A non-irritating warm-sensing mud mask and preparation method thereof

Abstract

The present invention discloses a non-irritating temperature-sensitive mud mask and a preparation method thereof, which belongs to the field of cosmetics. The non-irritating temperature-sensitive mud mask described in the present invention comprises components including: Yuncheng Salt Pond black mud powder, oil, alkanediol, moisturizer, filler adsorbent, emulsifier, pH adjuster, antibacterial and antibacterial synergist, thickener, chelating agent, thermal agent, auxiliary ingredients and glycerol; wherein the thermal agent is a combination of vanillyl butyl ether and clove bud oil, and the mass ratio of the two is 1 to 10: 1 to 10. The temperature-sensitive facial mask of the present invention is non-irritating and can provide a gentle and lasting heating effect to the skin. It has good temperature sensation, moisturizing, brightening skin tone and anti-inflammatory effects. It is suitable for most people and has broad market prospects.

Description

Technical Field

[0001] The invention relates to a non-irritating warm-sensing mud mask and a preparation method thereof, and belongs to the field of cosmetics. Background Art

[0002] The mechanism of action of "warm skin care" is similar to traditional hot compress therapy and sauna baths. It increases the temperature of the skin to cause capillary dilation and speed up blood flow. This process helps soften the stratum corneum and causes the pores to open, thereby increasing the skin's absorption efficiency of nutrients in skin care products and ultimately achieving deep nourishment of the skin. The popularity of "warm skin care" stems from consumers' pursuit of refined, precise and exquisite skin care, which further promotes consumers' sensory enjoyment during product use. Different from the "cool skin care" concept in summer, in winter, consumers' skin is drier and more sensitive, and there is a greater demand for moisturizing skin care products that are gentle on the skin and non-irritating.

[0003] In the prior art, one type of heating mask uses the principle of a "warm baby" patch to release heat through a chemical reaction between reduced iron powder and oxygen and water vapor in the atmosphere. For example, a self-heating mask mentioned in the literature (Long Lihui, Xue Jianqiang, Yao Yang, Yang Kuan, Qin Bei. Research on the optimal ratio of each component of a self-heating mask [J]. Chinese Journal of Aesthetic Medicine, 2020, 29(2): 68-70) is relatively complex in structure and the production process is relatively cumbersome.

[0004] In the prior art, another type of heat-generating cosmetics generates heat by adding inorganic heat-generating agents, such as chlorides, sulfates, zeolites, etc., and mixing with water. For example, CN1487823A discloses an anhydrous cosmetic composition, which includes a heat-generating agent that generates heat by mixing with water; CN116350528A discloses a zeolite temperature-sensitive cleansing mud mask and its preparation method and use method; however, the use method of such heat-generating cosmetics is limited. When using, the anhydrous composition must be mixed with water before applying it on the hair and / or skin, or the facial skin must be moistened with a spray before using the mud mask product.

[0005] In the prior art, there is another type of heating mask that achieves the heat sensation by adding a heat-sensing agent. Among them, vanillyl butyl ether is a fat-soluble heat-sensing agent that can quickly produce a strong hot and spicy sensation after local application on the skin, stimulate subcutaneous fat metabolism, and promote capillary blood circulation. Therefore, it is often used in weight loss and fat-reducing products. For example: CN109419637A discloses a heating facial mask, in which the heating agent combination includes a thermal agent and an auxiliary heating agent, the thermal agent is vanillyl butyl ether, and the auxiliary heating agent is one or a combination of wild mountain pepper fruit oil and star anise seed oil; CN109091405A discloses a warm skin care product and a preparation method thereof, which utilizes a combination of glycerol and vanillyl butyl ether to generate heat; CN111773122A discloses a heating facial mask with moisturizing effect and a preparation method thereof, in which a combination of vanillyl butyl ether and ginger root oil is used as a heating agent; although the above-mentioned documents reduce the irritation of vanillyl butyl ether by adding some oil phases (wild mountain pepper fruit oil, star anise seed oil, ginger root oil), or add glycerol to assist vanillyl butyl ether in generating heat, the product still has the problems of slow heating speed and strong irritation. Summary of the invention

[0006] In view of the deficiencies in the prior art, the warm-sensing mask of the present invention adopts an anhydrous system with glycerol as a solvent to prevent water evaporation from taking away skin heat. When it is used on the face, a high content of glycerol forms hydrated molecules with the moisture of the skin surface, and immediately and quickly releases heat to increase the temperature, which has a heating effect; while using a combination of vanillyl butyl ether and clove bud oil as a thermal agent, it can not only ensure that the heat is mild and non-irritating, but also ensure a continuous sense of heating. In addition, with the black mud of Yuncheng Salt Pond, the black mud is rich in minerals, trace elements, organic matter and a large amount of colloidal substances that are beneficial to human skin. These effective ingredients can increase the moisture of skin tissue, enhance the activity of superoxide dismutase (SOD) and glutathione peroxidase (GSH-Px) in the skin, remove excess free radicals on the skin, and delay skin aging. The warm-sensing mask of the present invention is non-irritating, and can provide a gentle and lasting heating effect to the skin, with good temperature sensation, moisturizing, brightening skin tone and anti-inflammatory effects, suitable for most people to use, with a wide market prospect.

[0007] The first object of the present invention is to provide a non-irritating temperature-sensitive mud mask, the components of which include: Yuncheng Salt Pond black mud powder, grease, alkanediol, moisturizer, filler adsorbent, emulsifier, pH regulator, antibacterial and antibacterial synergist, thickener, chelating agent, heat-sensitive agent, auxiliary material components and glycerol;

[0008] Among them, the thermal agent is a combination of vanillyl butyl ether and clove bud oil, and the mass ratio of the two is 1-10:1-10.

[0009] As an embodiment of the present invention, the mass ratio of vanillyl butyl ether to clove bud oil in the thermal sensitizer is further preferably 1:1.

[0010] As an embodiment of the present invention, the mass percentages of Yuncheng Salt Pond black mud powder, oil, alkanediol, humectant, filler adsorbent, emulsifier, pH adjuster, antibacterial and antibacterial synergist, thickener, chelating agent, thermal agent and auxiliary material components are 10-40%: 5-20%: 5-15%: 5-15%: 1-15%: 2-10%: 0.5-3.0%: 0.2-2%: 0.1-2%: 0.05-0.4%: 0.04-0.6%: 0.01-1%, and the rest is glycerol, and the total is 100%.

[0011] As an embodiment of the present invention, the Yuncheng Salt Pond black mud powder is rich in minerals and trace elements such as potassium, sodium, calcium, magnesium, zinc, selenium, iron, chlorine, iodine, bromine, sulfates and carbonates required by the human body. It also contains the remains of plants and animals such as algae, aquatic plants and crustaceans, and organic substances such as humic acid, protein, amino acids and polysaccharides that are beneficial to human skin after years of siltation. These active ingredients can increase the moisture of skin tissue, enhance the activity of superoxide dismutase and glutathione peroxidase in the skin, remove excess free radicals on the skin, and delay skin aging.

[0012] As an embodiment of the present invention, the oil is one or more of white meadowfoam seed oil, olive oil, coconut oil, camellia seed oil, jojoba seed oil, shea butter, grape seed oil, hydrogenated lecithin, squalane, caprylic / capric / triglyceride, cetearyl alcohol, and monoglyceryl stearate.

[0013] As an embodiment of the present invention, the emulsifier is one or more of fatty acid esters, sucrose fatty acid esters, fatty acid sorbitan, polyoxyethylene ethers, polyoxypropylene ethers, alkyl glucoside, glucose esters, stearyl esters, and alkyl ethers.

[0014] As an embodiment of the present invention, the alkanediol is one or more of butanediol, pentanediol, hexanediol, 1,3-propylene glycol and octyl glycol.

[0015] As an embodiment of the present invention, the filling adsorbent is selected from one or more of kaolin, bentonite, hectorite, diatomaceous earth, magnesium aluminum silicate, hydroxyethyl cellulose, sodium starch octenyl succinate, silica, charcoal, bamboo charcoal, activated carbon, and oat kernel powder.

[0016] As an embodiment of the present invention, the moisturizing agent is one or more of sodium hyaluronate, hyaluronic acid, hydrolyzed hyaluronic acid, hydrolyzed sodium hyaluronate, sodium hyaluronate cross-polymer, acetylated sodium hyaluronate, tetrahydromethylpyrimidine carboxylic acid, glyceryl polyether-26, hydrolyzed corn starch, carbohydrate isomers, polyquaternium-51, sodium pyrrolidone carboxylate, zinc pyrrolidone carboxylate, sorbitol, trehalose, urea, β-glucan, yeast β-glucan, Dendrobium nobile stem extract, ceramide, dihydroxypropyl arginine hydrochloride, sodium alginate, acetyl glucosamine, niacinamide, betaine, allantoin, panthenol, Tremella polysaccharide, maltodextrin, bifid yeast fermentation product lysate, yeast polypeptides, yeast fermentation product, yeast lysate, yeast extract, Pichia pastoris fermentation lysate filtrate, Bacillus fermentation product, Lactobacillus fermentation product, and Lactobacillus fermentation lysate.

[0017] As an embodiment of the present invention, the pH adjuster is citric acid.

[0018] As an embodiment of the present invention, the chelating agent is EDTA-2Na.

[0019] As an embodiment of the present invention, the antibacterial and antibacterial synergist is one or more of ethylhexylglycerol, p-hydroxyacetophenone, caprylhydroxamic acid, dianthin, fullerene, astaxanthin, zinc lactate, zinc gluconate, and zinc sulfate.

[0020] As an embodiment of the present invention, the thickener is one or more of ammonium acryloyldimethyltaurate / behenyl alcohol polyether-25 methacrylate cross-linked polymer, hydroxypropyl starch phosphate, sodium polyacryloyldimethyltaurate, ammonium acryloyldimethyltaurate / VP copolymer, xanthan gum, carbomer, sodium chloride, and Yuncheng Salt Lake Salt.

[0021] As an embodiment of the present invention, the auxiliary material ingredients are one or more of Centella asiatica extract, Centella asiatica leaf extract, Portulaca oleracea extract, Glycyrrhiza glabra extract, Polygonum cuspidatum root extract, Ginseng extract, Scutellaria baicalensis root extract, Berberis vulgaris root extract, Andrographis paniculata extract, Gentiana root extract, Glycyrrhiza uralensis root extract, Gardenia jasminoides extract, Peony root bark extract, Ennan tomato bark extract, Chamomile flower extract, Camellia japonica extract, Artemisia argyi extract, Tea leaf extract, Rosemary leaf extract, Aloe leaf extract, Mulberry leaf extract, Thyme leaf extract, Black mulberry fruit extract, Lycium barbarum fruit extract, Strawberry fruit extract, Brazil nut seed extract, Akebia quinata extract, collagen, asiaticoside, madecassoside, N-palmitoyl hydroxyproline cetyl ester, rape sterols, and bisabolol.

[0022] The second object of the present invention is to provide a method for preparing a non-irritating warm-sensing mud mask, comprising the following steps:

[0023] (1) mixing glycerin, alkanediol, humectant, pH adjuster, antibacterial and antibacterial synergist, thickener and chelating agent to obtain phase A;

[0024] (2) mixing the filling adsorbent and the Yuncheng salt pond black mud powder uniformly to form phase B; then, adding phase B to phase A in batches under high-speed stirring until phase B is uniformly dispersed in the system to obtain a mixed phase;

[0025] (3) mixing the oil and the emulsifier uniformly to obtain phase C;

[0026] (4) mixing the thermal sensitizing agent and the auxiliary material components uniformly to obtain phase D;

[0027] (5) Heat the mixed phase and phase C to 80-90°C respectively, then add phase C into the mixed phase for emulsification, and homogenize at high speed for 3-5 minutes; after the emulsification is completed, cool to 40-50°C, add phase D, mix evenly, and cool to 20-30°C to obtain a temperature-sensitive mud film.

[0028] As an embodiment of the present invention, the uniform mixing in step (1) is carried out by homogenizing and mixing at 20 to 40° C. and 3000 to 5000 r / min.

[0029] As an embodiment of the present invention, in step (2), phase B is added to phase A in batches at 8000-10000 r / min. After the addition of phase B is completed, homogenization is continued at 8000-10000 r / min for 20-25 minutes until it is completely dispersed. The purpose of adding in batches is to make the system homogenous and uniform. The subsequent mixing is continued to make the system completely homogenous so that there is no graininess when applying on the face.

[0030] As an embodiment of the present invention, the uniform mixing in step (2) means achieving an effect of no obvious particles in the mixed phase.

[0031] As an embodiment of the present invention, the uniform mixing in step (3) is performed at 80-90° C. and 3000-5000 r / min.

[0032] As an embodiment of the present invention, the uniform mixing in step (4) is performed at 40-50° C. and 3000-5000 r / min.

[0033] As an embodiment of the present invention, the emulsification in step (5) is carried out at 80-90° C. and 8000-10000 r / min for 3-5 min.

[0034] As an embodiment of the present invention, the uniform mixing in step (5) is carried out by homogenizing and mixing at 40-50° C. and 2500-3500 r / min for 2-3 min.

[0035] The third object of the present invention is to provide a method for improving the temperature-sensing performance of a mud mask and reducing irritation, which uses the temperature-sensing mud mask of the present invention.

[0036] The fourth object of the present invention is a warm-sensing dressing, which adopts the warm-sensing mud mask of the present invention.

[0037] The beneficial effects of the present invention are as follows:

[0038] (1) The temperature-sensitive mud mask of the present invention adopts a water-free formula. The black mud mask prepared under optimized conditions has moderate viscosity, uniform and fine texture, and fragrant smell. The results of physical and chemical property measurements show that the pH value and stability experiment of the black mud mask product meet national standards.

[0039] (2) After using the temperature-sensitive mud mask of the present invention, compared with the temperature before use, the average temperature during use increased by 0.95°C, and the average temperature before washing the mud mask increased by 0.58°C, with improvement rates of 2.75% and 1.69%, respectively, and both were significantly different (***P<0.001). This shows that the temperature-sensitive mud mask can increase the skin temperature after use, producing a warm feeling, and is suitable for use in winter.

[0040] (3) After using the mud mask product, the moisture content and glossiness of the skin's stratum corneum were significantly increased, and the facial blood perfusion was significantly reduced, and both were significantly different (***P<0.001), indicating that the warm mud mask has the effects of moisturizing, brightening and anti-inflammatory.

[0041] (4) The warm mud mask of the present invention adopts a combination of vanillin butyl ether and clove bud oil to achieve non-irritation and is suitable for use by most people; and it can use the Yuncheng Salt Pond black mud as a base, so that the Yuncheng Salt Pond black mud mask can have a certain warmth without affecting its other properties, such as moisturizing. BRIEF DESCRIPTION OF THE DRAWINGS

[0042] Figure 1 Flow chart of the test for efficacy evaluation.

[0043] Figure 2 Schematic diagram of the sample of the temperature-sensitive mud film prepared in Example 1.

[0044] Figure 3 This is a graph showing the skin temperature change before and after using the warm-sensing mud mask prepared in Example 1.

[0045] Figure 4 This is a graph showing the change in moisture content of the stratum corneum of the skin before and after use of the warm-sensitive mud mask prepared in Example 1.

[0046] Figure 5 This is a graph showing the change in skin gloss before and after using the warm-sensitive mud mask prepared in Example 1.

[0047] Figure 6 This is a graph showing changes in blood perfusion volume before and after use of the temperature-sensitive mud mask prepared in Example 1.

[0048] Figure 7 This is an analysis chart of the questionnaire results before and after the use of the temperature-sensitive mud mask prepared in Example 1.

[0049] Figure 8 This is a picture of the water-containing mud mask formula prepared in Comparative Example 1 after use. DETAILED DESCRIPTION

[0050] The preferred embodiments of the present invention are described below. It should be understood that the embodiments are for better explaining the present invention and are not used to limit the present invention.

[0051] Test method:

[0052] 1. Product sensory and human efficacy evaluation:

[0053] (1) Test instrument:

[0054] Infrared thermometer, BNT410CN, Haozhan Medical Technology (Wujiang) Co., Ltd.;

[0055] Multi-probe skin testing system MPA10, CK company, Germany;

[0056] Laser Doppler flowmeter, PeriFlux 5000, Perimed, Sweden.

[0057] (2) Test environment:

[0058] Temperature 21±1℃; humidity 50±10%;

[0059] (3) Selection of subjects:

[0060] Age range: 18 to 30 years old; no serious systemic diseases, immunodeficiency or autoimmune diseases; the tested area has not received skin treatment, cosmetic treatment or other tests that may affect the results; no active allergic diseases; no highly sensitive constitution; no use of hormone drugs and immunosuppressants in the past month; the tested area has not participated in other clinical trials in the past month.

[0061] (4) Test process:

[0062] like Figure 1: After cleaning the face, the subjects sat quietly in a laboratory that met the regulations for 20 minutes, and the experimenters operated the relevant instruments to collect blank data on the right face of the subjects; then 1.5g of the temperature-sensitive mud mask sample was evenly applied to the right half of the subject's face, and the skin temperature data of the right cheek was collected; after waiting for 15 minutes, the skin temperature and skin blood perfusion data of the right cheek were collected; then the temperature-sensitive mud mask was washed off, and the experimenters operated the relevant instruments to collect the skin stratum corneum moisture content, skin color, skin gloss, and skin blood perfusion data of the right face of the subject.

[0063] (5) Test parameters:

[0064] ①Skin temperature test:

[0065] The skin temperature of the right cheek was measured using an infrared thermometer, and the average value was taken after three measurements.

[0066] The multi-probe skin testing system MPA10 was used to measure the changes in skin-related data before and 5 minutes, 2 hours, 4 hours, and 8 hours after using the black mud mask;

[0067] ②Skin moisture content:

[0068] Use the moisture test probe Corneometer CM825 to measure the moisture content of the stratum corneum in the test area on the right side of the face, and take the average value of the measurements three times;

[0069] ③Skin glossiness:

[0070] Use the glossymeter GL200 to measure the glossiness of the right facial test area, and take the average value of the three measurements;

[0071] ④ Blood perfusion test:

[0072] Laser Doppler blood flowmetry was used to measure the changes in skin blood flow values ​​before using the black mud mask, 15 minutes after use, and 5 minutes and 2 hours after washing;

[0073] Place the part to be measured under the scanning window of the instrument, make the laser window parallel to the measured part, and the laser beam perpendicular to the measured part without touching the skin. Scan the same part on the right side of the face 15 times and take the average value.

[0074] (6) Data statistical analysis:

[0075] IBM SPSS Statistics 26 was used for data statistical analysis. Paired t-test was performed for data with normal distribution (normality test P value>0.05), otherwise paired rank sum test was used. P<0.05 was considered significant, with *P<0.05, **P<0.01, ***P<0.001.

[0076] (7) Questionnaire survey after product use:

[0077] Combined with questionnaires, multiple-choice questions, and essay questions, we can fully understand the subjects' feelings after using the product.

[0078] The questionnaire surveyed 34 subjects' feelings about the use of warm mud mask products, including 9 males and 25 females, of which 8 had dry skin, 6 had oily skin, 3 had normal skin, 12 had combination skin, and 5 had sensitive skin.

[0079] Table 1 Questionnaire

[0080] 1. What is your gender? O male O female 2.Please select your skin type? O Oily skin O Dry skin O Neutral skin O Combination skin O Sensitive skin (lactic acid tingling, can be felt within 1 minute) 3. Do you feel a warm sensation after applying this product? If so, how long does the warm sensation last? O No O Yes 4. Do you feel the following after applying this product? OTingling feelingONumbness feelingOHot feelingONo feeling 5. Do you feel any discomfort after cleaning the mud mask? O No O If yes, please describe: 6. Are there any adverse reactions when using this product? O No O If yes, please describe: 7. Do you agree that this product is mild and non-irritating? O AgreeO Disagree

[0081] 2. Physical and chemical properties testing of products:

[0082] (1) pH value:

[0083] The pH value of the mud mask sample was determined according to the method in the national standard “Facial Mask” (QB / T 2872-2017).

[0084] (2) Appearance:

[0085] At room temperature without direct sunlight, observe whether the color and texture of the mud film sample are uniform and free of impurities.

[0086] (3) Smell:

[0087] Smell the prepared mud film sample to see if it has any unpleasant odor.

[0088] (4) High temperature stability test:

[0089] The mud film samples were placed in a constant temperature oven at 45°C, taken out after 24 hours, cooled to room temperature, and the changes in the properties of the mud film samples were observed.

[0090] (5) Low temperature stability test:

[0091] The mud film samples were placed in a 5°C constant temperature refrigerator, taken out after 24 hours, cooled to room temperature, and the changes in the properties of the mud film samples were observed.

[0092] (6) Centrifugal stability test:

[0093] The mud film sample was placed in a centrifuge and centrifuged at 3000r / min for 5 minutes, and then the mud film sample was taken out and the changes in its properties were observed.

[0094] Yuncheng Salt Lake Black Mud Powder: Provided by the enterprise, the sample is dried and sterilized and then passed through a 800-1000 mesh sieve.

[0095] Vanillyl butyl ether: purchased from TCI (Shanghai) Chemical Industry Development Co., Ltd.

[0096] Sodium hyaluronate: molecular weights of 30,000 to 50,000 Da and 200,000 to 400,000 Da, purchased from Bloomage Biotechnology Co., Ltd.

[0097] Clove bud oil: purchased from Chongqing Zhengyuan Trading Co., Ltd.

[0098] Example 1

[0099] A method for preparing a non-irritating warm-sensing mud mask comprises the following steps:

[0100] (1) Glycerin, 1,3-butylene glycol, hexylene glycol, glyceryl polyether-26, EDTA-2Na, niacinamide, sodium hyaluronate (molecular weight of 30,000 to 50,000 Da), sodium hyaluronate (molecular weight of 200,000 to 400,000 Da), citric acid, sodium polyacryloyldimethyl taurate, ammonium acryloyldimethyl taurate / behenyl alcohol polyether-25 methacrylate crosspolymer, Yuncheng Salt Lake Salt, acetyl glucosamine, tetrahydromethylpyrimidine carboxylic acid and p-hydroxyacetophenone are homogenously mixed at 30° C. and 4000 r / min to obtain phase A;

[0101] (2) mixing hectorite, Yuncheng salt pond black mud powder and oat kernel fine powder uniformly to form phase B; then adding phase B to phase A in three batches according to mass under high-speed stirring (at 10,000 r / min); after the addition is completed, homogenizing is continued at 10,000 r / min for 20 minutes until the phases are completely dispersed to obtain a mixed phase;

[0102] (3) mixing cetearyl alcohol, PEG-4 polyglyceryl-2 stearate and tri(laureth-4) phosphate at 85° C. and 4000 r / min to obtain phase C;

[0103] (4) mixing the thermal agent, Centella asiatica leaf extract, lactobacillus fermentation product, α-bisabolol, and collagen at 45° C. and 4000 r / min to obtain phase D;

[0104] (5) The mixed phase and phase C are heated to 85°C respectively, and then phase C is added to the mixed phase, emulsified at 3000r / min, and high-speed homogenized for 4 minutes; after the emulsification is completed, the temperature is lowered to 40°C, phase D is added, mixed evenly, and cooled to 25°C to obtain a temperature-sensitive mud film;

[0105] Among them, Yuncheng Salt Pond Black Mud Powder, Cetearyl Alcohol, 1.3-Butanediol, Hexylene Glycol, Glyceryl Polyether-26, Niacinamide, Sodium Hyaluronate (Molecular Weight 30,000-50,000 Da), Sodium Hyaluronate (Molecular Weight 200,000-400,000 Da), Acetyl Glucosamine, Tetrahydromethylpyrimidine Carboxylic Acid, Hectorite, Oat Kernel Powder, PEG-4 Polyglyceryl-2 Stearate, Tri (Laureth-4) Phosphate, Citric Acid, Parahydroxyacetophenone, Sodium Polyacryloyldimethyl Taurate, Ammonium Acryloyldimethyl Taurate / Behenyl Alcohol Polyether-25 Methacrylate Crosspolymer, Yuncheng Salt Pond Salt The mass percentages of EDTA-2Na, thermal agent, Centella asiatica leaf extract, lactobacillus fermentation product, α-bisabolol and collagen are 12%: 12%: 8%: 0.5%: 5%: 2%: 0.05%: 0.05%: 1%: 0.1: 2%: 0.2%: 2%: 2%: 1%: 0.5%: 0.2%: 0.1%: 0.9%: 0.2%: 0.2%: 0.1%: 0.1%: 0.1%: 0.02%, and the remainder is glycerol, and the total is 100%; the mass ratio of vanillyl butyl ether to clove bud oil in the thermal agent is 1:1.

[0106] The obtained temperature-sensitive mud film was subjected to performance tests, and the test results are as follows:

[0107] (1) Physical and chemical properties test results:

[0108] ① pH value:

[0109] 6.86, weakly acidic, which is in line with the range of 3.5 to 8.5 specified in the "QB / T 2872-2017" standard.

[0110] ②Appearance and smell:

[0111] like Figure 2 The warm mud mask has good color, fine paste, smooth and particle-free, free of impurities and stains, no bad odor, and has a warm and sweet lilac aroma.

[0112] ③ Centrifugal stability test:

[0113] There was no obvious change in the temperature-sensitive mud film after centrifugation, indicating that the temperature-sensitive mud film had good centrifugal stability.

[0114] ④High temperature and low temperature stability test:

[0115] There was no significant difference between the temperature-sensitive mud film and before the experiment after it returned to room temperature, indicating that the temperature-sensitive mud film has good high and low temperature stability.

[0116] (2) Sensory and human efficacy evaluation test:

[0117] Figure 3 This is a graph showing the skin temperature change before and after using the warm-sensing mud mask prepared in Example 1. Figure 3 It can be seen that compared with the temperature before use, the average temperature during use increased by 0.95°C, and the average temperature before cleaning the mud mask increased by 0.58°C, with improvement rates of 2.75% and 1.69% respectively, and both were significantly different (***P<0.001). This shows that the warm mud mask can increase the skin temperature and produce a warm feeling after use.

[0118] Figure 4 This is a graph showing the change in moisture content of the stratum corneum of the skin before and after use of the warm-sensing mud mask prepared in Example 1. Figure 4 It can be seen that compared with the blank value (before use), the moisture content of the skin in the test area was significantly improved compared with the initial value after using the warm mud mask for 5 minutes, 2 hours, 4 hours and 8 hours, and the improvement rates were 35.86%, 22.37%, 15.23% and 16.50% respectively, and all of them were significantly different (***P<0.001). This shows that the warm mud mask can quickly replenish moisture for the skin in a short period of time, and the effect can last for a period of time.

[0119] Figure 5 This is a graph showing the change in skin glossiness before and after using the warm mud mask prepared in Example 1. Figure 5 It can be seen that after using the warm mud mask, the skin's glossiness has been significantly improved. Compared with the blank value (before use), the improvement rates after using the warm mud mask for 5 minutes, 2 hours, 4 hours and 8 hours were 6.61%, 16.09%, 14.89% and 16.85%, respectively, and all of them were significantly different (***P < 0.001). This shows that as the use time increases, the warm mud mask can significantly improve the skin's glossiness and has a certain degree of sustainability. The reason may be that the active ingredients in the warm mud mask are gradually absorbed and acted on the skin, thus bringing about sustained improvement.

[0120] Due to genetic and environmental factors, such as excessive ultraviolet radiation, aging, psychological stress, and allergies, skin disorders can lead to the release of inflammatory mediators in keratinocytes in the epidermis, mediating the participation of microvascular fibroblasts and endothelial cells in immune and inflammatory responses and increasing microvascular blood flow. When Wu Chuanhong and others studied the effect of Mayinglong Babao Eye Cream on improving dark circles, the results showed that Mayinglong Babao Eye Cream can reduce local blood perfusion, proving that the product has an anti-inflammatory effect. Figure 6 This is a graph showing the changes in blood perfusion volume before and after the use of the temperature-sensitive mud mask prepared in Example 1. Figure 6It can be seen that after using the warm mud mask for 15 minutes, the blood flow value in the test area decreased significantly compared with the blank value, and the improvement rate reached 38.98%, and the data had significant differences (***P < 0.001). The blood perfusion at 5 minutes and 2 hours after cleaning decreased by 7.18% (significant difference, *P < 0.05) and 2.94% respectively compared with the blank value. The results show that the warm mud mask can significantly reduce the blood perfusion of the skin, proving that the warm mud mask has the effect of inhibiting inflammation. The reason may be that the mineral elements such as lithium, selenium, magnesium, iron, potassium, copper, zinc, and selenium contained in the black mud act as skin cleansing and purifying agents, which have the effects of anti-inflammatory desensitization and preventing natural aging of the skin.

[0121] Figure 7 This is an analysis chart of the questionnaire results before and after the use of the temperature-sensitive mud mask prepared in Example 1. Figure 7 It can be seen that: 91% of the subjects believed that the warm mud mask had a continuous warm feeling during use, 97% of the subjects believed that the warm mud mask was gentle and non-irritating, and more than 94% of the subjects believed that there was no discomfort or adverse reaction.

[0122] Example 2

[0123] The black mud powder of Yuncheng Salt Pond, cetearyl alcohol, 1.3-butylene glycol, hexylene glycol, glyceryl polyether-26, niacinamide, sodium hyaluronate (molecular weight of 30,000-50,000 Da), sodium hyaluronate (molecular weight of 200,000-400,000 Da), acetyl glucosamine, tetrahydromethylpyrimidine carboxylic acid, hectorite, oat kernel powder, PEG-4 polyglyceryl-2 stearate, tri(laureth-4) phosphate, citric acid, p-hydroxyacetophenone, sodium polyacryloyldimethyl taurate, ammonium acryloyldimethyl taurate / behenyl alcohol polyether-25 methacrylate crosslinked polymer, Yuncheng Salt Pond salt, EDTA-2Na, hot The mass percentages of the thermal agent, Centella asiatica leaf extract, lactobacillus fermentation product, α-bisabolol and collagen are 10%: 12%: 6%: 0.5%: 8%: 3%: 0.05%: 0.05%: 2%: 0.1: 4%: 0.5%: 2%: 2%: 0.8%: 0.5%: 0.2%: 0.1%: 0.9%, 0.2%: 0.16%: 0.1%: 0.1%: 0.1%: 0.02%, and the remainder is glycerol, and the total is 100%; among them, the mass percentages of vanillyl butyl ether and clove bud oil in the thermal agent are 1:1; the others are consistent with Example 1, and a warm facial mask is obtained.

[0124] turn out:

[0125] When the mud mask is applied on the face, a gentle warm sensation can be felt immediately, and the warm sensation can last for a long time. After waiting for 15 minutes, the mud mask is washed off. The skin's moisture and glossiness are significantly improved, and the subjects have a good user experience.

[0126] Example 3

[0127] The black mud powder of Yuncheng Salt Pond in Example 1, cetearyl alcohol, 1.3-butylene glycol, hexylene glycol, glyceryl polyether-26, niacinamide, sodium hyaluronate (molecular weight of 30,000-50,000 Da), sodium hyaluronate (molecular weight of 200,000-400,000 Da), acetyl glucosamine, tetrahydromethylpyrimidine carboxylic acid, hectorite, oat kernel powder, PEG-4 polyglyceryl-2 stearate, tri(laureth-4) phosphate, citric acid, p-hydroxyacetophenone, sodium polyacryloyldimethyl taurate, ammonium acryloyldimethyl taurate / behenyl alcohol polyether-25 methacrylate crosslinked polymer, Yuncheng Salt The mass percentages of pool salt, EDTA-2Na, thermal agent, Centella asiatica leaf extract, lactobacillus fermentation product, α-bisabolol and collagen are 14%: 9%: 8%: 0.5%: 5%: 2%: 0.1%: 0.1%: 1%: 0.1: 1%: 0.1%: 1.5%: 1.5%: 1.2%: 0.5%: 0.1%: 0.15%: 0.9%: 0.1%: 0.2%: 0.1%: 0.1%: 0.1%: 0.02%, and the remainder is glycerol, and the total is 100%; the rest is consistent with Example 1 to obtain a thermal mask.

[0128] turn out:

[0129] When the mud mask is applied on the face, a gentle warm sensation can be felt immediately, and the warm sensation can last for a long time. After waiting for 15 minutes, the mud mask is washed off. The skin's moisture and glossiness are significantly improved, and the subjects have a good user experience.

[0130] Example 4 Selection of thermal sensitizer

[0131] The thermal agent of phase D in Example 1 was adjusted to be oryzanol, ginger root extract / bisabolol (1:50, raw materials from Symrise 100), vanillyl butyl ether, by reducing or increasing the amount of glycerol, the amount of thermal sensitizer is as shown in Table 2, and other conditions or parameters are consistent with those in Example 1 to obtain a mud film.

[0132] The mud film was subjected to performance testing, and the test results are as follows;

[0133] Table 2 Effects of different types of thermal agents on heating of mud film

[0134]

[0135] Note: Data in the table are all mass percentage unless otherwise specified.

[0136] As can be seen from Table 2: referring to the existing literature (Xu Renpu, Xu Dashen. Application and development of oryzanol in the field of skin [J]. Grain and Oil, 1995, (4): 32-36.), the dosage of oryzanol is generally 0.5%-1%. However, the experimental results show that the mud mask prepared by adding 5% oryzanol in the formula does not feel hot during use; similarly, the mud mask prepared by adding 5% ginger root extract / bisabolol does not feel hot during use; adding the above two heat-sensing agents in a mass ratio of 1:1 to the mud mask still has no obvious effect; adding only 0.03% of vanillyl butyl ether, there is a feeling of heat, and it lasts for a long time. In summary, vanillyl butyl ether was finally selected as the heat-sensing agent for subsequent research.

[0137] Example 5

[0138] The essential oil variety in the thermal agent of phase D of Example 1 was adjusted, and the clove bud oil was replaced with clove basil oil, fennel oil, caraway oil, and oregano oil, respectively, and the amounts used were as shown in Table 3. Other conditions or parameters were consistent with those in Example 1 to obtain a mud mask.

[0139] The mud film was subjected to performance testing, and the test results are as follows;

[0140] Table 3 Effects of different types of essential oils on heating of mud mask

[0141]

[0142] Note: Data in the table are all mass percentage unless otherwise specified.

[0143] It can be seen from Table 3 that clove bud oil has the effect of uniform heat sensation and auxiliary heating, but the effects of other essential oils are not obvious.

[0144] Example 6

[0145] The amount of vanillyl butyl ether in the phase D thermal agent of Example 1 was adjusted by reducing or increasing the amount of glycerol so that the mass fraction of vanillyl butyl ether was 2%, 1%, 0.5%, 0.25%, 0.1%, and 0.05%, and other conditions or parameters were consistent with those in Example 1 to obtain a mud film.

[0146] The obtained mud film was subjected to performance test, and the test results are as follows:

[0147] Table 4 Effect of vanillyl butyl ether content on facial use effect

[0148]

[0149] Note: Data in the table are all mass percentage unless otherwise specified.

[0150] It can be seen from Table 4 that the optimal amount of vanillyl butyl ether in the formula is 0.1%.

[0151] Example 7

[0152] The mass fraction of vanillyl butyl ether in the phase D thermal agent of Example 1 was adjusted to 0.1%, and the amount of clove bud oil and the amount of glycerol were adjusted so that the amount of clove bud oil was as shown in Table 5. Other conditions or parameters were consistent with those in Example 1 to obtain a mud film.

[0153] The obtained mud film was subjected to performance test, and the test results are as follows:

[0154] Table 5 Effect of different ratios of vanillyl butyl ether and clove bud oil on heating of mud mask

[0155]

[0156] Note: Data in the table are all mass percentage unless otherwise specified.

[0157] From Table 5, we can see that clove bud oil can reduce the hot and spicy sensation of vanillyl butyl ether, making the heat more uniform, and at the same time can cover up the unpleasant earthy and greasy smell in the product, giving the product a sweet and elegant floral fragrance, increasing the product's appeal and improving the product's quality. Therefore, the optimal mass ratio of vanillyl butyl ether to clove bud oil was finally determined to be 1:1.

[0158] Comparative Example 1

[0159] The glycerin in Example 1 was replaced by water, and other conditions or parameters were consistent with those in Example 1 to obtain a mud film.

[0160] The results showed that the mud mask was prone to cracking. There was a strong hot and irritating sensation during use. After waiting for 15 minutes, the skin on the face area where it was used would turn red (such as Figure 8 ).

[0161] Comparative Example 2

[0162] The vanillyl butyl ether in Example 1 was omitted, the amount of clove bud oil was adjusted to 0.2%, and the other conditions or parameters were consistent with those in Example 1 to obtain a mud film.

[0163] The questionnaire results found that 100% of the subjects believed that mud masks had no heating effect.

[0164] Comparative Example 3

[0165] The clove bud oil in Example 1 was omitted, the amount of vanillyl butyl ether was adjusted to 0.2%, and the other conditions or parameters were consistent with those in Example 1 to obtain a mud film.

[0166] The results of the questionnaire found that 100% of the subjects believed that the skin irritation was particularly severe, with a hot or tingling sensation.

[0167] However, Example 1 uses a combination of vanillyl butyl ether and clove bud oil to achieve a warming, non-irritating effect, and the moisturizing, brightening, and anti-inflammatory properties do not change significantly.

[0168] Although the present invention has been disclosed as above in the form of a preferred embodiment, it is not intended to limit the present invention. Anyone familiar with this technology can make various changes and modifications without departing from the spirit and scope of the present invention. Therefore, the scope of protection of the present invention should be based on the definition of the claims.

Claims

1. A non-irritating warm-sensing mud mask, characterized in that: Its components include: Yuncheng Salt Pond black mud powder, oil, alkanediol, moisturizer, filler adsorbent, emulsifier, pH adjuster, antibacterial and antibacterial synergist, thickener, chelating agent, thermal agent, auxiliary ingredients and glycerin; Among them, the thermal agent is a combination of vanillyl butyl ether and clove bud oil, and the mass ratio of the two is 1-10:1-10.

2. The temperature-sensitive mud film according to claim 1, characterized in that: The mass percentages of Yuncheng Salt Pond black mud powder, oil, alkanediol, moisturizer, filler adsorbent, emulsifier, pH adjuster, antibacterial and antibacterial synergist, thickener, chelating agent, thermal agent and auxiliary ingredients are 10-40%: 5-20%: 5-15%: 5-15%: 1-15%: 2-10%: 0.5-3.0%: 0.2-2%: 0.1-2%: 0.05-0.4%: 0.04-0.6%: 0.01-1%, and the rest is glycerol, and the total is 100%.

3. The temperature-sensitive mud film according to claim 1, characterized in that: The oil is one or more of white meadowfoam seed oil, olive oil, coconut oil, camellia seed oil, jojoba seed oil, shea butter, grape seed oil, hydrogenated lecithin, squalane, caprylic / capric / triglyceride, cetearyl alcohol, and monoglyceryl stearate; The emulsifier is one or more of fatty acid esters, sucrose fatty acid esters, fatty acid sorbitan, polyoxyethylene ethers, polyoxypropylene ethers, alkyl glucoside, glucose esters, stearyl esters, and alkyl ethers; The alkanediol is one or more of butanediol, pentanediol, hexanediol, 1,3-propylene glycol and octyl glycol; The filling adsorbent is selected from one or more of kaolin, bentonite, hectorite, diatomaceous earth, magnesium aluminum silicate, hydroxyethyl cellulose, sodium starch octenyl succinate, silica, charcoal, bamboo charcoal, activated carbon, and oat kernel powder; The moisturizing agent is one or more of sodium hyaluronate, hyaluronic acid, hydrolyzed hyaluronic acid, hydrolyzed sodium hyaluronate, sodium hyaluronate cross-polymer, acetylated sodium hyaluronate, tetrahydromethylpyrimidine carboxylic acid, glyceryl polyether-26, hydrolyzed corn starch, saccharide isomers, polyquaternium-51, sodium pyrrolidone carboxylate, zinc pyrrolidone carboxylate, sorbitol, trehalose, urea, β-glucan, yeast β-glucan, Dendrobium nobile stem extract, ceramide, dihydroxypropyl arginine hydrochloride, sodium alginate, acetyl glucosamine, niacinamide, betaine, allantoin, panthenol, Tremella fuciformis polysaccharide, maltodextrin, bifidosaccharomyces cerevisiae fermentation product lysate, yeast polypeptides, yeast fermentation product, yeast lysate, yeast extract, Pichia pastoris fermentation lysate filtrate, Bacillus fermentation product, Lactobacillus fermentation product, and Lactobacillus fermentation lysate; The pH adjuster is citric acid; The chelating agent is EDTA-2Na; The antibacterial and antibacterial synergist is one or more of ethylhexylglycerin, p-hydroxyacetophenone, caprylhydroxamic acid, dianthin, fullerene, astaxanthin, zinc lactate, zinc gluconate, and zinc sulfate; The thickener is one or more of ammonium acryloyldimethyltaurate / behenyl alcohol polyether-25 methacrylate cross-linked polymer, hydroxypropyl starch phosphate, sodium polyacryloyldimethyltaurate, ammonium acryloyldimethyltaurate / VP copolymer, xanthan gum, carbomer, sodium chloride, and Yuncheng Salt Lake Salt.

4. The temperature-sensitive mud film according to claim 1, characterized in that: The auxiliary ingredients are one or more of Centella asiatica extract, Centella asiatica leaf extract, Portulaca oleracea extract, Licorice root extract, Polygonum cuspidatum root extract, Ginseng extract, Scutellaria baicalensis root extract, Berberis vulgaris root extract, Andrographis paniculata extract, Gentiana root extract, Glycyrrhiza uralensis root extract, Gardenia jasminoides extract, Peony root bark extract, Ennan tomato bark extract, Chamomile flower extract, Camellia extract, Artemisia argyi leaf extract, Tea leaf extract, Rosemary leaf extract, Aloe vera leaf extract, Mulberry leaf extract, Thyme leaf extract, Black mulberry fruit extract, Lycium barbarum fruit extract, Strawberry fruit extract, Brazil nut seed extract, Akebia trifoliata extract, collagen, asiaticoside, madecassoside, N-palmitoyl hydroxyproline cetyl ester, rape sterols, and bisabolol.

5. A method for preparing the non-irritating warm-sensing mud mask according to any one of claims 1 to 4, characterized in that: The steps include: (1) mixing glycerin, alkanediol, humectant, pH adjuster, antibacterial and antibacterial synergist, thickener and chelating agent to obtain phase A; (2) mixing the filling adsorbent and the Yuncheng salt pond black mud powder uniformly to form phase B; then, adding phase B to phase A in batches under high-speed stirring until phase B is uniformly dispersed in the system to obtain a mixed phase; (3) mixing the oil and the emulsifier uniformly to obtain phase C; (4) mixing the thermal sensitizing agent and the auxiliary material components uniformly to obtain phase D; (5) Heat the mixed phase and phase C to 80-90°C respectively, then add phase C into the mixed phase for emulsification, and homogenize at high speed for 3-5 minutes; after the emulsification is completed, cool to 40-50°C, add phase D, mix evenly, and cool to 20-30°C to obtain a temperature-sensitive mud film.

6. The method according to claim 5, characterized in that In step (2), phase B is added to phase A in batches at 8000-10000 r / min. After the addition of phase B is completed, homogenization is continued at 8000-10000 r / min for 20-25 minutes until it is completely dispersed.

7. The method according to claim 5, characterized in that The emulsification in step (5) is carried out at 80-90° C. and 8000-10000 r / min for 3-5 min.

8. The method according to claim 5, characterized in that The uniform mixing in step (5) is carried out at 2500-3500 r / min for 2-3 min.

9. A method for improving the temperature sensitivity of a mud mask and reducing irritation, characterized in that: The non-irritating warm-sensing mud mask according to any one of claims 1 to 4 is used.

10. A warming dressing, characterized in that: The non-irritating warm-sensing mud mask according to any one of claims 1 to 4 is used.

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