CN107951732B - Rectorite tearing slurry mask - Google Patents

Rectorite tearing slurry mask Download PDF

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CN107951732B
CN107951732B CN201711436906.8A CN201711436906A CN107951732B CN 107951732 B CN107951732 B CN 107951732B CN 201711436906 A CN201711436906 A CN 201711436906A CN 107951732 B CN107951732 B CN 107951732B
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rectorite
mask
mud mask
chitosan
tear
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CN107951732A (en
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戴跃锋
康文术
何广文
颜少慰
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Syoung Cosmetics Manufacturing Co Ltd
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Hunan Yujia Cosmetics Manufacturing Co ltd
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A61K8/26Aluminium; Compounds thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/02Cosmetics or similar toiletry preparations characterised by special physical form
    • A61K8/0212Face masks
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A61K8/20Halogens; Compounds thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/36Carboxylic acids; Salts or anhydrides thereof
    • A61K8/365Hydroxycarboxylic acids; Ketocarboxylic acids
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/73Polysaccharides
    • A61K8/733Alginic acid; Salts thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/73Polysaccharides
    • A61K8/736Chitin; Chitosan; Derivatives thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q17/00Barrier preparations; Preparations brought into direct contact with the skin for affording protection against external influences, e.g. sunlight, X-rays or other harmful rays, corrosive materials, bacteria or insect stings
    • A61Q17/005Antimicrobial preparations
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/41Particular ingredients further characterized by their size
    • A61K2800/412Microsized, i.e. having sizes between 0.1 and 100 microns

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  • General Health & Medical Sciences (AREA)
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Abstract

The invention relates to a rectorite tearing mud mask, which comprises a mud mask composition and a film-forming spray composition; the mud mask composition comprises: 30-40% of rectorite powder, 1-2.6% of sodium alginate, 10-20% of auxiliary material and 100% of water; the film-forming spray composition comprises solvent water and: 1-2% of calcium chloride, 0.01-0.5% of chitosan and 0.01-0.1% of sodium citrate. The novel prepared mineral slurry tearing mask overcomes the defect that the drying speed of the slurry mask is high, reduces the risk of skin minimally-invasive injury caused by tearing the slurry mask to the maximum extent, enables the slurry mask to be easy to clean, and improves the skin care experience of a consumer using the slurry mask.

Description

Rectorite tearing slurry mask
Technical Field
The invention relates to the technical field of mud masks, in particular to a rectorite tearing mud mask.
Background
The facial masks are classified into a water washing facial mask and a paste facial mask, and only the paste facial mask can be classified into a bio-fiber facial mask, a non-woven fabric facial mask, a superfine fiber facial mask, a bamboo charcoal fiber facial mask and the like, and the water washing facial mask is mainly classified into a slurry facial mask and a non-slurry water washing facial mask (a sleeping facial mask, a fresh facial mask and the like).
The mask market is a monopoly competitive market, a large number of sellers and buyers exist in the market, a large number of enterprises produce different masks, manufacturers can easily enter and exit, and the characteristic that a large number of enterprises produce different masks is seen, from the product research and development to the final application on the face of a consumer, the consumer is not easy to determine what choice, but a plurality of components form different purchasing motivations.
On the premise of meeting the quality and safety of the facial mask, the innovation of considering the efficacy of the facial mask and solving the skin care requirement of consumers is fundamental. The domestic market is a market with huge throughput. No matter how many attractive facial masks exist at any time, the requirements are met, the effects are achieved, and as long as a new facial mask product with convincing effect is provided, a new consumption space can be opened, and the requirements of consumers are met.
The mud mask is an important branch in mask fine classification, is mainly deeply cleaned and is popular with the experience of nourishing skin by mineral trace elements, and is popular with consumers. The mud mask also has places with poor beauty, and is easy to dry quickly, so that the skin is tight; the traditional mud tearing mask is easy to infect and inflame due to the minimal trauma to the skin surface caused by strong tearing. The traditional mud mask mainly adopts kaolin, volcanic mud, deep sea mud and the like, and is lack of innovation breakthrough for the mud mask again.
Thus, the prior art remains to be improved.
Disclosure of Invention
Based on this, the invention aims to provide a novel two-component rectorite tear mud mask.
The specific technical scheme is as follows:
a rectorite tear mud mask comprises a mud mask composition and a film-forming spray composition;
the mud mask composition comprises the following components in percentage by mass: 30-40% of rectorite powder, 1-2.6% of sodium alginate, 10-20% of auxiliary material and 100% of water;
the film-forming spray composition comprises solvent water and the following components in percentage by mass: 1-2% of calcium chloride, 0.01-0.5% of chitosan and 0.01-0.1% of sodium citrate.
In some of these embodiments, the rectorite powder has a particle size of 1-10 μm.
In some of these embodiments, the chitosan has a molecular weight of 8000-12000 KD.
In some embodiments, the adjuvant is selected from one or more of a humectant, a thickener, a film forming agent, or a preservative.
In some of these embodiments, the adjuvant comprises glycerol, propylene glycol, butylene glycol, beta-glucan, xanthan gum, Sepic350, niacinamide, caprylyl glycine, arginine, titanium dioxide, tetrandra root extract, allantoin, and caprylyl hydroxamic acid.
Sepic350 special thickener, consisting of:
components Mass percent% Remarks for note
Polyacrylamide 40
C13-14 isoparaffin 20
Laureth-7 5
Water (W) 35
In some embodiments, the mud mask composition comprises the following components in percentage by mass: 30-40% of rectorite powder, 1-2.6% of sodium alginate, 1-3% of glycerol, 0.5-2% of propylene glycol, 2-4% of butanediol, 0.1-1% of beta-glucan, 0.1-0.5% of xanthan gum, 1-3% of Sepic350, 1-3% of nicotinamide, 0.1-1% of caprylyl glycine, 0.1-1% of arginine, 1-2% of titanium dioxide, 0.1-1% of tetrandra root extract, 0.1-0.5% of allantoin, 0.5-2% of caprylyl hydroximic acid and water which is added to reach 100%.
In some of these embodiments, the film-forming spray composition further comprises a preservative.
In some embodiments, the film-forming spray composition comprises solvent water and the following components in percentage by mass: 1-2% of calcium chloride, 0.01-0.5% of chitosan, 0.01-0.1% of sodium citrate and 0.5-2% of caprylyl hydroximic acid.
In some embodiments, the mud mask composition comprises the following components in percentage by mass: 35% of rectorite powder, 1.5% of sodium alginate, 2% of glycerol, 1% of propylene glycol, 3% of butanediol, 0.5% of beta-glucan, 0.2% of xanthan gum, 0.5% of Sepic 3502%, 2% of nicotinamide, 0.5% of caprylyl glycine, 0.5% of arginine, 1.5% of titanium dioxide, 0.5% of radix stephaniae tetrandrae extract, 0.2% of allantoin, 1% of caprylyl hydroximic acid and water until the content of water reaches 100%;
the film-forming spray composition comprises solvent water and the following components in percentage by mass: calcium chloride 1.5 percent, 0.1 percent of chitosan, 0.05 percent of sodium citrate and 1 percent of caprylyl hydroximic acid.
The rectorite tearing slurry mask is a bi-component mask and comprises a slurry mask composition and a film-forming spray composition, when the rectorite tearing slurry mask is used, the slurry mask composition is firstly coated on the surface of skin for about 10min, and then the film-forming spray composition is sprayed on the surface of the slurry mask, so that the slurry mask can form a film, the film can be completely peeled off from the skin, and the skin is not damaged minimally.
The novel mineral slurry tearing mask prepared by taking rectorite slurry as a mineral raw material, adopting sodium alginate and chitosan and calcium chloride as a moisturizing film-forming agent solves the defect of high drying speed of the slurry mask, reduces the risk of skin minimally-invasive injury caused by tearing the slurry mask to the maximum extent, enables the slurry mask to be easy to clean, and improves the skin care experience of a consumer using the slurry mask. The rectorite tearing mud mask can promote wound healing, control oil and inhibit bacteria, and accelerate repair of the acne skin.
The core raw materials of the rectorite tearing slurry mask, namely the rectorite, the chitosan, the sodium alginate and the calcium chloride, have unique mechanism and effect and bring excellent skin care experience, and are briefly described as follows:
1. rectorite
Rectorite is a mixture of dihedral mica and dihedral montmorillonite consisting of 1: the type 1 regular interstratified mineral has a structure formed by regularly and alternately stacking mica-like unit layers and montmorillonite-like unit layers. According to clay mineral structure classification, according to four-side wafer and octahedral wafer structure layer type classification, the rectorite structure unit layer contains two 2: 1 layer. In the mica unit layer 2: the interlayer cation of layer 1 may be Na+、K+、Ca2+(ii) a And 2 of the montmorillonite unit: 1 layer contains exchangeable hydrated cation Na+、Ca2+、Mg2 +、Al3+、Sr2+And the like. The octahedra in the two types of unit layers are largely occupied by aluminum, and the trimethylcationic aluminum occupies only 2/3 octahedra, i.e., the dihedral subclass. The crystal structure of rectorite determines that rectorite minerals have unique mineral physical properties.
(1) Adsorptivity and cation exchange Property
The crystal structure of the rectorite is formed by regularly and alternately stacking the mica-like and the montmorillonite-like. Interlayer domain bound by highly negatively charged tetrahedral sheets of mica as charge-compensated Na+、K+、Ca2+The separation is fixed and not exchangeable, and the layers are not expanded. Montmorillonite is 2: layer 1 layered aluminosilicate minerals, the hydrated cations between layers can be exchanged by a large number of other inorganic, organic cations, such as sodium, aluminum, silicon, etc. in single or composite form, which can adsorb various inorganic particles, organic componentsAnd both the adsorption and exchange processes are reversible.
(2) High dispersibility
The rectorite is easy to disperse when meeting water, the particle size of the rectorite is less than 1 mu m, the particles form a smooth film, the effect is better after the rectorite is added with a small amount of alkali, and the rectorite can suspend for a long time.
(3) Ultraviolet blocking
The colloid value of the rectorite is 50-90ml/15g, the rectorite has good ultraviolet blocking capability naturally, and the absorption and blocking effect on short-wavelength light or radiation waves is obvious.
(4) Inter-layer pore diameter variability
The pore size between layers of rectorite can be modified after ion exchange with different treating agents. Calcium-based exchange and synthesis of cross-linked rectorite can form a large-aperture layer columnar two-dimensional channel structure between 1.5 and 4nm, so that the interlayer aperture is variable. The physical properties of the clay mineral are changed, but the structure is inconvenient, for example, the clay mineral is hydrophilic, and the clay organic complex can be changed into oleophilic, which is more beneficial to deep cleaning and absorbs redundant grease.
The method selects rectorite powder with the grain diameter of 1250 meshes as a core raw material.
2. Sodium alginate
Sodium alginate is a natural polysaccharide compound extracted from seaweed, is a powdery solid with white to faint yellow color, is almost odorless and tasteless, low-heat and nontoxic, has strong hygroscopicity, high water retention capacity, is easy to dissolve in water, is easy to swell in warm water, and is insoluble in ethanol and diethyl ether. It is a linear block copolymer formed by linking 2 structural units of guluronic acid (G section) and a stereoisomer mannuronic acid (M section) thereof in three modes (MM section, GG section and MG section) through alpha (1,4) glycosidic bonds. Adding Ca to the aqueous solution2+After cation, Na on G block unit+After ion exchange with divalent ions, G groups are stacked to form a cross-linked grid structure, so that the hydrogel is converted.
The extraction process of the sodium alginate comprises the following steps: drying harvested seaweed, crushing, washing with water to remove impurities to obtain clean seaweed, adding hot alkali solution, dissolving the seaweed, removing impurities, adding calcium chloride solution, mixing to obtain calcium alginate precipitate, adding acid solution to obtain seaweed colloid, adding sodium carbonate to obtain sodium alginate, drying, and grinding to obtain sodium alginate powder.
The invention is based on the consideration of film forming performance and cost, and the control range of sodium alginate concentration is selected to be 1-2.6%.
3. Chitosan
The chitosan is prepared by deacetylating chitin to remove more than 50% of acetyl, and is chemically poly (1,4) -2-amino-deoxy-beta-D-glucan. It is the only basic polysaccharide in natural polysaccharides and has many unique physicochemical properties. Because of its good biocompatibility, very little toxicity and economy, it is receiving attention from various pharmaceutical research institutes.
By utilizing the fact that a large number of primary amino groups are arranged on a molecular chain of chitosan and a large number of carboxyl groups are arranged on a molecular chain of sodium alginate, a polyelectrolyte membrane can be formed through positive and negative charges in an attractive mode under the action of static electricity. The film formation mechanism was investigated by differential scanning calorimetry. The chitosan and the sodium alginate are promoted to be not independently present in the mask, but to be subjected to electrostatic interaction and present in a new mutual combination state. The electrostatic interaction of sodium alginate carboxyl and chitosan amino quality inspection is the main force of a complex structure.
The sodium alginate/chitosan microcapsule is formed by utilizing two natural high molecular polysaccharides of sodium alginate and chitosan through polyelectrolyte complexation, which is beneficial to effective slow release of active ingredients in a formula and provides long-acting moisture retention.
4. Calcium chloride
Calcium chloride of the chemical formula CaCl2. Slightly bitter and tasteless. It is typically an ionic halide that is white, hard, in small pieces or particles at room temperature. Colorless cubic crystal, white or off-white, granular, honeycomb block, spherical, irregular granular and powdery. Slight toxicity, no odor, and slightly bitter taste. The moisture absorption is extremely strong, and the deliquescence is extremely easy when the paint is exposed to the air. Is easily dissolved in water, and releases a large amount of heat (the dissolution enthalpy of calcium chloride is-176.2 cal/g), and the aqueous solution is slightly acidic. Dissolving in alcohol, acetone, and acetic acid. Reacting with ammonia or ethanol to respectively generate CaCl2·8NH3And CaCl2·4C2H5An OH complex. The solution is crystallized at low temperature to precipitate hexahydrate, which is dissolved in self-crystallization water when gradually heated to 30 ℃, and is gradually dehydrated when continuously heated to 200 ℃ to become dihydrate, and is changed into white porous anhydrous calcium chloride when heated to 260 ℃.
The rectorite tearing slurry mask adopts 1.5% of calcium chloride aqueous solution, and calcium chloride solution with different concentrations and sodium alginate form hydrogel fiber, so that the mineral slurry mask can be quickly peeled off from the face, and the mineral slurry mask can be easily cleaned and cleaned, and brings interesting and good skin care experience to consumers.
4.1 hydrogel mechanism
Sodium alginate is a linear anionic polysaccharide extracted from natural brown algae, and is a copolymer mainly composed of alpha-mannuronic acid (M section) and beta-D guluronic acid (G section) which are linked by virtue of 1,4 glycosidic bonds and according to different G-G, M-M, G-M segments, when divalent calcium ions exist, the calcium ions and the G section in the macromolecules of the sodium alginate are stacked to form a core-shell structure, and the three-dimensional network hydrogel is obtained through crosslinking.
The calcium alginate hydrogel is ion-embedded hydrogel, sodium alginate is combined with solution containing calcium ions, only G unit participates in ion crosslinking, two homopolymerized G units are combined through synergistic effect, diamond-type hydrophilic space is formed in the middle, and Ca is contained in the hydrophilic space2+Occupy these spaces and chelate with multiple oxygen atoms on the G unit, the alginate chains are tightly bound to each other and interact to form a three-dimensional network structure, Ca2+Embedded in the egg like an egg to form an egg lattice structure, while the homopolymerized M block cannot react with Ca2+The structure is formed due to the characteristics of high toughness, easy bending and the like. The alternating GM blocks link the blocks together during the formation of the hydrogel and do not have a direct effect.
4.2 hydrogel efficacy
The calcium alginate hydrogel network structure provides convenience for the mineral slurry mask after use and easy peeling and cleaning, and also provides a mild environment for skin and allows the discharge of oxygen, protein and metabolites. The calcium alginate hydrogel provides a good physical barrier for skin, increases the moisture content on the surface of the skin, and reduces the moisture loss.
5. Film formation influencing factor
5.1 Effect of Chitosan
(1) Influence of molecular weight
The influence mechanism of the chitosan molecular weight on the microcapsule membrane strength comprises the diffusion rate and degree of chitosan molecules entering a calcium alginate gel network and the reaction degree between the chitosan molecules and sodium alginate molecules. Chitosan with large molecular mass has larger size of the link space, so that the resistance of the chitosan diffusing into the calcium alginate network is larger, and the diffusion rate and the diffusion degree are relatively lower, so that the film forming reaction mainly occurs on the surface of the calcium alginate gel, and even if the number of amino groups positively charged on the chain links is more, the reaction degree with sodium alginate molecules is still lower, and the formed film is thin; the chitosan with low molecular weight has low steric hindrance, is easy to enter a calcium alginate gel network, and the number of the entered molecules is increased while the number of the provided amino groups is also increased, so that the degree of reaction with sodium alginate molecules is increased, the thickness of the generated film is increased, and the anti-swelling force is enhanced.
(2) Influence of pH value
The sodium alginate-chitosan capsule membrane is formed by the electrostatic interaction of protonated amino groups on chitosan molecules and carboxyl groups of an M unit of sodium alginate, the pH value of a chitosan solution directly influences the charge distribution and the molecular structure of two natural polymer materials, and when the pH value of the solution is close to the PKA (PKA) of chitosan of 6.3, the chitosan molecules are almost uncharged at the moment, the charge density is remarkably reduced, the molecular space extension is small, the molecular diffusion coefficient is high, the solution can enter a calcium alginate gel network more deeply, and the degree of polyelectrolyte complexation is deep, so the membrane thickness is thick;
(3) influence of solution concentration
The calcium alginate gel is prepared under the same condition, when the concentration gradient of the chitosan solution and the chitosan concentration gradient in the calcium alginate are increased, the diffusion power of chitosan molecules is increased, the diffusion degree and the reaction degree are correspondingly increased, the membrane is thickened, and the anti-swelling capacity is enhanced.
The rectorite tearing slurry mask selects chitosan oligosaccharide with the molecular weight of 8000-12000KD, the concentration range of the chitosan is controlled to be 0.01-0.5 percent based on the consideration of cost and film-forming performance, and the PH of the prepared aqueous solution is close to 6.3.
The slurry mask composition in the rectorite slurry mask is prepared by using rectorite and sodium alginate as main raw materials, and the film-forming spray composition is prepared by using calcium chloride, chitosan and sodium citrate to prepare a solution. The invention adopts a one-step film forming technology, and the mixed solution of chitosan, calcium chloride and sodium citrate is directly sprayed on a mineral slurry mask containing sodium alginate, so that the sodium alginate sequentially forms a chitosan deposition layer, a chitosan/sodium alginate complex layer and a calcium alginate coacervate.
The rectorite tearing slurry mask is unique in use method, a customer generally applies the slurry mask for about 15 minutes, the mask is applied with the slurry mask for about 10 minutes, calcium chloride solution is sprayed on the surface of the slurry mask by using calcium chloride spray under the condition of eye closure, the mask is applied for 5 minutes, the whole slurry mask can be peeled off from the facial skin, the skin is deeply cleaned and oiled, the skin is sealed and moisturized, and good skin care experience is brought.
Drawings
FIG. 1 is a graph comparing the percentage reduction of oil content;
FIG. 2 is a graph of the percent change in moisture content increase;
fig. 3 is a graph comparing the percent increase in moisture loss.
Detailed Description
In order that the invention may be more fully understood, reference will now be made to the following description. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
The rectorite tear mud mask of the embodiment comprises a mud mask composition and a film-forming spray composition.
1. Mud mask composition
(1) Formula proportion
Figure BDA0001525975890000081
Figure BDA0001525975890000091
(2) Formula process of mud mask composition
1) Weighing glycerol, propylene glycol, butanediol, beta-glucan, allantoin and sodium alginate according to the formula ratio, respectively adding into deionized water, heating to 80-85 ℃, stirring for 25min at the temperature of 200-;
2) reducing the temperature to 75-80 ℃, sequentially adding nicotinamide, caprylyl glycine, arginine and xanthan gum, stirring at 500r/min for 15 min;
3) weighing rectorite powder, titanium dioxide powder and SPEC305 according to the formula ratio, sequentially adding the rectorite powder, the titanium dioxide powder and the SPEC305, starting a homogenizer, homogenizing for 10min at 8000-10000r/min, and preserving heat for 30 min;
4) reducing the temperature to 45-55 ℃, sequentially adding the tetrandra root extract and the caprylyl hydroximic acid, stirring at the speed of 600-800r/min for 30min, and cooling to the normal temperature.
2. Film-forming spray composition
(1) Formula proportion
Formulation components Example 1 (%) Example 2 (%) Example 3 (%)
Calcium chloride 1.5 1 2
Chitosan 0.1 0.5 0.05
Citric acid sodium salt 0.05 0.01 0.1
Octanoyl hydroximic acid 1 2 0.5
Deionized water To 100 To 100 To 100
(2) Film-forming spray composition formulation process
1) Weighing chitosan according to the formula ratio, adding the chitosan into deionized water, heating to 75-80 ℃, stirring for 20-30min at the speed of 500-;
2) cooling to 45-50 ℃, sequentially adding calcium chloride, sodium citrate and caprylyl hydroximic acid at the speed of 200-300r/min until all the calcium chloride, the sodium citrate and the caprylyl hydroximic acid are dissolved, stopping stirring and cooling to room temperature.
3. Efficacy evaluation
3.1 oil control evaluation
(1) Principle of testing
The efficacy of the oil absorption paper using effect is evaluated by a skin oil tester Sebumeter SM815 of German CK. The oil content test adopts a world recognized SEBUMETER method, which is based on the principle of photometer, after a special extinction adhesive tape with the thickness of 0.1mm absorbs oil on human skin, the special extinction adhesive tape becomes a semitransparent adhesive tape, the light transmission quantity of the semitransparent adhesive tape changes, the more the absorbed oil, the greater the light transmission quantity, and thus, the content of the skin oil can be measured. The test probe has the greatest advantages of small volume and convenient use, and can test any part of the skin. This is an indirect measurement of the secretion of the oil glands, and the result can be used to distinguish between different skin types, making it possible to accurately understand the changes in oil caused by internal and external causes.
(2) Test method
The test selects 21 test objects, 3 people are divided into 7 groups, 3 areas with the size of 3cm x 3cm are drawn on the forehead respectively, skin oil content evaluation is carried out on blank samples (samples are not wiped), reference samples (slurry mask composition in example 1 is washed by water and is not sprayed) and patent samples (slurry mask composition in example 1 and film-forming spraying) respectively, and the average value of three persons of each reference sample is calculated to calculate the percentage of the oil content increment for carrying out correlation evaluation.
1) The selected test subjects were aged 18 to 30 years and were informed and consented to the subjects, and after the subjects cleaned their faces for 15 minutes, the fat content in the forehead was determined as an initial value.
2) The method comprises the following steps of (1) not coating a sample on the blank area of the forehead of a subject, weighing 0.5ml of essence in a control sample area and a patent sample area, soaking and covering the skin with 3cm × 3cm of non-woven fabric membrane cloth for 20min, taking down the non-woven fabric, standing for 10min, respectively measuring the oil content of three areas, testing once every 30min, and continuously evaluating for 2 h;
3) and (3) testing environment: testing the environment temperature T of 25 ℃ and the humidity H of 50;
4) and (3) testing time: cleaning the face before testing, testing the initial oil content in 15 minutes, and testing the oil content data in 30min,60min,90min and 120min respectively;
5) testing parts: the test area of the blank, control sample, patent sample is marked on the forehead.
3.2 evaluation of moisturization
(1) Testing instrument
A multifunctional skin tester, model CUTOMETER DUAL MPA 580, from CK, Germany, selects a skin moisture content test probe and a skin moisture loss TEWL test probe.
(2) Test method
1) MMV (moisture content) testing method for skin moisture content
The test principle is as follows:
the method adopts a capacitance method to test the moisture content of the horny layer of the human skin, the principle is that the capacitance value of the skin is different according to the difference of the water content of the skin based on the obvious difference of the dielectric constants of water and other substances, and the observation parameters can represent the moisture value of the skin.
Test conditions and volunteer requirements
And (3) testing environmental conditions: the testing environment temperature is 22 +/-1 ℃, the humidity is 50 +/-5%, and real-time dynamic detection is carried out;
the volunteer requires: at least 30 effective volunteers, aged between 16-65 years (except pregnant or lactating women): the base value of the capacitance skin moisture determination meaning of the forearm test area is between 15 and 100: patients without severe systemic disease, immunodeficiency or autoimmune disease; those with no active allergic disease; those who have not had a history of severe allergy to skin care cosmetics in the past; hormone drugs and immunosuppressants have not been used in the last month: for participating in other clinical trials; the tested drugs are used according to the regulations and the data is complete; all volunteers should fill out informed consent before testing;
preparation before testing:
any product (cosmetic or external medicine) cannot be used for 2-3 days before the tested part. Before the experiment, the subject should agree to clean the forearm of both hands, measure the forearm and wipe it clean with dry tissue. After cleaning, the measuring area mark is made on the inner side of the forearm of the test subject. Before formal test, sitting still in a room meeting the standard for at least 30min, no drinking water, exposing forearms, placing in a test state, and keeping relaxed.
The testing steps are as follows:
the inner side of the left and right arm in the experiment is marked with 3 x 3cm2In the test area, the same arm can mark a plurality of areas, and the areas are spaced by 1 cm. Both the patent sample (example 1 mud mask composition + film forming spray composition) and the control sample (example 1 mud mask composition water scrub) were randomly distributed on the left and right arms. The measurement of the test area and the control area was performed using a capacitance skin meter. Each area was assayed 15 times in parallel. The blank value of each test area was measured and then measured at 1.0. + -. 0.1mg sample/cm2The test was evenly spread into the test area using a latex finger cot. The skin moisture content of the test area and the control area (determined according to the time during verification) is measured by smearing for 30min,60min and 90min respectively, and the test of the same volunteer is completed by the same measuring person.
Test data:
and respectively measuring the MMV value of each time period according to the design of the experiment.
2) Percutaneous water loss TEWL test method
The test principle is as follows:
the measurement principle of the test instrument is derived from FICK Fick diffusion law: dm/dt ═ d.a.dp/dx. Two groups of temperature and humidity sensors are used for measuring the water vapor pressure gradient formed by the loss of moisture in the near epidermis (within about 1 cm) from the cuticle at different bright points, and the moisture content of the percutaneous emission is directly measured. The TEWL value is an important indicator of the quality of the skin barrier, and a lower TEWL value indicates a better barrier function of the skin, whereas a worse.
Test conditions and volunteer requirements
And (3) testing environmental conditions: the testing environment temperature is 22 +/-1 ℃, the humidity is 50 +/-5%, and real-time dynamic detection is carried out;
the volunteer requires: at least 30 effective volunteers, aged between 16-65 years (except pregnant or lactating women): the base value of the capacitance skin moisture determination meaning of the forearm test area is between 15 and 100: patients without severe systemic disease, immunodeficiency or autoimmune disease; those with no active allergic disease; those who have not had a history of severe allergy to skin care cosmetics in the past; hormone drugs and immunosuppressants have not been used in the last month: for participating in other clinical trials; the tested drugs are used according to the regulations and the data is complete; all volunteers should fill out informed consent before testing;
preparation before testing:
any product (cosmetic or external medicine) cannot be used for 2-3 days before the tested part. Before the experiment, the subject should agree to clean the forearm of both hands, measure the forearm and wipe it clean with dry tissue. After cleaning, the measuring area mark is made on the inner side of the forearm of the test subject. Before formal test, sitting still in a room meeting the standard for at least 30min, no drinking water, exposing forearms, placing in a test state, and keeping relaxed.
The testing steps are as follows:
the inner side of the left and right arm in the experiment is marked with 3 x 3cm2In the test area, the same arm can mark a plurality of areas, and the areas are spaced by 1 cm. Both the patent sample (example 1 mud mask composition + film forming spray composition) and the control sample (example 1 mud mask composition water scrub) were randomly distributed on the left and right arms. The measurement of the test area and the control area was performed using a capacitance skin meter. Each area was assayed 15 times in parallel. The blank value of each test area was measured and then measured at 1.0. + -. 0.1mg sample/cm2The test was evenly spread into the test area using a latex finger cot. The smearing was measured for 30min,60min and 90min, respectively, and the skin moisture loss TEWL (measured at this time during the verification) was measured for the test area and the control area, and the test was performed by the same measuring person for the same volunteer. Test data
The TEWL values were measured for each time interval according to the experimental design.
4. Evaluation results of efficacy
4.1 oil content
O%=(O1-O2)/O1*100%
O1-skin oil content before use;
o2-skin oil content after application;
o% -reduction of oil content;
as shown in fig. 1: example 1 a slurry facial mask prepared from rectorite powder and sodium alginate, and a tear slurry facial mask prepared from chitosan and calcium chloride as main raw materials by spraying, wherein the dense slurry facial mask formed from sodium alginate, chitosan and calcium chloride has the advantages of remarkably reducing oil secretion, reducing the oil content to 78.38% in 30min, and inhibiting the oil secretion to 47.61% after 120 min.
4.2 moisture content
W%=(W2-W1)/W1*100%
W1-skin moisture content before use;
w2-moisture content of skin after application;
w% -percentage increase in skin moisture content before and after use.
As shown in fig. 2: in the embodiment 1, the slurry facial mask prepared by rectorite powder and sodium alginate and the tear slurry facial mask prepared by spraying and prepared by taking chitosan and calcium chloride as main raw materials form a compact slurry facial mask due to the sodium alginate, the chitosan and the calcium chloride, so that the effect of remarkably improving the moisture content of skin is achieved, the moisture content is improved by 18.83% in a control sample, and the moisture content is improved by 35% in a patent sample.
4.3 Water loss
T%=(T2-T1)/T1*100%
T1-moisture loss value on skin surface before use;
t2-moisture loss value on skin surface after use;
t% -the percentage increase of the water loss of the skin before and after use.
As shown in fig. 3: in the embodiment 1, the slurry facial mask prepared by rectorite slurry and sodium alginate and the tearing slurry facial mask prepared by spraying and prepared by taking chitosan and calcium chloride as main raw materials form a compact slurry facial mask and have the effect of relatively reducing the water loss of skin, so that the tearing slurry is proved to be mild in surface and not to cause skin barrier damage by peeling.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.

Claims (9)

1. A rectorite tear mud mask is characterized by comprising a mud mask composition and a film-forming spray composition;
the mud mask composition comprises the following components in percentage by mass: 30-40% of rectorite powder, 1-2.6% of sodium alginate, 10-20% of auxiliary material and 100% of water;
the film-forming spray composition comprises solvent water and the following components in percentage by mass: 1-2% of calcium chloride, 0.01-0.5% of chitosan and 0.01-0.1% of sodium citrate.
2. The rectorite tear mud mask as claimed in claim 1, wherein said rectorite powder has a particle size of 1-10 μm.
3. The rectorite tear away mud mask as claimed in claim 1, wherein the chitosan has a molecular weight of 8000-12000 KD.
4. The rectorite tear mud mask as claimed in any one of claims 1 to 3, wherein said excipients are selected from one or more of humectants, thickeners, film formers or preservatives.
5. The rectorite tear mud mask as claimed in claim 4, wherein said excipients comprise glycerin, propylene glycol, butylene glycol, β -glucan, xanthan gum, Sepic350, niacinamide, caprylyl glycine, arginine, titanium dioxide, tetrandra root extract, allantoin and caprylyl hydroxamic acid.
6. The rectorite tear mud mask as claimed in claim 5, wherein said mud mask composition comprises the following components in percentage by mass: 30-40% of rectorite powder, 1-2.6% of sodium alginate, 1-3% of glycerol, 0.5-2% of propylene glycol, 2-4% of butanediol, 0.1-1% of beta-glucan, 0.1-0.5% of xanthan gum, 1-3% of Sepic350, 1-3% of nicotinamide, 0.1-1% of caprylyl glycine, 0.1-1% of arginine, 1-2% of titanium dioxide, 0.1-1% of tetrandra root extract, 0.1-0.5% of allantoin, 0.5-2% of caprylyl hydroximic acid and water which is added to reach 100%.
7. The rectorite tear mud mask as claimed in any one of claims 1 to 3, wherein said film forming spray composition further comprises a preservative.
8. The rectorite tear mud mask as claimed in claim 7, wherein said film forming spray composition comprises solvent water and the following components in mass percent: 1-2% of calcium chloride, 0.01-0.5% of chitosan, 0.01-0.1% of sodium citrate and 0.5-2% of caprylyl hydroximic acid.
9. The rectorite tear mud mask as claimed in claim 1,
the mud mask composition comprises the following components in percentage by mass: 35% of rectorite powder, 1.5% of sodium alginate, 2% of glycerol, 1% of propylene glycol, 3% of butanediol, 0.5% of beta-glucan, 0.2% of xanthan gum, 0.5% of Sepic 3502%, 2% of nicotinamide, 0.5% of caprylyl glycine, 0.5% of arginine, 1.5% of titanium dioxide, 0.5% of radix stephaniae tetrandrae extract, 0.2% of allantoin, 1% of caprylyl hydroximic acid and water until the content of water reaches 100%;
the film-forming spray composition comprises solvent water and the following components in percentage by mass: 1.5 percent of calcium chloride, 0.1 percent of chitosan, 0.05 percent of sodium citrate and 1 percent of caprylyl hydroximic acid.
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Address after: 410000 No. 390, Guyuan Road, Changsha hi tech Development Zone, Changsha City, Hunan Province

Patentee after: Shuiyang Cosmetics Manufacturing Co.,Ltd.

Address before: No. 668, Qingshan Road, Changsha hi tech Development Zone, Changsha City, Hunan Province, 410205

Patentee before: HUNAN YUJIA COSMETICS MANUFACTURING Co.,Ltd.