown that the external application of heat-clearing and detoxifying prescriptions can effectively reduce erythema and edema. In the field of Western medicine, after-sun repair cosmetics mainly carry out cell-level treatment. The main effective ingredients are retinol, niacinamide, panthenol, etc., with a single effect and prone to adverse side effects. There are few prescriptions and medicines for after-sun repair in ancient Chinese medical books. Clinical medicine shows that Chinese medicines for clearing heat and detoxification, treating burns, and treating sunburn all have the potential for after-sun repair. Studies have shown that natural plant ingredients rich in flavonoids and sugar compounds have anti-inflammatory damage, anti-photosensitivity and antioxidant effects, which can inhibit the production of inflammatory factors, reduce the damage of ultraviolet radiation to skin cells, and relieve inflammatory reactions. These active ingredients derived from traditional Chinese medicine have the advantages of multi-target synergy, significant efficacy, and few side effects. However, due to the large amount of sugars contained in these plant extracts, they are prone to agglomeration during storage, affecting the convenience of use. Summary of the invention

[0004] In view of the above problems, the present invention provides a composition that can soothe skin inflammation and has a repairing effect on skin discomfort caused by external stimuli. Experimental results show that it not only has a significant inhibitory effect on hyaluronidase involved in skin inflammation and allergic reactions, but also has an effect on elastase that affects skin elasticity and causes wrinkles. It is used in skin care product preparations, and the results of human safety tests show that there is no adverse reaction to the skin. The results of human efficacy tests show that it has a soothing, repairing, nourishing and firming effect on the skin. Different from the prior art, the composition is composed of a plant extract part and calcined calamine, which solves the problem that the plant extract is easy to agglomerate, has stable quality, is more convenient to use, and has an improved inhibitory effect on hyaluronidase, and the soothing effect is enhanced.

[0005] One of the objects of the present invention is to provide a repairing composition.

[0006] The second object of the present invention is to provide a method for preparing the repair composition.

[0007] The third object of the present invention is to provide a repair preparation comprising the repair composition.

[0008] In order to achieve the above-mentioned purpose of the present invention, the following technical solutions are particularly adopted:

[0009] In a first aspect, the present invention provides a repair composition prepared from the following raw materials in parts by weight: 5 to 20 parts of wolfberry fruit, 2 to 10 parts of scutellaria root, 1.5 to 9 parts of licorice root, and 4.5 to 20 parts of calamine.

[0010] Preferably, the wolfberry fruit is Ningxia wolfberry fruit.

[0011] Preferably, the calamine is calcined calamine.

[0012] Typical but non-limiting weight portions of wolfberry are, for example, 5, 8, 10, 12, 14, 15, 16, 18, or 20 portions.

[0013] Typical but non-limiting weight portions of Scutellaria baicalensis Root are, for example, 2, 3, 4, 5, 6, 7, 8, 9, or 10 parts.

[0014] Typical but non-limiting weight fractions of liquorice root are, for example, 1.5, 2, 3, 4, 5, 6, 7, 8, 9 parts.

[0015] Typical but non-limiting mass fractions of calamine are, for example, 4.5, 5, 6, 8, 10, 12, 14, 15, 16, 18, 20 parts.

[0016] In a second aspect, the present invention provides a method for preparing the above-mentioned repair composition, comprising the following steps:

[0017] (1) Weigh the dried Scutellaria baicalensis root and Licorice root according to the formula, crush them, soak them in ethanol, and set aside;

[0018] (2) weighing wolfberry fruit according to the formula amount, adding it into an extraction tank together with the soaked scutellaria root and liquorice root, and extracting it with ethanol reflux three times, collecting the filtrates, filtering them respectively, and combining them to obtain an extract;

[0019] (3) concentrating the extract obtained in step (2) to obtain a concentrated solution, spray-drying the concentrated solution into powder, and sieving to obtain a plant extract powder;

[0020] (4) Drying and sieving the calamine according to the formula amount, and then adding the plant extract powder obtained in step (3) and mixing them thoroughly to obtain a repair composition.

[0021] Preferably, in step (1), the ethanol concentration is 40% to 50%;

[0022] Preferably, in step (2), 9 to 10 times the amount of ethanol is added for the first time and the extraction is carried out for 110 minutes; 8 to 10 times the amount of ethanol is added for the second time and the extraction is carried out for 90 minutes; and 8 to 10 times the amount of ethanol is added for the third time and the extraction is carried out for 100 minutes.

[0023] The plant component of the repair composition provided by the present invention is that scutellaria baicalensis is the main drug, wolfberry fruit, liquorice and calamine are the auxiliary drugs, and various raw materials and components perform their respective functions and cooperate with each other, so as to effectively reduce skin inflammation caused by ultraviolet irradiation, soothe and repair sunburned skin and improve skin elasticity. Scutellaria baicalensis has a cold medicinal property and a bitter taste. The active ingredients are flavonoid compounds, mainly baicalin, baicalein, wogonin and wogonin, among which baicalin is the most abundant. Scutellaria baicalensis extract can promote the regeneration of endogenous type I and type IV collagen, reverse the loss of collagen caused by ultraviolet irradiation, and work together in multiple aspects to resist cell photoaging, and has the effect of protecting the skin from ultraviolet damage. As a main drug, it can effectively soothe skin inflammation, improve skin redness, and enhance skin elasticity. Lycium barbarum, with sweet and flat medicinal properties, has the effects of nourishing the liver and kidney, improving the essence and improving eyesight; it is used for deficiency of essence, soreness of waist and knees, internal heat and thirst, blood deficiency and sallowness, blurred vision, etc. Lycium barbarum contains ingredients such as Lycium barbarum polysaccharides, carotenoids, Lycium barbarum flavonoids and Lycium barbarum polyphenols, which have the effects of immunomodulation, anti-oxidation and anti-radiation. The present invention selects Ningxia Lycium barbarum extract with excellent quality. As a ministerial drug, it repairs the skin barrier function, helps the effective ingredients in the Scutellaria baicalensis extract enter the basal layer of the skin, and exerts anti-inflammatory effects. Licorice is sweet and flat in nature, nourishes the spleen and replenishes qi, clears away heat and detoxifies, and can be used for symptoms such as weak spleen and stomach, cough and sputum, carbuncle, sore and poison, etc. The active ingredients of licorice have good anti-inflammatory effects. Licorice chalcone A, as one of the main chemical components of licorice anti-inflammatory, can play a significant inhibitory role in the expression pathways of inflammatory factors such as IL-6 and TNF-α. As a ministerial drug, licorice not only has good anti-inflammatory effects, but also can assist the monarch drug to expand the scope of anti-inflammatory factors and enhance the overall anti-inflammatory and soothing effects of the repair composition. Calamine has the effects of detoxification, improving eyesight, removing cataracts, absorbing moisture, relieving itching and healing sores. It is used for red and swollen eyes, red and rotten eyelids, cataracts covering the eyes, pterygium climbing the eyes, ulcers that do not heal, pus dripping, and itching of wet sores. The main component of calamine is natural zinc carbonate, which is a moderate antiseptic and astringent protective agent, and has a significant effect in treating skin inflammation or surface trauma. In order to improve the appearance and coating spreading performance of the product, calcined calamine with stable properties, fine and uniform texture, and the main component of zinc oxide is selected. It can not only effectively prevent the agglomeration of plant extract powder, but also enhance the astringent, anti-inflammatory and antiseptic effects of the repair composition, and also improve its spreadability and coating feel.

[0024] The repair composition provided by the present invention is dialectically formulated on the basis of the practice of traditional Chinese medicine for treating skin diseases. The plant extract part is a spray-dried powder with the solvent removed, and the impurities that may be contained are fully removed through ethanol extraction, and the effective ingredients in the plant are fully retained. In actual production, the plant extract powder rich in sugar substances will agglomerate and discolor after long-term storage. Adding calamine solves the problem of accurate weighing affected by agglomeration in actual applications and affecting the production timeliness of the formula preparation, thereby improving the utilization rate of raw materials and the convenience of use.

[0025] The present invention selects calamine and plant extracts to be compatible, which can not only solve the problem of powder agglomeration, but also significantly improve the inhibitory effect on hyaluronidase. Other montmorillonite powder, talcum powder or calcined gypsum powder cannot achieve similar effects.

[0026] In a third aspect, the present invention provides a repair preparation comprising the above-mentioned repair composition.

[0027] Repair preparations include but are not limited to repair lotions, repair night creams, repair facial masks, etc.

[0028] The repair preparation formula includes, in addition to the above-mentioned repair composition, solvents, skin conditioners, thickeners, skin feel regulators, penetration enhancers, chelating agents, preservatives, moisturizers, emollients, emulsifiers, antioxidants, and the like.

[0029] Beneficial effects:

[0030] The results of laboratory experiments on soothing efficacy show that the repair composition of the present invention has a significant inhibitory effect on hyaluronidase, indicating that it has soothing and anti-allergic effects. It can also effectively inhibit elastase, help maintain the integrity and elasticity of the skin structure, improve skin sagging, reduce wrinkles, and make the skin firm and elastic. Safety assessment, human safety and human efficacy tests were conducted on the soothing repair products added with the repair composition. The product safety assessment results show that under normal, reasonable and foreseeable use, it will not cause harm to human health. The results of the human skin patch test on human safety show that all 30 subjects had no adverse reactions. It can be seen from the results of the human efficacy experiment that the soothing repair lotion and soothing repair mask in the present invention can effectively reduce capillary dilation and relieve the redness of the skin after stimulation. In addition, it also has the effect of repairing the skin barrier function, increasing the moisture content of the stratum corneum, reducing the amount of water loss, increasing the glossiness of the skin, improving the elasticity and firmness of the skin, reducing the roughness, and improving the smoothness of the skin. It has a soothing, repairing, firming and nourishing effect on the skin. The invention is applicable to skin care products such as repairing lotion, repairing mask, repairing cream, base cream, etc., and is easy to operate, has remarkable effect, and its safety meets relevant requirements. The invention uniformly mixes the plant extract powder with the calcined calamine powder, solves the agglomeration problem in storage, and improves the utilization rate of the raw materials and the convenience of application. In addition, compared with the comparative example without calamine, the inhibition rate of hyaluronidase is improved.

[0031] The present invention has been described in detail above, but the above embodiments are only illustrative in nature and are not intended to limit the present invention. In addition, this article is not limited by any theory described in the above prior art or invention content or the following examples. BRIEF DESCRIPTION OF THE DRAWINGS

[0032] Figure 1 This is the changing trend of the moisture content in the stratum corneum.

[0033] Figure 2 This is the changing trend of transepidermal water loss.

[0034] Figure 3 The changing trend of skin glossiness.

[0035] Figure 4 This is the changing trend of the skin erythema index (EI).

[0036] Figure 5 This is the changing trend of skin elasticity R2 value.

[0037] Figure 6 This is the changing trend of skin elasticity R5 value.

[0038] Figure 7 This is the changing trend of skin elasticity Q1 value.

[0039] Figure 8 This is the changing trend of skin firmness F4 value.

[0040] Fig. 9 This is the changing trend of skin roughness parameter (SEr).

[0041] Fig.10 This is the changing trend of skin smoothness parameter (SEsm). DETAILED DESCRIPTION

[0042] The present invention is further described below in conjunction with examples. It should be noted that the following examples are provided for illustrative purposes only and do not constitute a limitation on the scope of protection claimed for the present invention.

[0043] Unless otherwise specified, the raw materials, reagents, methods, etc. used in the examples are conventional raw materials, reagents, methods in the art.

[0044] The sources of raw materials are shown in Table 1 Raw Materials Information Table.

[0045] Table 1

[0046]

[0047]

[0048] Example 1

[0049] A soothing and repairing composition, the raw materials of which include 5 parts by weight of Ningxia wolfberry fruit, 2 parts by weight of scutellaria root, 1.8 parts by weight of liquorice root, and 4.6 parts by weight of calamine.

[0050] Preparation process:

[0051] The first step is to weigh the dried scutellaria root and liquorice root according to the formula amount, crush them, soak them in 50% ethanol and set them aside.

[0052] The second step is to weigh the wolfberry fruit of the formula, add it into the extraction tank together with the soaked scutellaria root and liquorice root, add 9 times the amount of 50% ethanol for the first time, extract for 110 minutes; add 9 times the amount of 50% ethanol for the second time, extract for 90 minutes; add 8 times the amount of 50% ethanol for the third time, extract for 100 minutes. Collect the extract, filter, and combine the filtrate to obtain the extract.

[0053] The third step is to concentrate the extract obtained in the second step to obtain a concentrated solution without alcohol taste, spray-dry the concentrated solution into powder, pass it through a 120-mesh sieve, and set aside.

[0054] The fourth step is to dry the calcined calamine, pass it through a 120-mesh sieve, and then add the plant extract powder obtained in the third step, and mix them thoroughly to obtain a repairing composition.

[0055] Example 2

[0056] A soothing and repairing composition, the raw materials of which include 7 parts by weight of Ningxia wolfberry fruit, 2.6 parts by weight of scutellaria root, 2.3 parts by weight of liquorice root, and 6.4 parts by weight of calamine.

[0057] The preparation process is the same as that of Example 1.

[0058] Example 3

[0059] A soothing and repairing composition comprises 9 parts by weight of Ningxia wolfberry fruit, 3.8 parts by weight of scutellaria root, 3 parts by weight of liquorice root and 7.5 parts by weight of calamine.

[0060] The preparation process is the same as that of Example 1.

[0061] Example 4

[0062] A soothing and repairing composition comprises raw materials including 12 parts by weight of Ningxia wolfberry fruit, 5 parts by weight of scutellaria root, 4 parts by weight of liquorice root and 11 parts by weight of calamine.

[0063] The preparation process is the same as that of Example 1.

[0064] Example 5

[0065] A soothing and repairing composition comprises raw materials including 14 parts by weight of Ningxia wolfberry fruit, 6 parts by weight of scutellaria root, 5 parts by weight of liquorice root and 13 parts by weight of calamine.

[0066] The preparation process is the same as that of Example 1.

[0067] Example 6

[0068] A soothing and repairing composition comprises raw materials including 16 parts by weight of Ningxia wolfberry fruit, 7 parts by weight of scutellaria root, 5.4 parts by weight of liquorice root and 15 parts by weight of calamine.

[0069] The preparation process is the same as that of Example 1.

[0070] Example 7

[0071] A soothing and repairing composition, the raw materials of which include 18 parts by weight of Ningxia wolfberry fruit, 8.8 parts by weight of scutellaria root, 6 parts by weight of liquorice root, and 16.5 parts by weight of calamine.

[0072] The preparation process is the same as that of Example 1.

[0073] Example 8

[0074] A soothing and repairing composition comprises raw materials including 20 parts by weight of Ningxia wolfberry fruit, 9.5 parts by weight of scutellaria root, 9 parts by weight of liquorice root and 20 parts by weight of calamine.

[0075] The preparation process is the same as that of Example 1.

[0076] The components are shown in Table 2.

[0077] Table 2

[0078]

[0079]

[0080] Comparative Examples 1-8

[0081] The comparative example is a plant extract powder without calamine, and the components are shown in Table 3.

[0082] Table 3

[0083]

[0084] Comparative Example Preparation Process:

[0085] The first step is to weigh the dried scutellaria root and liquorice root according to the formula amount, crush them, soak them in 50% ethanol and set them aside.

[0086] The second step is to weigh the wolfberry fruit of the formula, add it into the extraction tank together with the soaked scutellaria root and liquorice root, add 9 times the amount of 50% ethanol for the first time, extract for 110 minutes; add 9 times the amount of 50% ethanol for the second time, extract for 90 minutes; add 8 times the amount of 50% ethanol for the third time, extract for 100 minutes. Collect the extract, filter, and combine the filtrate to obtain the extract.

[0087] The third step is to concentrate the extract obtained in the second step to obtain a concentrated solution without alcohol taste, spray-dry the concentrated solution into powder, and pass it through a 120-mesh sieve to obtain a plant extract powder.

[0088] Application Example 1: Repair Lotion Formula and Preparation

[0089] Table 4 Repairing lotion formula composition

[0090]

[0091]

[0092] The formula of the repairing lotion consists of three parts: water phase, oil phase and repairing composition. The water phase contains phase B, phase C and phase D, the oil phase is phase A, and the repairing composition is phase E. The formula includes the following raw materials in weight percentage: 2% glycerol; 3% caprylic / capric triglyceride; 2% wheat germ oil; 1% evening primrose oil; 1% avocado tree butter; 0.3% polysorbate-80; 0.3% lecithin; 0.8% steareth-21; 0.4% steareth-20; 0.3% xanthan gum; 0.4% phenoxyethanol; 0.3% sodium benzoate; 0.2% panthenol; 0.2% tocopherol acetate; 0.15% allantoin; 0.1% disodium EDTA; 0.08% menthol lactate; 2% repairing composition; purified water is added to 100%.

[0093] Preparation method: add phase B raw materials to the water phase pot, heat to 70℃~75℃, and stir to mix evenly; add phase A raw materials to the oil phase pot, heat to 60℃~65℃, and stir to mix evenly; add phase E to the water phase pot, stir to mix evenly at 70℃~75℃; add phase A in the oil phase pot to the water phase pot, homogenize at 65℃~70℃ for 3~5 minutes, and then stir for 5~8 minutes; when the temperature drops to 40℃~42℃, add the pre-mixed C raw materials and stir evenly; add phase D and mix evenly; continue to cool to room temperature and discharge.

[0094] Application Example 2: Formulation and Preparation of Repair Night Cream

[0095] Table 5 Repair Night Cream Formula Composition

[0096]

[0097] The formula of the repairing night cream consists of three parts: water phase, oil phase and repairing composition. The water phase contains phase B, phase C and phase D, the oil phase is phase A, and the repairing composition is phase E. The formula includes the following raw materials in weight percentage: 3% glycerin; 3% caprylic / capric triglyceride; 2% wheat germ oil; 2% evening primrose oil; 2% avocado butter; 2% repairing composition; 0.3% polysorbate-80; 0.4% lecithin; 1.5% steareth-21; 1% steareth-2; 0.5% xanthan gum; 0.4% phenoxyethanol; 0.3% sodium benzoate; 0.2% tocopheryl acetate; 0.15% allantoin; 0.1% disodium EDTA; 0.05% menthol lactate; and purified water added to 100%.

[0098] Preparation method: add phase B raw materials to the water phase pot, heat to 70℃~75℃, and stir to mix evenly; add phase A raw materials to the oil phase pot, heat to 60℃~65℃, and stir to mix evenly; add phase E to the water phase pot, stir and mix evenly at 70℃~75℃; add phase A in the oil phase pot to the water phase pot, homogenize at 65℃~70℃ for 3~5 minutes, then stir and cool; when the temperature drops to 40℃~42℃, add pre-mixed C raw materials and stir evenly; add phase D and mix evenly; continue to cool to room temperature and discharge.

[0099] Application Example 3: Repairing Facial Mask Formula and Preparation

[0100] Table 6 Repairing mask formula composition

[0101]

[0102]

[0103] The repair mask formula consists of three parts: water phase, oil phase and repair composition. The water phase contains phase B, phase C and phase D, the oil phase is phase A, and the repair composition is phase E. The raw materials are as follows in weight percentage: 3% glycerol; 1.5% caprylic / capric triglyceride; 2% wheat germ oil; 2% evening primrose oil; 0.5% avocado tree butter; 0.3% polysorbate-80; 0.4% lecithin; 1% steareth-21; 0.6% steareth-2; 0.3% xanthan gum; 0.4% phenoxyethanol; 0.3% sodium benzoate; 0.2% tocopheryl acetate; 0.15% allantoin; 0.1% disodium EDTA; 0.05% menthol lactate; 2% repair composition; purified water is added to 100%.

[0104] Preparation method: add phase B raw materials to the water phase pot, heat to 70℃~75℃, and stir to mix evenly; add phase A raw materials to the oil phase pot, heat to 60℃~65℃, and stir to mix evenly; add phase E to the water phase pot, stir to mix evenly at 70℃~75℃; add phase A in the oil phase pot to the water phase pot, homogenize at 65℃~70℃ for 3~5 minutes, and then stir for 5~8 minutes; when the temperature drops to 40℃~42℃, add the pre-mixed C raw materials and stir evenly; add phase D and mix evenly; continue to cool to room temperature and discharge.

[0105] Test example: Stability test

[0106] With reference to the fourth part of the Pharmacopoeia (2020 edition) 9001 Guidelines for Stability Testing of Raw Materials and Preparations, an accelerated stability test was designed. The test samples were placed at a temperature of 40°C ± 2°C and a relative humidity of 75% ± 5% for 3 months. Samples were taken at the initial and final 4 time points (such as 0, 1, 2, and 3 months) to examine changes in appearance, heat resistance, cold resistance, and water content. The results are shown in Tables 7-1 to 7-4 below: Stability Test Results.

[0107] Table 7-1 Initial results of the accelerated stability test in month 0

[0108]

[0109]

[0110] The results of various test indicators of the test samples after one month of accelerated testing are shown in Table 7-2: Results of the first month of the stability test accelerated test.

[0111] Table 7-2 Results of the first month of the accelerated stability test

[0112]

[0113] The results of various test indicators of the test samples after 2 months of accelerated testing are shown in Table 7-3 below: Results of the second month of the stability test accelerated test.

[0114] Table 7-3 Results of the second month of the accelerated stability test

[0115]

[0116] The results of various test indicators of the test samples after 3 months of accelerated testing are shown in Table 7-4 below: Results of the third month of the stability test accelerated test.

[0117] Table 7-4 Results of the third month of the accelerated stability test

[0118]

[0119]

[0120] The test samples were subjected to accelerated testing for 3 months at a temperature of 40℃±2℃ and a relative humidity of 75%±5%. The samples were tested in accordance with the "Technical Specification for Safety of Cosmetics" (2015 edition) and GB / T29665-2013 at 0, 1, 2 and 3 months. The microbial indicators: total colony count, total mold and yeast count all met the requirements of the "Technical Specification for Safety of Cosmetics" (2015 edition).

[0121] The embodiment containing calamine showed no significant changes in appearance, heat resistance and cold resistance after three months of accelerated testing, and the pass rate of passing through an 80-mesh sieve was greater than 98% after fineness inspection. The comparative example without calamine showed caking in the first month, and still had caking in the second to third months, and the pass rate of passing through an 80-mesh sieve was about 80% after fineness inspection. It can be seen that calamine helps to reduce the caking phenomenon during the storage of the plant extract of the composition.

[0122] Test example: Soothing and improving skin elasticity efficacy test

[0123] 1. Experiment on the efficacy of inhibiting hyaluronidase

[0124] 1. Experimental principle: Hyaluronidase is an enzyme that can hydrolyze hyaluronic acid and is a participant in type I allergic reactions. Hyaluronidase has a strong correlation with inflammation and allergies. Therefore, the in vitro inhibition test of hyaluronidase can reflect the soothing, anti-allergic, and anti-inflammatory effects of the corresponding product on the skin to a certain extent. Hyaluronidase catalyzes a reaction with the enzyme substrate, and the absorbance changes after the active substance is added. The hyaluronidase activity inhibition rate is calculated by the change in absorbance. The color development degree of the reaction solution is linearly related to the sample concentration, which can evaluate the ability of the test sample to inhibit the activity of hyaluronidase, which can be used as one of the evidences for evaluating the soothing effect of the sample.

[0125] 2. Test method: Sodium hyaluronate 0.5mg / mL, acetic acid buffer as solvent. Prepare ascorbic acid as positive control, pure water as negative control, and prepare samples of a certain concentration as test samples. Add positive control / negative control / test sample, hyaluronidase and acetic acid buffer into the test tube; then add CaCl2, sodium hyaluronate, NaOH solution and acetylacetone solution respectively; after boiling water ice bath, let it stand at room temperature; then add color developer to develop color, and measure the absorbance value after standing.

[0126] A: test sample + hyaluronidase;

[0127] B: test sample + acetate buffer;

[0128] C: distilled water + hyaluronidase;

[0129] D: distilled water + acetate buffer;

[0130] The absorbance value was measured at a wavelength of 530 nm. AD ​​was performed in triplicate each time, and the hyaluronidase activity inhibition rates of the positive control, negative control, and test sample were calculated.

[0131] The calculation formula of hyaluronidase activity inhibition rate is:

[0132]

[0133] 3. Results and Conclusions

[0134] The test results of hyaluronidase activity inhibition rate of the test samples, positive controls and negative controls are shown in Table 8-1, Table 8-2 and Table 9 are the test results of hyaluronidase inhibition rate of the application preparations.

[0135] Table 8-1 Example hyaluronidase activity inhibition rate test results

[0136]

[0137] Table 8-2 Comparative Example Hyaluronidase Activity Inhibition Rate Test Results

[0138]

[0139]

[0140] Table 9 Test results of hyaluronidase activity inhibition rate of applied preparations

[0141]

[0142] The positive control can effectively inhibit the activity of hyaluronidase, and the inhibition rate of hyaluronidase activity is ≥20%, and the test system is effective. The standard deviation (Standard Deviation, SD) of the inhibition rate of hyaluronidase activity in each group measured by SD statistics, SD value ≤20%, the parallelism of this test is effective.

[0143] On the basis that the test meets the validity verification, the inhibition rate of hyaluronidase activity of the tested samples is greater than 20%, which is significantly different from the negative control (P<0.05). The results show that under this concentration condition, the tested samples have a soothing effect. Moreover, under the same test concentration, the inhibition rate of hyaluronidase in the embodiment is better than that in the control example; the inhibitory effect of the application preparation with the repair composition on hyaluronidase is significantly better than that of the control example.

[0144] 2. Elastase Inhibition Efficacy Experiment

[0145] 1. Experimental principle: Elastin mainly maintains the integrity and elasticity of the skin structure. The consumption of elastin will cause skin sagging and wrinkles. Therefore, inhibiting the activity of elastase can achieve the purpose of reducing skin sagging. The elastase activity inhibition test is a currently recognized laboratory method for evaluating anti-wrinkle and firming effects. Porcine pancreatic elastase catalyzes the reaction with the substrate. After adding the inhibitor, the absorbance of the enzyme-substrate reaction solution changes. The change value is linearly related to the concentration of the test sample. This can evaluate the ability of the test sample to inhibit the activity of elastase and evaluate the anti-wrinkle and firming effects of the sample and the improvement of skin elasticity.

[0146] 2. Test method: Use tea polyphenols with a concentration of 500 μg / mL as the positive control and pure water as the negative control to prepare samples of a certain concentration as test samples. Accurately weigh 5 mg of N-succinyl-alanine-alanine-alanine-p-nitroaniline and dissolve it in 0.1 M Tris-HCl buffer (pH = 8.0) to prepare a substrate solution.

[0147] Different reagent solutions were added to the 96-well plate, and the plate was gently shaken. After incubation for 30 minutes, the 96-well plate was placed on the detection platform of the microplate reader, and the wavelength was set to 405 nm. The absorbance value was measured and the measurement was repeated three times in parallel.

[0148] The calculation formula of elastase activity inhibition rate is:

[0149]

[0150] A: The average of three absorbance values ​​of the substrate solution;

[0151] B: The average of three absorbance values ​​of the mixed solution of substrate and elastase;

[0152] Cx: average of three absorbance values ​​of the test object;

[0153] Taking tea polyphenols as the positive control, at a concentration of 500μg / mL, the inhibition rate of elastase activity is ≥20%, and the test system is effective. On the basis that the test meets the validity verification, the inhibition rate of elastase activity of the test sample is significantly different from that of the negative control (P<0.05), indicating that the test sample has an inhibitory effect on the activity of elastase at this concentration.

[0154] 3. Results and Conclusions

[0155] The results of the inhibition rate of elastinase activity by the test samples, positive controls and negative controls are shown in Table 10 below.

[0156] Table 10 Elastase inhibition test results

[0157] Test samples Test concentration (%) Inhibition rate (%) P-value Repair Lotion 20 30.52±0.03 <0.05 Comparative Example 1 20 22.98±0.03 <0.05 Repair Cream 20 32.53±0.04 <0.05 Comparative Example 2 20 23.02±0.03 <0.05 Repair Mask 20 34.41±0.01 <0.05 Comparative Example 3 20 29.02±0.03 <0.05 Positive Control / 31.74±0.01 <0.05 Negative control / -0.53±0.02 /

[0158] P<0.05, there was a significant difference between the test sample and the negative control.

[0159] SPSS was used for statistical analysis of the data. An independent sample t-test was used between the groups. The above statistical analyses were all two-tailed tests with a significance level of ɑ=0.05. P>0.05 means there is no significant difference between the two groups; P<0.05 means there is a significant difference between the two groups. On the basis that the test meets the validity verification, the inhibition rate of elastase activity of the test sample is significantly different from that of the negative control (P<0.05), indicating that the test sample can inhibit the activity of elastase at this concentration, and the test sample has the effect of improving skin elasticity, firming and anti-wrinkle. The inhibitory effect of the application preparation with the addition of the repair composition on elastase is better than that of the preparation control.

[0160] Test example: Application preparation safety evaluation and efficacy test

[0161] 3. Safety Assessment

[0162] The soothing and repairing composition of the present invention is composed of 5% to 20% wolfberry fruit extract, 2% to 10% scutellaria root extract, 1.5% to 9% liquorice root extract, and 4.5% to 20% calamine. The recommended addition amount for skin care product formula is 1% to 5%. Calculated based on the maximum addition amount of 5%, the actual maximum content in the final skin care product is 1% wolfberry fruit extract, 0.5% scutellaria root extract, 0.45% liquorice root extract, and 1% calamine. The historical usage of these ingredients in the used cosmetic raw material catalog is shown in Table 11 below. The maximum addition amount of the selected raw materials in the repairing composition is within the range of the historical usage of cosmetics, which is lower than the maximum historical usage in the approved resident cosmetics, and can be used safely. The pesticide residues that may be contained therein are randomly inspected, and the result is that no detection is found.

[0163] Table 11 Historical usage of the repair composition in the "Catalogue of Used Cosmetic Raw Materials" (2021 Edition)

[0164]

[0165] Both the Soothing Repair Lotion and Soothing Repair Night Cream are leave-on cosmetics suitable for the face and neck. According to the relevant provisions of the "Technical Guidelines for Cosmetic Safety Assessment", the various raw materials used in the formula were evaluated, the harmful substances and microorganisms of the products were tested, and the possible risk substances such as dioxane, diethylene glycol, phenol and pesticide residues were evaluated. The test results meet the relevant requirements of the "Technical Specifications for Cosmetic Safety" (2015 edition), and the results show that the products will not cause harm to human health under normal, reasonable and foreseeable use.

[0166] 4. Human Safety Evaluation

[0167] Refer to Chapter 7 of the "Technical Specifications for Safety of Cosmetics" (2015 edition) for human safety test methods for human safety evaluation.

[0168] Test article: Test sample.

[0169] Negative control: blank filter paper control.

[0170] Subjects: A total of 30 subjects, including 4 males and 26 females, age range: 19 to 60 years old, average age 47.00±1.92 years old, met the voluntary inclusion criteria.

[0171] Test method: Select qualified patch test equipment and use the closed patch test method. Place about 0.020g~0.025g (solid) or 0.020mL~0.025mL (liquid) of the test substance in the patch test device, and apply it to the curved side of the subject's forearm with low-allergenic tape. Remove the test substance after 24 hours, and observe the skin reaction at 0.5, 24, and 48 hours after removal. Record the results according to the skin reaction grading standards in the current valid technical specifications, as shown in Table 12.

[0172] Table 12 Skin reaction grading standards for skin occlusive patch test

[0173]

[0174] Results and Conclusions:

[0175] Table 13 summarizes the results of human skin patch tests in human safety evaluation tests. The results showed that no adverse reactions occurred in 30 subjects.

[0176] Table 13

[0177]

[0178] It can be seen from the above test results that the soothing and repairing preparation of the present invention has no adverse reaction to the skin and will not cause irritation to the skin.

[0179] 5. Human efficacy evaluation test

[0180] 1. Detection method

[0181] Healthy Chinese subjects aged 18 to 55 years old with dry skin, self-reported skin sensitivity, positive lactic acid reaction (score ≥ 3 points), skin prone to redness and fever after exposure to ultraviolet rays, and skin barrier damage were selected. Before the subjects used the samples (0d), 14 days after using the samples (14d), and 28 days after using the samples (28d), VISIA-CR and MM100 were used to collect the subjects' facial images, and VC20 Plus was used to collect the subjects' facial images and analyze the cheek roughness parameter (SEr) and smoothness parameter (SEsm). The instruments measured the moisture content of the cheek stratum corneum, transepidermal water loss, skin gloss, skin erythema index EI value, skin oil content, skin elasticity R2 value, skin elasticity R5 value, skin elasticity Q1 value, and skin firmness F4 value. The subjects conducted self-assessment according to the questionnaire, and the data results before and after the use of the samples and the evaluation results were compared by statistical test methods to determine whether there were statistical differences.

[0182] 2. Testing instruments

[0183] The stratum corneum moisture content tester was Corneometer CM 825 (Courage & Khazaka, Germany).

[0184] Skin water loss tester Tewameter TM 300 (Courage & Khazaka, Germany).

[0185] Skin gloss probe Glossymeter GL200 (Courage & Khazaka, Germany).

[0186] Skin melanin and hemoglobin tester Mexameter MX 18 (Courage & Khazaka, Germany).

[0187] Skin elasticity tester Cutometer (Courage & Khazaka, Germany).

[0188] VisioScan VC20 Plus Cutometer (Courage & Khazaka, Germany).

[0189] 3. Detection indicators and parts

[0190] Efficacy test items and sites are shown in Table 14.

[0191] Table 14 Test items and parts

[0192]

[0193]

[0194] 4. Results and Conclusions

[0195] The test results were obtained after 31 healthy Chinese subjects aged 18 to 55 years old, who had dry skin, self-reported skin sensitivity, positive lactic acid reaction (score ≥ 3 points), skin prone to redness and fever after exposure to ultraviolet rays, and skin barrier damage, used the test sample for 28 days. The test results show that the sample has the effects of soothing, repairing, nourishing, and improving skin elasticity. For specific test results, please see Table 15 below, Summary of Human Efficacy Test Results.

[0196] Table 15 Summary of human efficacy test results

[0197]

[0198]

[0199] After using the test sample for 14 days, the moisture content of the stratum corneum on the cheeks of the subjects increased significantly by 29.53% (p<0.001) compared with before use; after using the test sample for 28 days, the moisture content of the stratum corneum on the cheeks of the subjects increased significantly by 47.80% (p<0.001). The trend of the moisture content of the stratum corneum in the test area of ​​the subjects is shown in Figure 1 .

[0200] After using the test sample for 14 days, the transepidermal water loss of the cheek was significantly reduced by 8.19% (p<0.001); after using the test sample for 28 days, the transepidermal water loss of the cheek was significantly reduced by 21.32% (p<0.001). The trend of transepidermal water loss in the test area of ​​the subjects is shown in Figure 2 .

[0201] After using the test sample for 14 days, the glossiness of the cheek skin increased significantly by 10.85% (p<0.001); after using the test sample for 28 days, the glossiness of the cheek skin increased significantly by 14.81% (p<0.001). The trend of the glossiness of the cheek skin in the test area of ​​the subjects is shown in Figure 3 .

[0202] After using the test sample for 14 days, the EI value of the cheek skin erythema index was significantly reduced by 5.69% (p<0.001); after using the test sample for 28 days, the EI value of the cheek skin erythema index was significantly reduced by 8.19% (p<0.001). The trend of the EI value of the skin erythema index in the test area of ​​the subjects is shown in Figure 4 .

[0203] After using the test sample for 14 days, the R2 value of cheek skin elasticity increased significantly by 7.05% (p<0.001) compared with before use; after using the test sample for 28 days, the R2 value of cheek skin elasticity increased significantly by 14.43% (p<0.001). The trend of the R2 value of skin elasticity in the test area of ​​the subjects is shown in Figure 5 .

[0204] After using the test sample for 14 days, the R5 value of cheek skin elasticity increased significantly by 6.06% (p<0.01); after using the test sample for 28 days, the R5 value of cheek skin elasticity increased significantly by 12.02% (p<0.001). The trend of the R5 value of skin elasticity in the test area of ​​the subjects is shown in Figure 6 .

[0205] After using the test sample for 14 days, the Q1 value of cheek skin elasticity increased significantly by 6.66% (p<0.001); after using the test sample for 28 days, the Q1 value of cheek skin elasticity increased significantly by 14.15% (p<0.001). The trend of the Q1 value of skin elasticity in the test area of ​​the subjects is shown in Figure 7 .

[0206] After using the test sample for 14 days, the F4 value of cheek skin firmness was significantly reduced by 6.20% (p<0.001) compared with before use; after using the test sample for 28 days, the F4 value of cheek skin firmness was significantly reduced by 12.00% (p<0.001). The trend of the F4 value of skin firmness in the test area of ​​the subjects is shown in Figure 8 .

[0207] After using the test sample for 14 days, the cheek roughness parameter (SEr) improved by 6.01% compared with before use; after using the test sample for 28 days, the cheek roughness parameter (SEr) improved significantly by 9.42% (p<0.05). See the trend of the skin roughness parameter (SEr) in the test area of ​​the subjects for details. Fig. 9 .

[0208] After using the test sample for 14 days, the cheek smoothness parameter (SEsm) improved by 4.06% compared with before use; after using the test sample for 28 days, the cheek smoothness parameter (SEsm) improved significantly by 13.83% (p<0.001). See the trend of the skin smoothness parameter (SEsm) in the test area of ​​the subjects for details. Fig.10 .

[0209] The above embodiments are only used to illustrate the technical solutions of the present invention, rather than to limit them. Although the present invention has been described in detail with reference to the above embodiments, those skilled in the art should understand that the technical solutions described in the above embodiments may be modified, or some or all of the technical features thereof may be replaced by equivalents, without departing from the spirit and essence of the claims of the present invention; and these modifications or replacements are still within the scope defined by the claims of the present invention.

Claims

1. A repair composition, characterized in that: The invention is prepared from the following raw materials in parts by weight: 5-20 parts of wolfberry fruit, 2-10 parts of scutellaria root, 1.5-9 parts of liquorice root and 4.5-20 parts of calamine.

2. The repair composition according to claim 1, characterized in that The wolfberry fruit is Ningxia wolfberry fruit.

3. The repair composition according to claim 1, characterized in that The calamine is calcined calamine.

4. A method for preparing the repair composition according to any one of claims 1 to 3, characterized in that: The following steps are involved: (1) Weigh the dried Scutellaria baicalensis root and Licorice root according to the formula, crush them, soak them in ethanol, and set aside; (2) weighing wolfberry fruit according to the formula amount, adding it into an extraction tank together with the soaked scutellaria root and liquorice root, and extracting it with ethanol reflux three times, collecting the filtrates, filtering them respectively, and combining them to obtain an extract; (3) concentrating the extract obtained in step (2) to obtain a concentrated solution, spray-drying the concentrated solution into powder, and sieving to obtain a plant extract powder; (4) Drying and sieving the calamine according to the formula amount, and then adding the plant extract powder obtained in step (3) and mixing them thoroughly to obtain a repair composition.

5. The preparation method according to claim 4, characterized in that: In step (1), the ethanol concentration is 40% to 50%.

6. The preparation method according to claim 4, characterized in that: In step (2), 9 to 10 times the amount of ethanol is added for the first time, and the extraction is carried out for 110 minutes; 8 to 10 times the amount of ethanol is added for the second time, and the extraction is carried out for 90 minutes; and 8 to 10 times the amount of ethanol is added for the third time, and the extraction is carried out for 100 minutes.

7. A repair preparation, characterized in that: The invention comprises the repair composition according to any one of claims 1 to 3 or the repair composition prepared by the preparation method according to any one of claims 4 to 6.

8. The repair preparation according to claim 7, characterized in that The repair preparation is a repair lotion, a repair night cream or a repair facial mask.

9. The repair preparation according to claim 7, characterized in that The repair preparation also includes at least one of the following raw materials: Solvents, skin conditioners, thickeners, concealers, skin feel regulators, penetration enhancers, chelating agents, preservatives, humectants, emollients, emulsifiers, antioxidants, fragrances, pH adjusters.

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