Repair nano-emulsion and preparation method thereof
By adding specific ingredients and high-pressure microjet homogenization technology to repair cosmetics, a repair nanoemulsion was prepared, which solved the problems of existing repair products being unfriendly to sensitive skin and poor absorption of active ingredients, and achieved efficient skin repair and moisturizing effects.
Patent Information
- Application Number
- CN202510084471.3
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-01-20
- Publication Date
- 2025-04-18
AI Technical Summary
Existing repair cosmetics are not friendly to sensitive skin, which can easily cause skin blockage and allergic reactions. The active ingredients are poorly absorbed and have poor stability, which cannot effectively solve problems such as dryness, roughness, desquamation and sensitivity of the skin.
Provide a repair nanoemulsion, containing emulsifiers, squalane, emollients, glycerin, butylene glycol, tetrahydromethylpyrimidine carboxylic acid, lycoryl root extract, pineol mixture, sodium stearoyl glutamate, trihydroxy palmitamide hydroxypropyl myristyl ether, fume, rapesterol, safflower oleyl, 5HA hyaluronic acid, sickle-shaped kelp bark extract, cornflower extract, tocopherol, disodium EDTA, flavor, preservative and other components, and is prepared by high-pressure microjet homogenization technology to improve the absorption rate and stability of the components.
This repair nano lotion can effectively inhibit the activity of hyaluronidase, soothe sensitive skin, enhance the skin barrier, improve dry, rough and sensitive skin, reduce allergic reactions, improve the skin's moisturizing and water-locking function, has high stability and is easy to absorb, and is suitable for all skin types.
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Abstract
Description
Technical Field
[0001] The invention relates to the technical field of cosmetic skin care products, and in particular to a repairing nanoemulsion and a preparation method thereof. Background Art
[0002] As time, environment, various living habits, pressure, and physical factors cause skin aging and damage, more and more people are experiencing skin problems such as dry skin, roughness, desquamation, and sensitive skin. In addition, the number of people with sensitive skin is increasing. As people's awareness of skin protection gradually increases, the demand for repair cosmetics is also expanding. There are many repair products on the market, which are basically emulsions made of closed oils, polyol moisturizers, emulsifiers and other ingredients, mainly to improve moisturizing, dryness, and desquamation. However, closed oils are not friendly to sensitive skin and are prone to cause skin blockage, redness, swelling, and itching. Excessive addition of polyols has strong hygroscopicity and is irritating, and cannot provide long-term protection, and cannot solve multiple skin problems such as allergies and sensitive skin. However, the active ingredients of ordinary emulsion cosmetics are not easily absorbed, cannot achieve the expected effect, have poor stability, and the product active ingredients have a high decline rate during the shelf life. Products that have not expired have stratification, discoloration, and taste changes. Summary of the invention
[0003] The present invention provides a repairing nanoemulsion and a preparation method thereof. The nanoemulsion can help absorb active ingredients, improve skin dryness, roughness, desquamation, sensitivity and other problems, enhance the skin's water-locking ability, and repair the skin barrier.
[0004] In order to solve the above problems, the technical solution adopted by the present invention is as follows:
[0005] In a first aspect, the present invention provides a repairing nanoemulsion, comprising the following components in percentage by weight: 1.0-5.0% of emulsifier, 1.0-5.0% of squalane, 2.0-10.0% of emollient, 3.0-10.0% of glycerin, 3.0-10.0% of butylene glycol, 0.5-3.0% of tetrahydromethylpyrimidine carboxylic acid, 0.5-3.0% of vetiver root extract, 0.5-3.0% of soft hair pine algae mixture, 0.5-3.0% of sodium stearoyl glutamate, 0.5-3.0% of trihydroxypalmitamidohydroxypropyl Myristyl ether 0.1-1.0%, fumonisin 0.1-1.0%, rape sterols 0.1-1.0%, safflower oil body 0.1-1.0%, 5HA hyaluronic acid 0.1-1.0%, sickle pod tree bark extract 0.05-0.5%, cornflower flower extract 0.05-0.5%, tocopherol 0.1-1.0%, disodium EDTA 0.03-0.2%, flavor 0.03-0.1%, preservative 0.5-2.0%, deionized water to 100%.
[0006] Specifically, the emulsifier is one or more of olive oil polyglycerol-6 esters, watermelon seed oil polyglycerol-6 esters, wild almond oil polyglycerol-6 esters, polyglyceryl-3 methyl glucose distearate, polyglyceryl-10 oleate, polyglyceryl-10 laurate and polyglyceryl-10 myristate.
[0007] Specifically, the emollient is one or more of arachidyl alcohol, hydrogenated rapeseed alcohol, neopentyl glycol diheptanoate, vegetable palm oil, Alnus macrophylla seed oil, hop cone oil, Camellia purslane seed oil, Malus domestica seed oil, cholesterol hydroxystearate, phytosteryl macadamia oleate, sunflower seed oil, isononyl isononanoate, triethylhexanoin, dicaprylyl carbonate and C10-40 isoalkanoic acid cholesterol esters.
[0008] Specifically, the vetiver root extract contains 25.0-50.0% 1,3-propylene glycol and 25.0-50.0% water by weight;
[0009] The preparation process of the vetiver root extract is as follows:
[0010] 1) Select the root of Vetiver, clean and dry it, grind it into 20-40 mesh size for later use;
[0011] 2) adding vetiver root and water in a mass ratio of 1:50-60 into a container, soaking for 30-60 minutes, and homogenizing with a high-speed homogenizer at a speed of 12000-15000 r / min for 180-240 seconds to obtain a mixture I;
[0012] 3) Weigh 1,3-propylene glycol in a mass ratio of 1:50-60 to vetiver root and add it to mixture I, and stir at a speed of 25-30 r / min for 45-60 minutes to obtain mixture II;
[0013] 4) homogenizing the mixture II once through a high-pressure homogenizer with a working pressure of 350 to 500 bar, and then circulating the homogenized mixture through a high-pressure homogenizer with a working pressure of 800 to 1000 bar for two times;
[0014] 5) The homogenized mixture was centrifuged at 20,000 r / min for 20 minutes using a low-temperature micro-table centrifuge, and the upper clear liquid was taken to obtain the vetiver root extract.
[0015] Specifically, the tricholoma pubescens mixture is obtained by a low-temperature homogenization preparation process, and comprises the following components in weight percentage: 1.0-3.0% of tricholoma pubescens extract, 8.0-12.0% of 1,2-pentanediol, and up to 100% of water.
[0016] Specifically, the Yufuan includes the following components in weight percentage: 49.0-55.0% glycerin, 10-25% butylene glycol, 5.0-10.0% eyebright extract, 1.0-5.0% lemon balm leaf extract, 0.1-1.0% primula bud / flower extract, 0.8-1.0% lecithin, 0.3-0.5% potassium sorbate, and 16.9-23.85% water.
[0017] Specifically, the 5HA hyaluronic acid includes the following components in weight percentage: 0.5-2.0% sodium hyaluronate, 0.1-1.0% dimethylsilanol hyaluronate, 0.1-1.0% sodium dimethylsilanol hyaluronate, 0.1-1.0% sodium hyaluronate cross-linked polymer, 0.1-1.0% hydrolyzed sodium hyaluronate, 0.5-1.0% phenoxyethanol, 0.05-0.1% ethylhexylglycerin, and water to 100%.
[0018] Specifically, the falcaria bark extract contains 90.0% maltodextrin by weight; and the cornflower flower extract contains 80% maltodextrin by weight.
[0019] Specifically, the preservative is one or more of phenoxyethanol, 1,2-hexanediol, p-hydroxyacetophenone, glyceryl undecylenate, phenoxyethanol, caprylhydroxamic acid, glyceryl caprylate, ethylhexylglycerin, 1,2-pentanediol, caprylyl glycol, glyceryl caprate, camphor bark oil, Melaleuca alternifolia leaf oil, Zanthoxylum bungeanum fruit extract, hops cone oil, and vanilla flat fruit oil.
[0020] In a second aspect, the present invention provides a method for preparing the repair nanoemulsion according to the first aspect, comprising the following steps:
[0021] 1) Emulsifiers, squalane, emollients, rape sterols, safflower oleosomes, and tocopherol are classified as raw materials in group A; deionized water, disodium EDTA, glycerin, butylene glycol, and sodium stearoyl glutamate are classified as raw materials in group B; tetrahydromethylpyrimidine carboxylic acid and trihydroxypalmitamidohydroxypropyl myristyl ether are classified as raw materials in group C; vetiver root extract, pine algae extract, Yufuan, and 5HA hyaluronic acid are classified as raw materials in group D; sicklewood bark extract and cornflower flower extract are classified as raw materials in group E; preservatives and flavors are classified as raw materials in group E;
[0022] 2) Add the raw materials of group A into the oil tank, stir and heat to 75-80°C at a speed of 20-25 r / min for use, and obtain the dissolved raw materials of group A for use;
[0023] 3) Add the raw materials of group B to the aqueous phase, stir at a speed of 30-35 r / min and homogenize at a speed of 3000-3500 r / min for 60-90 seconds, heat to 83-85° C. for standby use, and obtain the heated raw materials of group B;
[0024] 4) Pump the heated raw materials of group B into the emulsifying pot, stir at a speed of 30-35 r / min and keep the temperature constant at 83-85°C, then pump the dissolved raw materials of group A into the emulsifying pot, and homogenize at a speed of 5000-6000 r / min for 8-15 minutes;
[0025] 5) The material in the emulsifier begins to cool down. During this process, it is stirred at a speed of 30 to 35 r / min and vacuumed to -0.03 to -0.05 MPa;
[0026] 6) When the temperature of the material in the emulsification pot drops to 42-48°C, add the components in Group C into the emulsification pot one by one, stir at 30-35r / min for 8-15 minutes, and evacuate to -0.03-0.05Mpa;
[0027] 7) Add the components in group D into the emulsifying pot one by one according to the order of division, stir at 30-35 r / min for 8-10 minutes, and evacuate to -0.03-0.05 MPa;
[0028] 8) Add each component in the raw material of group E into the emulsifying pot one by one, stir at a speed of 30-35 r / min for 12-15 minutes, and evacuate to -0.03-0.05 MPa;
[0029] 9) Add each component in group F into the emulsifying pot one by one, stir at 30-35 r / min and homogenize at 3000-3500 r / min for 30-90 seconds, stir for 12-15 minutes, and evacuate to -0.03-0.05 Mpa;
[0030] 10) After the physical and chemical indicators are tested to be qualified, the material is filtered out to obtain the initially prepared emulsion for use;
[0031] 11) The working pressure of the high-pressure microfluidizer is adjusted to 20,000-30,000 psi, and the preliminarily prepared emulsion is added to the high-pressure microfluidizer for cyclic homogenization for 3 times to obtain a repair nanoemulsion.
[0032] Compared with the prior art, the present invention has the following beneficial effects:
[0033] 1) The tetrahydromethylpyrimidine carboxylic acid provided by the present invention works in coordination with the vetiver root extract to effectively inhibit the activity of hyaluronidase, soothe sensitive skin, repair skin inflammation and allergic symptoms, strengthen the damaged skin barrier, and resist the damage of the external environment to the skin.
[0034] 2) The tetrahydromethylpyrimidine carboxylic acid provided by the present invention and the rape sterols act synergistically to improve dry, rough and sensitive skin, enhance the moisturizing and water-locking function of dry skin, reduce allergic reactions caused by inflammation, improve skin allergies caused by seasonality and environment, and enhance the barrier function of the skin.
[0035] 3) The synergistic effect of the pine algae extract provided by the present invention and Yufuan can effectively inhibit the activity of hyaluronidase, improve the soothing and anti-inflammatory effects on symptoms such as redness, dryness, and itching of sensitive skin, and help the skin to be stimulated and repaired by environmental and seasonal changes.
[0036] 4) The trihydroxypalmitamide hydroxypropyl myristyl ether, the falcate sappanwood bark extract, and the cornflower flower extract provided by the present invention work synergistically to quickly relieve symptoms such as burning, pain, and itching of sensitive skin, inhibit inflammatory response and release, and inhibit erythema formation; regulate the skin immune system, inhibit lymphocytes from moisturizing the skin tissue, and reduce the skin's sensitivity to stimulation.
[0037] 5) The ectoine and 5HA hyaluronic acid provided by the present invention work in coordination to improve skin hydration, maintain skin elasticity, reduce damage to the skin caused by external pressure, increase skin moisturizing, relieve dry, rough, and sensitive skin, maintain moisture in the skin, and increase the skin repair barrier.
[0038] 6) The ectoine and cornflower extract provided by the present invention work in coordination to regulate the activity of TRPV1 nerve receptors, reduce the flow of calcium in the cell membrane, restore the sensitivity of the skin to normal levels, reduce the tingling sensation of the skin, relieve the excessive reaction of the skin, and reduce sensitive symptoms.
[0039] 7) The repairing nanoemulsion of the present invention has high stability and is easily absorbed. It can improve skin dryness, roughness, desquamation, sensitivity and other problems, enhance the skin's ability to lock water, repair the skin barrier, and has a simple preparation method, which is conducive to industrial production and has a good market prospect.
[0040] In order to make the above-mentioned objects, features and advantages of the present invention more obvious and easy to understand, the embodiments of the present invention are specifically cited below and described in detail as follows. DETAILED DESCRIPTION
[0041] In order to make the purpose, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. Obviously, the described embodiments are only part of the embodiments of the present invention, rather than all the embodiments.
[0042] The technical standards of the repair nanoemulsion product prepared in the embodiment of the present invention are as follows:
[0043] Appearance: White to light yellow flowable emulsion;
[0044] pH: 5.0-7.0;
[0045] Centrifugal test: 2000r / min, 30min, no oil-water separation;
[0046] Stability (cold resistance): kept in a (-8±2)℃ refrigerator for 24 hours, there is no significant difference after returning to room temperature;
[0047] Stability (heat resistance): After being kept in a (40±1)℃ constant temperature box for 24 hours, there is no significant difference between the test results and those before the test after returning to room temperature;
[0048] Total colony count: <10CFU / g;
[0049] Mold and yeast: <10CFU / g;
[0050] Thermotolerant coliform bacteria: shall not be detected;
[0051] Staphylococcus aureus: shall not be detected;
[0052] Pseudomonas aeruginosa: shall not be detected;
[0053] Heavy metals (lead ≤ 10 mg / kg, mercury ≤ 1 mg / kg, arsenic ≤ 2 mg / kg, cadmium ≤ 5 mg / kg, dioxane ≤ 1 mg / kg).
[0054] Example 1
[0055] This embodiment prepares the repair nanoemulsion, using the following weight percentage components:
[0056] Emulsifier 3.0%, squalane 3.0%, emollient 5.5%, glycerin 5.0%, butylene glycol 3.5%, tetrahydromethylpyrimidine carboxylic acid 1.0%, vetiver root extract 1.0%, soft hair pine algae mixture 3.0%, sodium stearoyl glutamate 1.2%, trihydroxypalmitamido hydroxypropyl myristyl ether 1.0%, fucosan 0.5%, rapeseed sterols 1.0%, safflower oleosomes 0.1%, 5HA hyaluronic acid 0.2%, sickle pod bark extract 0.1%, cornflower flower extract 0.5%, tocopherol (vitamin E) 0.1%, disodium EDTA 0.03%, fragrance 0.03%, preservative 2.0%, deionized water to 100%.
[0057] The emulsifier is olive oil polyglycerol-6 ester and polyglycerol-10 laurate, which are mixed in a mass ratio of 1:2.
[0058] The emollient is hydrogenated rapeseed alcohol, neopentyl glycol diheptanoate, crabapple seed oil, and dicaprylyl carbonate, which are used in a mass ratio of 0.5:3:3:2.
[0059] Vetiver root extract contains 49.5% 1,3-propylene glycol and 50.0% water by weight. The preparation process of vetiver root extract is as follows:
[0060] 1) Select the root of Vetiver, clean and dry it, grind it into 20 mesh size for later use;
[0061] 2) adding vetiver root and water in a mass ratio of 1:50 into a container, soaking for 30 minutes, and homogenizing with a high-speed homogenizer at a speed of 12000 r / min for 180 seconds to obtain a mixture I;
[0062] 3) Weigh 1,3-propylene glycol in a mass ratio of 1:50 to vetiver root and add it to mixture I, and stir at a speed of 25 r / min for 45 minutes to obtain mixture II;
[0063] 4) homogenizing the mixture II once through a high-pressure homogenizer at a working pressure of 350 bar, and then circulating the homogenized mixture through a high-pressure homogenizer at a working pressure of 800 bar for two times;
[0064] 5) The homogenized mixture was centrifuged at 20,000 r / min for 20 minutes using a low-temperature micro-table centrifuge, and the upper clear liquid was taken to obtain the vetiver root extract.
[0065] The tricholoma pubescens mixture is obtained by adopting a low-temperature homogenization preparation process, and comprises the following components in weight percentage: 3.0% of tricholoma pubescens extract, 12.0% of 1,2-pentanediol, and water to 100%.
[0066] Yufuan includes the following components in weight percentage: 52.2% glycerin, 20% butylene glycol, 6.0% eyebright extract, 1.0% lemon balm leaf extract, 0.1% primula bud / flower extract, 0.8% lecithin, 0.4% potassium sorbate, and 19.5% water.
[0067] 5HA hyaluronic acid includes the following components in weight percentage: sodium hyaluronate 1.0%, dimethylsilanol hyaluronate 0.2%, dimethylsilanol hyaluronate sodium 1.0%, sodium hyaluronate cross-polymer 0.1%, hydrolyzed sodium hyaluronate 0.5%, phenoxyethanol 0.5%, ethylhexylglycerin 0.06%, water to 100%.
[0068] The extract of the bark of the falcate sappan wood contains 90.0% maltodextrin by weight; and the extract of the cornflower flower contains 80% maltodextrin by weight.
[0069] The preservatives are 1,2-hexanediol, ethylhexylglycerin, glyceryl caprate, camphor bark oil, and hop cone oil, which are mixed in a mass ratio of 5:0.2:1:1:1.
[0070] The method for preparing the repair nanoemulsion in this embodiment comprises the following steps:
[0071] 1) Emulsifiers, squalane, emollients, rape sterols, safflower oleosomes, and tocopherol are classified as raw materials in group A; deionized water, disodium EDTA, glycerin, butylene glycol, and sodium stearoyl glutamate are classified as raw materials in group B; tetrahydromethylpyrimidine carboxylic acid and trihydroxypalmitamidohydroxypropyl myristyl ether are classified as raw materials in group C; vetiver root extract, pine algae extract, Yufuan, and 5HA hyaluronic acid are classified as raw materials in group D; sicklewood bark extract and cornflower flower extract are classified as raw materials in group E; preservatives and flavors are classified as raw materials in group E;
[0072] 2) Add the raw materials of group A into the oil tank, stir and heat to 80°C at a speed of 25 r / min for later use, and obtain the dissolved raw materials of group A for later use;
[0073] 3) Add the raw materials of group B into the water phase, stir at a speed of 30 r / min and homogenize at a speed of 3000 r / min for 90 seconds, heat to 83° C. for standby use, and obtain the heated raw materials of group B;
[0074] 4) Pump the heated raw materials of group B into the emulsifying pot, stir at a speed of 35r / min and keep the temperature constant at 83°C, then pump the dissolved raw materials of group A into the emulsifying pot, and homogenize at a speed of 6000r / min for 8 minutes;
[0075] 5) The material in the emulsifier begins to cool down. During this process, it is stirred at 35r / min and vacuumed to -0.03Mpa;
[0076] 6) When the temperature of the material in the emulsification pot drops to 48°C, add each component in the raw material group C into the emulsification pot one by one, stir at 30r / min for 15 minutes, and evacuate to -0.03Mpa;
[0077] 7) Add the components in group D into the emulsifying pot one by one according to the order of division, stir at 35 r / min for 8 minutes, and evacuate to -0.05 MPa;
[0078] 8) Add each component in group E into the emulsifying pot one by one, stir at 30 r / min for 15 minutes, and evacuate to -0.03 Mpa;
[0079] 9) Add each component in group F into the emulsifying pot one by one, stir at 35 r / min and homogenize at 3500 r / min for 90 seconds, stir for 12 minutes, and evacuate to -0.05 Mpa;
[0080] 10) After the physical and chemical indicators are tested to be qualified, the material is filtered out to obtain the initially prepared emulsion for use;
[0081] 11) The working pressure of the high-pressure microfluidizer was adjusted to 20,000 psi, and the preliminarily prepared emulsion was added to the high-pressure microfluidizer for 3 cycles of homogenization to obtain a repair nanoemulsion.
[0082] Example 2
[0083] Emulsifier 2.0%, squalane 2.5%, emollient 6.0%, glycerin 4.0%, butylene glycol 6.0%, tetrahydromethylpyrimidine carboxylic acid 3.0%, vetiver root extract 0.5%, soft hair pine algae mixture 0.5%, sodium stearoyl glutamate 2.0%, trihydroxypalmitamido hydroxypropyl myristyl ether 0.6%, fucosan 0.3%, rapeseed sterols 0.1%, safflower oil body 0.3%, 5HA hyaluronic acid 0.5%, sickle pod sappan bark extract 0.2%, cornflower flower extract 0.05%, tocopherol (vitamin E) 0.6%, disodium EDTA 0.2%, fragrance 0.05%, preservative 1.0%, deionized water to 100%.
[0084] The emulsifier is watermelon seed oil polyglycerol-6 esters, wild almond oil polyglycerol-6 esters, and polyglycerol-10 myristic acid ester, which are mixed and used in a mass ratio of 1:1:2.
[0085] The emollient is arachidyl alcohol, vegetable palm oil, Alnus macrophylla seed oil, phytosteryl macadamia oleate, and triethylhexanoin, which are used in a mass ratio of 1:1:1:1:5.
[0086] Vetiver root extract contains 50.0% 1,3-propylene glycol and 49.2% water by weight. The preparation process of Vetiver root extract is as follows:
[0087] 1) Select the root of Vetiver, clean and dry it, grind it into 40 mesh size for later use;
[0088] 2) adding vetiver root and water in a mass ratio of 1:60 into a container, soaking for 60 minutes, and homogenizing with a high-speed homogenizer at a speed of 15000 r / min for 240 seconds to obtain a mixture I;
[0089] 3) Weigh 1,3-propylene glycol in a mass ratio of 1:60 to vetiver root and add it to mixture I, and stir at a speed of 30 r / min for 60 minutes to obtain mixture II;
[0090] 4) homogenizing the mixture II once through a high-pressure homogenizer at a working pressure of 500 bar, and then circulating the homogenized mixture through a high-pressure homogenizer at a working pressure of 1000 bar for two times;
[0091] 5) The homogenized mixture was centrifuged at 20,000 r / min for 20 minutes using a low-temperature micro-table centrifuge, and the upper clear liquid was taken to obtain the vetiver root extract.
[0092] The tricholoma pubescens mixture is obtained by adopting a low-temperature homogenization preparation process, and comprises the following components in weight percentage: 1.0% of tricholoma pubescens extract, 8.0% of 1,2-pentanediol, and water to 100%.
[0093] Yufuan includes the following components in weight percentage: 49.0% glycerin, 25.0% butylene glycol, 5.0% eyebright extract, 1.0% lemon balm leaf extract, 1.0% formosan clover bud / flower extract, 1.0% lecithin, 0.5% potassium sorbate, and 17.5% water.
[0094] 5HA hyaluronic acid includes the following components in weight percentage: 2.0% sodium hyaluronate, 0.1% dimethylsilanol hyaluronate, 0.2% sodium dimethylsilanol hyaluronate, 0.15% sodium hyaluronate cross-polymer, 0.2% hydrolyzed sodium hyaluronate, 1.0% phenoxyethanol, 0.1% ethylhexylglycerin, and water to 100%.
[0095] The extract of the bark of the falcate sappan wood contains 90.0% maltodextrin by weight; and the extract of the cornflower flower contains 80% maltodextrin by weight.
[0096] The preservative is phenoxyethanol, Melaleuca alternifolia leaf oil, and Vanilla planifolia fruit oil, which are mixed in a mass ratio of 1:1:1.
[0097] The method for preparing the repair nanoemulsion in this embodiment comprises the following steps:
[0098] 1) Emulsifiers, squalane, emollients, rape sterols, safflower oleosomes, and tocopherol are classified as raw materials in group A; deionized water, disodium EDTA, glycerin, butylene glycol, and sodium stearoyl glutamate are classified as raw materials in group B; tetrahydromethylpyrimidine carboxylic acid and trihydroxypalmitamidohydroxypropyl myristyl ether are classified as raw materials in group C; vetiver root extract, pine algae extract, Yufuan, and 5HA hyaluronic acid are classified as raw materials in group D; sicklewood bark extract and cornflower flower extract are classified as raw materials in group E; preservatives and flavors are classified as raw materials in group E;
[0099] 2) Add the raw materials of group A into the oil tank, stir and heat to 80°C at a speed of 20 r / min for use, and obtain the dissolved raw materials of group A for use;
[0100] 3) Add the raw materials of group B into the water phase, stir at a speed of 30 r / min and homogenize at a speed of 3500 r / min for 60 seconds, heat to 85° C. for standby use, and obtain the heated raw materials of group B;
[0101] 4) Pump the heated raw materials of group B into the emulsifying pot, stir at a speed of 30r / min and keep the temperature constant at 85°C, then pump the dissolved raw materials of group A into the emulsifying pot, and homogenize at a speed of 5000r / min for 15 minutes;
[0102] 5) The material in the emulsifier begins to cool down. During this process, it is stirred at a speed of 30r / min and vacuumed to -0.05Mpa;
[0103] 6) When the temperature of the material in the emulsification pot drops to 42°C, add the components in group C into the emulsification pot one by one, stir at 30r / min for 15 minutes, and evacuate to -0.03Mpa;
[0104] 7) Add the components in group D into the emulsifying pot one by one according to the order of division, stir at 35 r / min for 8 minutes, and evacuate to -0.03 Mpa;
[0105] 8) Add each component in group E into the emulsifying pot one by one, stir at 30 r / min for 15 minutes, and evacuate to -0.05 MPa;
[0106] 9) Add each component in group F into the emulsifying pot one by one, stir at 35 r / min and homogenize at 3000 r / min for 50 seconds, stir for 15 minutes, and evacuate to -0.03 Mpa;
[0107] 10) After the physical and chemical indicators are tested to be qualified, the material is filtered out to obtain the initially prepared emulsion for use;
[0108] 11) The working pressure of the high-pressure microfluidizer was adjusted to 30,000 psi, and the preliminarily prepared emulsion was added to the high-pressure microfluidizer for 3 cycles of homogenization to obtain a repair nanoemulsion.
[0109] Example 3
[0110] Emulsifier 5.0%, squalane 5.0%, emollient 8.0%, glycerin 8.0%, butylene glycol 3.0%, tetrahydromethylpyrimidine carboxylic acid 0.5%, vetiver root extract 3.0%, soft hair pine algae mixture 2.0%, sodium stearoyl glutamate 0.5%, trihydroxypalmitamido hydroxypropyl myristyl ether 0.1%, fucosan 0.1%, rape sterols 0.5%, safflower oil body 0.5%, 5HA hyaluronic acid 0.1%, sickle pod bark extract 0.05%, cornflower flower extract 0.3%, tocopherol (vitamin E) 1.0%, disodium EDTA 0.1%, flavor 0.05%, preservative 0.5%, deionized water to 100%.
[0111] The emulsifier is wild almond oil polyglycerol-6 esters and polyglycerol-3 methyl glucose distearate, which are mixed in a mass ratio of 1:2.
[0112] The emollient is a composite of vegetable Etta palm fruit oil, Alnus macrophylla seed oil, cholesterol hydroxystearate, and sunflower seed oil in a mass ratio of 1:1:0.5:1.
[0113] Vetiver root extract contains 25.0% 1,3-propylene glycol and 25.0% water by weight. The preparation process of Vetiver root extract is as follows:
[0114] 1) Select the root of Vetiver, clean and dry it, grind it into 30 mesh size for later use;
[0115] 2) adding vetiver root and water in a mass ratio of 1:55 into a container, soaking for 45 minutes, and homogenizing with a high-speed homogenizer at a speed of 13500 r / min for 210 seconds to obtain a mixture I;
[0116] 3) Weigh 1,3-propylene glycol in a mass ratio of 1:55 to vetiver root and add it to mixture I, and stir at a speed of 28 r / min for 53 minutes to obtain mixture II;
[0117] 4) homogenizing the mixture II once through a high-pressure homogenizer at a working pressure of 420 bar, and then circulating the homogenized mixture through a high-pressure homogenizer at a working pressure of 900 bar for two times;
[0118] 5) The homogenized mixture was centrifuged at 20,000 r / min for 20 minutes using a low-temperature micro-table centrifuge, and the upper clear liquid was taken to obtain the vetiver root extract.
[0119] The tricholoma pubescens mixture is obtained by adopting a low-temperature homogenization preparation process, and comprises the following components in weight percentage: 2.0% of tricholoma pubescens extract, 10.0% of 1,2-pentanediol, and water to 100%.
[0120] Yufuan includes the following components in weight percentage: 55.0% glycerin, 15.0% butylene glycol, 10.0% eyebright extract, 2.0% lemon balm leaf extract, 0.8% primula bud / flower extract, 0.8% lecithin, 0.3% potassium sorbate, and 16.9% water.
[0121] 5HA hyaluronic acid includes the following components in weight percentage: sodium hyaluronate 0.5%, dimethylsilanol hyaluronate 0.5%, dimethylsilanol hyaluronate sodium 0.8%, sodium hyaluronate cross-polymer 0.1%, hydrolyzed sodium hyaluronate 0.1%, phenoxyethanol 0.63%, ethylhexylglycerin 0.07%, water to 100%.
[0122] The extract of the bark of the falcate sappan wood contains 90.0% maltodextrin by weight; and the extract of the cornflower flower contains 80% maltodextrin by weight.
[0123] The preservatives are phenoxyethanol, ethylhexylglycerin, and Melaleuca alternifolia leaf oil, which are mixed in a mass ratio of 1:0.1:0.5.
[0124] The method for preparing the repair nanoemulsion in this embodiment comprises the following steps:
[0125] 1) Emulsifiers, squalane, emollients, rape sterols, safflower oleosomes, and tocopherol are classified as raw materials in group A; deionized water, disodium EDTA, glycerin, butylene glycol, and sodium stearoyl glutamate are classified as raw materials in group B; tetrahydromethylpyrimidine carboxylic acid and trihydroxypalmitamidohydroxypropyl myristyl ether are classified as raw materials in group C; vetiver root extract, pine algae extract, Yufuan, and 5HA hyaluronic acid are classified as raw materials in group D; sicklewood bark extract and cornflower flower extract are classified as raw materials in group E; preservatives and flavors are classified as raw materials in group E;
[0126] 2) Add the raw materials of group A into the oil tank, stir and heat to 78°C at a speed of 23 r / min for standby use, and obtain the dissolved raw materials of group A for standby use;
[0127] 3) Add the raw materials of group B into the water phase, stir at a speed of 33 r / min and homogenize at a speed of 3300 r / min for 75 seconds, heat to 84° C. for standby use, and obtain the heated raw materials of group B;
[0128] 4) Pump the heated raw materials of group B into the emulsifying pot, stir at a speed of 33 r / min and keep the temperature constant at 84°C, then pump the dissolved raw materials of group A into the emulsifying pot, and homogenize at a speed of 5500 r / min for 10 minutes;
[0129] 5) The material in the emulsifier begins to cool down. During this process, it is stirred at 33r / min and vacuumed to -0.04Mpa;
[0130] 6) When the temperature of the material in the emulsification pot drops to 45°C, add the components in group C into the emulsification pot one by one, stir at 33r / min for 12 minutes, and evacuate to -0.04Mpa;
[0131] 7) Add the components in group D into the emulsifying pot one by one according to the order of division, stir at 32 r / min for 9 minutes, and evacuate to -0.04 Mpa;
[0132] 8) Add each component in group E into the emulsifying pot one by one, stir at 33 r / min for 13 minutes, and evacuate to -0.04 Mpa;
[0133] 9) Add each component in group F into the emulsifying pot one by one, stir at 33 r / min and homogenize at 3300 r / min for 60 seconds, stir for 13 minutes, and evacuate to -0.04 Mpa;
[0134] 10) After the physical and chemical indicators are tested to be qualified, the material is filtered out to obtain the initially prepared emulsion for use;
[0135] 11) The working pressure of the high-pressure microfluidizer was adjusted to 25000 psi, and the preliminarily prepared emulsion was added to the high-pressure microfluidizer for cyclic homogenization for 3 times to obtain a repair nanoemulsion.
[0136] Example 4
[0137] Emulsifier 4.0%, squalane 1.0%, emollient 10.0%, glycerin 3.0%, butylene glycol 7.0%, tetrahydromethylpyrimidine carboxylic acid 1.5%, vetiver root extract 2.0%, soft hair pine algae mixture 1.5%, sodium stearoyl glutamate 1.0%, trihydroxypalmitamido hydroxypropyl myristyl ether 0.3%, fucosan 0.2%, rape sterols 0.6%, safflower oleosomes 1.0%, 5HA hyaluronic acid 1.0%, sickle pod bark extract 0.3%, cornflower flower extract 0.4%, tocopherol (vitamin E) 0.5%, disodium EDTA 0.05%, fragrance 0.1%, preservative 1.5%, deionized water to 100%.
[0138] The emulsifier is polyglycerol-10 oleate and polyglycerol-10 myristic acid ester, which are mixed in a mass ratio of 1:2.
[0139] The emollient is neopentyl glycol diheptanoate, Alnus macrophylla seed oil, Camellia oleifera seed oil, cholesterol hydroxystearate, and C10-40 isoalkanoic acid cholesterol ester, which are used in a composite manner in a mass ratio of 1:0.5:0.5:0.5:1.
[0140] Vetiver root extract contains 50.0% 1,3-propylene glycol and 49.7% water by weight. The preparation process of Vetiver root extract is as follows:
[0141] 1) Select the root of Vetiver, clean and dry it, grind it into 40 mesh size for later use;
[0142] 2) adding vetiver root and water in a mass ratio of 1:60 into a container, soaking for 50 minutes, and homogenizing with a high-speed homogenizer at a speed of 13000 r / min for 200 seconds to obtain a mixture I;
[0143] 3) Weigh 1,3-propylene glycol in a mass ratio of 1:58 to vetiver root and add it to mixture I, and stir at a speed of 28 r / min for 60 minutes to obtain mixture II;
[0144] 4) homogenizing the mixture II once through a high-pressure homogenizer at a working pressure of 400 bar, and then circulating the homogenized mixture through a high-pressure homogenizer at a working pressure of 850 bar for two times;
[0145] 5) The homogenized mixture was centrifuged at 20,000 r / min for 20 minutes using a low-temperature micro-table centrifuge, and the upper clear liquid was taken to obtain the vetiver root extract.
[0146] The tricholoma pubescens mixture is obtained by adopting a low-temperature homogenization preparation process, and comprises the following components in weight percentage: 3.0% of tricholoma pubescens extract, 12.0% of 1,2-pentanediol, and water to 100%.
[0147] Yufuan includes the following components in weight percentage: 50.0% glycerin, 10.0% butylene glycol, 9.0% eyebright extract, 5.0% lemon balm leaf extract, 0.8% formosan clover bud / flower extract, 1.0% lecithin, 0.35% potassium sorbate, and 23.85% water.
[0148] 5HA hyaluronic acid includes the following components in weight percentage: 1.0% sodium hyaluronate, 0.2% dimethylsilanol hyaluronate, 0.15% sodium dimethylsilanol hyaluronate, 0.3% sodium hyaluronate cross-polymer, 0.2% hydrolyzed sodium hyaluronate, 0.73% phenoxyethanol, 0.07% ethylhexylglycerin, and water to 100%.
[0149] The extract of the bark of the falcate sappan wood contains 90.0% maltodextrin by weight; and the extract of the cornflower flower contains 80% maltodextrin by weight.
[0150] The preservatives are phenoxyethanol, 1,2-hexanediol, and Zanthoxylum bungeanum fruit extract, which are mixed in a mass ratio of 1:1:0.2.
[0151] The method for preparing the repair nanoemulsion in this embodiment comprises the following steps:
[0152] 1) Emulsifiers, squalane, emollients, rape sterols, safflower oleosomes, and tocopherol are classified as raw materials in group A; deionized water, disodium EDTA, glycerin, butylene glycol, and sodium stearoyl glutamate are classified as raw materials in group B; tetrahydromethylpyrimidine carboxylic acid and trihydroxypalmitamidohydroxypropyl myristyl ether are classified as raw materials in group C; vetiver root extract, pine algae extract, Yufuan, and 5HA hyaluronic acid are classified as raw materials in group D; sicklewood bark extract and cornflower flower extract are classified as raw materials in group E; preservatives and flavors are classified as raw materials in group E;
[0153] 2) Add the raw materials of group A into the oil tank, stir and heat to 80°C at a speed of 25 r / min for later use, and obtain the dissolved raw materials of group A for later use;
[0154] 3) Add the raw materials of group B into the water phase, stir at a speed of 35 r / min and homogenize at a speed of 3500 r / min for 90 seconds, heat to 85° C. for standby use, and obtain the heated raw materials of group B;
[0155] 4) Pump the heated raw materials of group B into the emulsifying pot, stir at a speed of 35r / min and keep the temperature constant at 85°C, then pump the dissolved raw materials of group A into the emulsifying pot, and homogenize at a speed of 6000r / min for 15 minutes;
[0156] 5) The material in the emulsifier begins to cool down. During this process, it is stirred at 35r / min and vacuumed to -0.05Mpa;
[0157] 6) When the temperature of the material in the emulsification pot drops to 48°C, add each component in the raw material group C into the emulsification pot one by one, stir at 35r / min for 15 minutes, and evacuate to -0.05Mpa;
[0158] 7) Add the components in group D into the emulsifying pot one by one according to the order of division, stir at 35 r / min for 10 minutes, and evacuate to -0.05 MPa;
[0159] 8) Add each component in group E into the emulsifying pot one by one, stir at 35 r / min for 15 minutes, and evacuate to -0.05 MPa;
[0160] 9) Add each component in group F into the emulsifying pot one by one, stir at 35 r / min and homogenize at 3500 r / min for 90 seconds, stir for 15 minutes, and evacuate to -0.05 Mpa;
[0161] 10) After the physical and chemical indicators are tested to be qualified, the material is filtered out to obtain the initially prepared emulsion for use;
[0162] 11) The working pressure of the high-pressure microfluidizer was adjusted to 30,000 psi, and the preliminarily prepared emulsion was added to the high-pressure microfluidizer for 3 cycles of homogenization to obtain a repair nanoemulsion.
[0163] Example 5
[0164] Emulsifier 1.0%, squalane 3.5%, emollient 2.0%, glycerin 10.0%, butylene glycol 10.0%, tetrahydromethylpyrimidine carboxylic acid 2.0%, vetiver root extract 0.5%, soft hair pine algae mixture 1.0%, sodium stearoyl glutamate 3.0%, trihydroxypalmitamido hydroxypropyl myristyl ether 0.4%, 1.0% fucoxanthin, rapeseed sterols 0.5%, safflower oil body 0.7%, 5HA hyaluronic acid 0.7%, sickle pod bark extract 0.5%, cornflower flower extract 0.1%, tocopherol (vitamin E) 0.3%, disodium EDTA 0.08%, fragrance 0.08%, preservative 1.8%, deionized water to 100%.
[0165] The emulsifier is wild almond oil polyglycerol-6 esters, polyglycerol-10 oleate, and polyglycerol-10 laurate, which are mixed in a mass ratio of 1:1:2.
[0166] The emollient is arachidyl alcohol, neopentyl glycol diheptanoate, crabapple seed oil, cholesterol hydroxystearate and dicaprylyl carbonate, which are used in a composite manner in a mass ratio of 0.5:1:0.1:0.1:1.
[0167] Vetiver root extract contains 49.25% 1,3-propylene glycol and 50.0% water by weight. The preparation process of Vetiver root extract is as follows:
[0168] 1) Select the root of Vetiver, clean and dry it, grind it into 20 mesh size for later use;
[0169] 2) adding vetiver root and water in a mass ratio of 1:60 into a container, soaking for 30 minutes, and homogenizing with a high-speed homogenizer at a speed of 15000 r / min for 180 seconds to obtain a mixture I;
[0170] 3) Weigh 1,3-propylene glycol in a mass ratio of 1:50 to vetiver root and add it to mixture I, and stir at a speed of 30 r / min for 45 minutes to obtain mixture II;
[0171] 4) homogenizing the mixture II once through a high-pressure homogenizer at a working pressure of 350 bar, and then circulating the homogenized mixture through a high-pressure homogenizer at a working pressure of 1000 bar for two times;
[0172] 5) The homogenized mixture was centrifuged at 20,000 r / min for 20 minutes using a low-temperature micro-table centrifuge, and the upper clear liquid was taken to obtain the vetiver root extract.
[0173] The tricholoma pubescens mixture is obtained by adopting a low-temperature homogenization preparation process, and comprises the following components in weight percentage: 1.0% of tricholoma pubescens extract, 8.0% of 1,2-pentanediol, and water to 100%.
[0174] Yufuan includes the following components in weight percentage: 54.0% glycerin, 12.5% butylene glycol, 9.5% eyebright extract, 1.5% lemon balm leaf extract, 0.2% formosan clover bud / flower extract, 0.85% lecithin, 0.5% potassium sorbate, and 20.95% water.
[0175] 5HA hyaluronic acid includes the following components in weight percentage: 1.5% sodium hyaluronate, 1.0% dimethylsilanol hyaluronate, 0.1% sodium dimethylsilanol hyaluronate, 1.0% sodium hyaluronate cross-polymer, 1.0% hydrolyzed sodium hyaluronate, 0.9% phenoxyethanol, 0.05% ethylhexylglycerin, and water to 100%.
[0176] The extract of the bark of the falcate sappan wood contains 90.0% maltodextrin by weight; and the extract of the cornflower flower contains 80% maltodextrin by weight.
[0177] The preservatives are 1,2-hexanediol, p-hydroxyacetophenone, glyceryl undecylenate, glyceryl caprate, and vanilla leaf oil, which are mixed and used in a mass ratio of 1:1:0.1:0.1:1.
[0178] The method for preparing the repair nanoemulsion in this embodiment comprises the following steps:
[0179] 1) Emulsifiers, squalane, emollients, rape sterols, safflower oleosomes, and tocopherol are classified as raw materials in group A; deionized water, disodium EDTA, glycerin, butylene glycol, and sodium stearoyl glutamate are classified as raw materials in group B; tetrahydromethylpyrimidine carboxylic acid and trihydroxypalmitamidohydroxypropyl myristyl ether are classified as raw materials in group C; vetiver root extract, pine algae extract, Yufuan, and 5HA hyaluronic acid are classified as raw materials in group D; sicklewood bark extract and cornflower flower extract are classified as raw materials in group E; preservatives and flavors are classified as raw materials in group E;
[0180] 2) Add the raw materials of group A into the oil tank, stir and heat to 75°C at a speed of 20 r / min for use, and obtain the dissolved raw materials of group A for use;
[0181] 3) Add the raw materials of group B into the water phase, stir at a speed of 30 r / min and homogenize at a speed of 3000 r / min for 60 seconds, heat to 83° C. for standby use, and obtain the heated raw materials of group B;
[0182] 4) Pump the heated raw materials of group B into the emulsifying pot, stir at a speed of 30r / min and keep the temperature constant at 83°C, then pump the dissolved raw materials of group A into the emulsifying pot, and homogenize at a speed of 5000r / min for 8 minutes;
[0183] 5) The material in the emulsifier begins to cool down. During this process, it is stirred at a speed of 30r / min and vacuumed to -0.03Mpa;
[0184] 6) When the temperature of the material in the emulsification pot drops to 42°C, add the components in group C into the emulsification pot one by one, stir at 30r / min for 8 minutes, and evacuate to -0.03Mpa;
[0185] 7) Add the components in group D into the emulsifying pot one by one according to the order of division, stir at 30r / min for 8 minutes, and evacuate to -0.03Mpa;
[0186] 8) Add each component in group E into the emulsifying pot one by one, stir at 30 r / min for 12 minutes, and evacuate to -0.03 Mpa;
[0187] 9) Add each component in group F into the emulsifying pot one by one, stir at 30 r / min and homogenize at 3000 r / min for 30 seconds, stir for 12 minutes, and evacuate to -0.03 Mpa;
[0188] 10) After the physical and chemical indicators are tested to be qualified, the material is filtered out to obtain the initially prepared emulsion for use;
[0189] 11) The working pressure of the high-pressure microfluidizer was adjusted to 20,000 psi, and the preliminarily prepared emulsion was added to the high-pressure microfluidizer for 3 cycles of homogenization to obtain a repair nanoemulsion.
[0190] In order to better demonstrate the present invention, the following is a comparative experiment conducted during the development of the technical solution provided by the present application:
[0191] Comparative Example 1
[0192] Compared with Example 1, tetrahydromethylpyrimidine carboxylic acid was replaced by the extract of the bark of Psoralea corylifolia, and the contents of other components and the process remained unchanged.
[0193] Comparative Example 2
[0194] Compared with Example 1, the vetiver root extract was replaced by Yufuan, and the contents of other components and the process remained unchanged.
[0195] Comparative Example 3
[0196] Compared with Example 1, the rape sterols were replaced by trihydroxypalmitamido hydroxypropyl myristyl ether and cornflower flower extract at a mass ratio of 1:1, and the contents of other components and the process remained unchanged.
[0197] Comparative Example 4
[0198] Compared with Example 1, 5HA hyaluronic acid is used as ectoine, and the contents of other components and the process remain unchanged.
[0199] Comparative Example 5
[0200] Compared with Example 1, the mixture of pine algae was replaced by cornflower flower extract, and the contents of other components and the process remained unchanged.
[0201] In order to demonstrate the advantages of the present invention, the repairing nanoemulsions obtained in Examples 1-5 and Comparative Examples 1-5 are experimentally compared below.
[0202] 1. In vitro test - inhibition of hyaluronidase activity test
[0203] 1.1 Test Principle
[0204] Since sensitive skin has the characteristics of impaired barrier function or abnormal nerve conduction function, it has weaker defense against exogenous irritants and allergens than normal skin. Therefore, sensitive skin is prone to a series of skin inflammatory reactions caused by irritation or allergies. The inflammatory reaction will further damage the skin barrier structure and nerve endings, leading to a vicious cycle. Hyaluronidase (HAase) is a specific cleavage enzyme of hyaluronic acid, a participant in allergic reactions, and has a strong correlation with the release of histamine by mast cells. Therefore, the anti-inflammatory activity of a substance can be evaluated using the hyaluronidase inhibition rate as an indicator. The greater the hyaluronic acid inhibition rate, the stronger the anti-inflammatory activity. Inhibiting hyaluronidase can reduce the skin inflammatory reaction that damages the skin barrier structure and nerve endings, and has a soothing effect.
[0205] 1.2. Reagent Setup
[0206] Acetate buffer (PH = 5.6), 0.5mg / ml sodium hyaluronate solution, 1250U / ml hyaluronidase solution, 0.5mg / ml calcium chloride solution, 0.5mg / ml sodium hydroxide solution, 1.0mg / ml sodium borate solution, 0.1mol / L p-dimethylaminobenzaldehyde
[0207] Test solution: Repair nanoemulsion of Examples 1-5 and Comparative Examples 1-5
[0208] 1.3 Instruments
[0209] Microplate reader (Multiskan FC), analytical balance (Mettler Toledo), pipette (Eppendorf), vortex mixer (Dragon), pH meter (Ramagnetic).
[0210] 1.4 Test Method
[0211] 1.4.1 Reaction process
[0212] Group A: Take 0.5ml calcium chloride solution and 0.1ml hyaluronidase solution and place them in a 37℃ water bath for 20min, add 0.5ml sodium hyaluronate solution and 1.0ml acetate buffer and keep warm for 30min; add 0.5ml sodium hydroxide solution and mix evenly, cool to room temperature with ice water, then add 0.1ml sodium silicate solution and mix evenly, add p-dimethylaminobenzaldehyde, let stand for 20min to develop color, take 1ml and measure the absorbance at 582nm.
[0213] Group B: Take 0.5ml calcium chloride and 1.1ml acetate buffer solution and place them in a 37℃ water bath for 20min, add 0.5ml sodium hyaluronate solution and keep warm for 30min; add 0.5ml sodium hydroxide solution and mix evenly, cool to room temperature with ice water, then add 0.1ml sodium silicate solution and mix evenly, add p-dimethylaminobenzaldehyde, let stand for 20min to develop color, take 1ml and measure the absorbance at 582nm.
[0214] Group C: Take 0.5ml calcium chloride solution and 0.1ml hyaluronidase solution and place them in a 37℃ water bath for 20min, add 0.5ml sodium hyaluronate solution and 1.0ml test solution and keep warm for 30min; add 0.5ml sodium hydroxide solution and mix evenly, cool to room temperature with ice water, then add 0.1ml sodium silicate solution and mix evenly, add p-dimethylaminobenzaldehyde, let stand for 20min to develop color, take 1ml and measure the absorbance at 582nm.
[0215] Group D: Take 0.5ml calcium chloride solution and 0.1ml acetate buffer and place them in a 37℃ water bath for 20min, add 0.5ml sodium hyaluronate solution and 1.0ml test solution and keep warm for 30min; add 0.5ml sodium hydroxide solution and mix evenly, cool to room temperature with ice water, then add 0.1ml sodium silicate solution and mix evenly, add p-dimethylaminobenzaldehyde, let stand for 20min to develop color, take 1ml and measure the absorbance at 582nm.
[0216] 1.4.2 Calculation formula:
[0217] The calculation formula of the activity inhibition rate T of hyaluronidase is:
[0218] T=[(AB)-(CD)] / (AB)×100%
[0219] Where:
[0220] A—is the absorbance value of the negative control group
[0221] B—is the blank absorbance value of the negative control group;
[0222] C—is the absorbance value of the sample group;
[0223] D—is the blank absorbance value of the sample group.
[0224] 1.4.3 Test results
[0225] The test data results are shown in Table 1.
[0226] Table 1 Data results
[0227] Sample name Inhibition rate (%) Example 1 63.50 Example 2 66.85 Example 3 64.45 Example 4 75.25 Example 5 74.55 Comparative Example 1 29.35 Comparative Example 2 33.35 Comparative Example 3 35.75 Comparative Example 4 28.65 Comparative Example 5 32.95
[0228] 1.5 Conclusion:
[0229] From the test results, it can be seen that Examples 1-5 have significant hyaluronidase inhibition ability, and the hyaluronidase inhibition rate reaches more than 63.50%. After the various ingredients in Comparative Examples 1-5 were substituted, the hyaluronidase inhibition rate was significantly reduced, and the hyaluronidase inhibition rate was below 35.75%. This shows that Examples 1-5 have good anti-inflammatory, anti-allergic and soothing effects, can improve the irritation, roughness, peeling and other phenomena caused by environmental and seasonal changes in the skin, and repair the skin barrier.
[0230] 2. Human body test - skin moisture content test
[0231] 2.1. Test purpose: To evaluate the skin moisture content of the repairing nanoemulsions of Examples 1 to 5 and Comparative Examples 1 to 5 before use and 1h, 2h, and 4h after use through a 4h human moisturizing test. The larger the skin moisture content value, the higher the skin moisture content.
[0232] 2.2 Test requirements
[0233] Number of volunteers: 50 (38 females; 12 males, aged 38-60 years old) in good health, without skin problems, no pregnant or lactating women, no dropouts, and no use of any drugs or cosmetics during the test.
[0234] Test area: Outer calf
[0235] Test time: 4h
[0236] 2.3 Test Instruments
[0237] Skin moisture content tester Corneometer (CM 825, Courage and Khazaka, Germany)
[0238] 2.4 Testing process
[0239] 1) Control the indoor temperature at 20-22°C and relative humidity at 50±5%RH.
[0240] 2) Divide the 50 people into 10 groups, with 5 people in each group.
[0241] 3) Before use, test the test skin area, record it as 0h data and mark it.
[0242] 4) Weigh the test sample at a dosage of (2.0±0.1) mg / cm2 and apply it once to the subject's marked test area before use, massage for 30 seconds until absorbed, and then conduct a follow-up visit.
[0243] 5) Retest 1 hour, 2 hours, and 4 hours after absorption. Use the area not coated with the product as a blank for testing.
[0244] 2.5. Test result calculation formula
[0245] Initial value: refers to the basic value when no product is used.
[0246] Where x = individual parameter measurement, n = number of valid data;
[0247] Difference from initial value = x T使用后 -x T使用前
[0248]
[0249] 2.6 Test Results
[0250] 2.6.1. The test results of skin moisture content before using the product and 1h, 2h and 4h after using the product are shown in Table 2.
[0251] Table 2 Average values and statistical results of skin moisture content before use of the product, 1h, 2h, and 4h after use of the product (n=50)
[0252]
[0253] 2.6.2 Conclusion
[0254] From the results in Table 2, it can be seen that compared with before use, after 4 hours of use, the increase rate of skin moisture content in Examples 1-5 is more than 20.56%, while compared with before use, after 4 hours of use, the increase rate of skin moisture content in Comparative Examples 1-5 is less than 13.20%, indicating that the components of the repairing nanoemulsions in Examples 1-5 of the present invention synergistically enhance each other, have significant skin moisturizing and soothing ability, can effectively improve skin dryness and desquamation problems, repair damaged skin barriers, make the skin moisturized and smooth, and achieve the effect of lasting moisturizing, moisturizing and locking water.
[0255] 3. Human test-skin barrier function test
[0256] 3.1. Principle: TEWL is an important parameter for evaluating the function of the skin's moisture protection layer and can be used to evaluate the strength of the skin's barrier function. The skin barrier repair function of Examples 1-5 and Comparative Examples 1-5 is judged by TEWL loss. The smaller the measured value, the less skin moisture loss. In the repair test, the smaller the TEWL, the better the skin barrier function. The unit of TEWL is: g / hm 2 .
[0257] 3.2 Test requirements
[0258] 3.2.1. Volunteers 50 volunteers completed the skin moisture content test at the same time.
[0259] 3.2.2 Test Instruments
[0260] Skin water loss test probe (Tewameter TM300, Courage & Khazaka, Germany)
[0261] 3.3. Test result calculation formula
[0262] Where x = individual parameter measurement, n = number of valid data;
[0263]
[0264] 3.4. Table 3 shows the mean values and statistical results of transepidermal water loss TEWL before use of the samples and 1, 2, and 4 hours after use (n=50).
[0265] Table 3 Average values and statistical results of transepidermal water loss TEWL before use, 1, 2, and 4 hours after use, n = 50
[0266]
[0267] 3.5 Conclusion
[0268] From the results in Table 3, it can be seen that compared with before use, Examples 1-5 can significantly reduce TEWL loss. After 4 hours of use, the degree of reduction of transepidermal water loss of the skin is more than 13.51%; while after 4 hours of use of Comparative Examples 1-5, the degree of reduction of transepidermal water loss of the skin is less than 6.76%, indicating that Examples 1-5 have lower TEWL loss, that is, better repair of skin barrier function, which can help promote the repair of the skin stratum corneum and improve skin problems such as dryness, roughness, sensitivity, and desquamation.
[0269] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. For those skilled in the art, the present invention may have various modifications and variations. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention shall be included in the protection scope of the present invention.
Claims
1. A repair nanoemulsion, characterized in that: The invention comprises the following components in weight percentage: 1.0-5.0% of emulsifier, 1.0-5.0% of squalane, 2.0-10.0% of emollient, 3.0-10.0% of glycerin, 3.0-10.0% of butylene glycol, 0.5-3.0% of tetrahydromethylpyrimidine carboxylic acid, 0.5-3.0% of vetiver root extract, 0.5-3.0% of soft hair pine algae mixture, 0.5-3.0% of sodium stearoyl glutamate, 0.1-1.0% of trihydroxypalmitamido hydroxypropyl myristyl ether .0%, Yufuan 0.1-1.0%, rape sterols 0.1-1.0%, safflower oleosomes 0.1-1.0%, 5HA hyaluronic acid 0.1-1.0%, sickle pod tree bark extract 0.05-0.5%, cornflower flower extract 0.05-0.5%, tocopherol 0.1-1.0%, disodium EDTA 0.03-0.2%, flavor 0.03-0.1%, preservatives 0.5-2.0%, deionized water to 100%.
2. The repair nanoemulsion according to claim 1, characterized in that The emulsifier is one or more of olive oil polyglycerol-6 esters, watermelon seed oil polyglycerol-6 esters, wild almond oil polyglycerol-6 esters, polyglyceryl-3 methyl glucose distearate, polyglyceryl-10 oleate, polyglyceryl-10 laurate and polyglyceryl-10 myristate.
3. The repair nanoemulsion according to claim 1, characterized in that: The emollient is one or more of arachidyl alcohol, hydrogenated rapeseed alcohol, neopentyl glycol diheptanoate, vegetable palm oil, Alnus macrophylla seed oil, hop cone oil, Camellia oleifera seed oil, Malus domestica seed oil, cholesterol hydroxystearate, phytosteryl macadamia oleate, sunflower seed oil, isononyl isononanoate, triethylhexanoin, dicaprylyl carbonate and C10-40 isoalkanoic acid cholesterol ester.
4. The repair nanoemulsion according to claim 1, characterized in that: The vetiver root extract contains 25.0-50.0% 1,3-propylene glycol and 25.0-50.0% water by weight; The preparation process of the vetiver root extract is as follows: 1) Select the root of Vetiver, clean and dry it, grind it into 20-40 mesh size for later use; 2) adding vetiver root and water in a mass ratio of 1:50-60 into a container, soaking for 30-60 minutes, and homogenizing with a high-speed homogenizer at a speed of 12000-15000 r / min for 180-240 seconds to obtain a mixture I; 3) Weigh 1,3-propylene glycol in a mass ratio of 1:50-60 to vetiver root and add it to mixture I, and stir at a speed of 25-30 r / min for 45-60 minutes to obtain mixture II; 4) homogenizing the mixture II once through a high-pressure homogenizer with a working pressure of 350 to 500 bar, and then circulating the homogenized mixture through a high-pressure homogenizer with a working pressure of 800 to 1000 bar for two times; 5) The homogenized mixture was centrifuged at 20,000 r / min for 20 minutes using a low-temperature micro-table centrifuge, and the upper clear liquid was taken to obtain the vetiver root extract.
5. The repair nanoemulsion according to claim 1, characterized in that: The tricholoma pubescens mixture is obtained by adopting a low-temperature homogenization preparation process, and comprises the following components in weight percentage: 1.0-3.0% of tricholoma pubescens extract, 8.0-12.0% of 1,2-pentanediol, and up to 100% of water.
6. The repair nanoemulsion according to claim 1, characterized in that: The Yufuan comprises the following components in percentage by weight: 49.0-55.0% glycerol, 10-25% butylene glycol, 5.0-10.0% eyebright extract, 1.0-5.0% lemon balm leaf extract, 0.1-1.0% primula formosanus bud / flower extract, 0.8-1.0% lecithin, 0.3-0.5% potassium sorbate, and 16.9-23.85% water.
7. The repair nanoemulsion according to claim 1, characterized in that: The 5HA hyaluronic acid includes the following components in weight percentage: 0.5-2.0% sodium hyaluronate, 0.1-1.0% dimethylsilanol hyaluronate, 0.1-1.0% sodium dimethylsilanol hyaluronate, 0.1-1.0% sodium hyaluronate cross-linked polymer, 0.1-1.0% hydrolyzed sodium hyaluronate, 0.5-1.0% phenoxyethanol, 0.05-0.1% ethylhexylglycerin, and water to 100%.
8. The repair nanoemulsion according to claim 1, characterized in that: The falcaria bark extract contains 90.0% maltodextrin by weight; and the cornflower flower extract contains 80% maltodextrin by weight.
9. The repair nanoemulsion according to claim 1, characterized in that: The preservative is one or more of phenoxyethanol, 1,2-hexanediol, p-hydroxyacetophenone, glyceryl undecylenate, phenoxyethanol, caprylhydroxamic acid, glyceryl caprylate, ethylhexylglycerin, 1,2-pentanediol, caprylyl glycol, glyceryl caprate, camphor bark oil, Melaleuca alternifolia leaf oil, Zanthoxylum bungeanum fruit extract, hop cone oil, and vanilla flat fruit oil.
10. The method for preparing the repair nanoemulsion according to claim 1, characterized in that: The steps include: 1) Emulsifiers, squalane, emollients, rape sterols, safflower oleosomes, and tocopherol are classified as raw materials in group A; deionized water, disodium EDTA, glycerin, butylene glycol, and sodium stearoyl glutamate are classified as raw materials in group B; tetrahydromethylpyrimidine carboxylic acid and trihydroxypalmitamidohydroxypropyl myristyl ether are classified as raw materials in group C; vetiver root extract, pine algae extract, Yufuan, and 5HA hyaluronic acid are classified as raw materials in group D; sicklewood bark extract and cornflower flower extract are classified as raw materials in group E; preservatives and flavors are classified as raw materials in group E; 2) Add the raw materials of group A into the oil tank, stir and heat to 75-80°C at a speed of 20-25 r / min for use, and obtain the dissolved raw materials of group A for use; 3) Add the raw materials of group B into the aqueous phase, stir at a speed of 30-35 r / min and homogenize at a speed of 3000-3500 r / min for 60-90 seconds, heat to 83-85° C. for standby use, and obtain the heated raw materials of group B; 4) Pump the heated raw materials of group B into the emulsifying pot, stir at a speed of 30-35 r / min and keep the temperature constant at 83-85°C, then pump the dissolved raw materials of group A into the emulsifying pot, and homogenize at a speed of 5000-6000 r / min for 8-15 minutes; 5) The material in the emulsifier begins to cool down. During this process, it is stirred at a speed of 30 to 35 r / min and vacuumed to -0.03 to -0.05 MPa; 6) When the temperature of the material in the emulsification pot drops to 42-48°C, add the components in Group C into the emulsification pot one by one, stir at 30-35r / min for 8-15 minutes, and evacuate to -0.03-0.05Mpa; 7) Add the components in group D into the emulsifying pot one by one according to the order of division, stir at a speed of 30-35 r / min for 8-10 minutes, and evacuate to -0.03-0.05 Mpa; 8) Add each component in the raw material of group E into the emulsifying pot one by one, stir at a speed of 30-35 r / min for 12-15 minutes, and evacuate to -0.03-0.05 MPa; 9) Add each component in group F into the emulsifying pot one by one, stir at 30-35 r / min and homogenize at 3000-3500 r / min for 30-90 seconds, stir for 12-15 minutes, and evacuate to -0.03-0.05 Mpa; 10) After the physical and chemical indicators are tested to be qualified, the material is filtered out to obtain the initially prepared emulsion for use; 11) The working pressure of the high-pressure microfluidizer is adjusted to 20,000-30,000 psi, and the preliminarily prepared emulsion is added to the high-pressure microfluidizer for cyclic homogenization for 3 times to obtain a repair nanoemulsion.