CN113181078A - Moistening and astringing type deep cleaning mask powder - Google Patents
Moistening and astringing type deep cleaning mask powder Download PDFInfo
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- CN113181078A CN113181078A CN202110556607.8A CN202110556607A CN113181078A CN 113181078 A CN113181078 A CN 113181078A CN 202110556607 A CN202110556607 A CN 202110556607A CN 113181078 A CN113181078 A CN 113181078A
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
- A61K8/73—Polysaccharides
- A61K8/738—Cyclodextrins
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
- A61K8/0216—Solid or semisolid forms
- A61K8/022—Powders; Compacted Powders
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- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
- A61K8/34—Alcohols
- A61K8/345—Alcohols containing more than one hydroxy group
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
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- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/67—Vitamins
- A61K8/671—Vitamin A; Derivatives thereof, e.g. ester of vitamin A acid, ester of retinol, retinol, retinal
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- A—HUMAN NECESSITIES
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- A61K8/922—Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof of vegetable origin
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- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
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Abstract
The invention discloses moistening and astringing type deep cleaning mask powder which comprises the following raw materials in parts by weight: 20-30 parts of modified cyclodextrin metal organic framework material, 10-15 parts of kaolin, 1-5 parts of trehalose, 3-5 parts of sodium hyaluronate, 3-5 parts of sorbitol powder, 1-5 parts of aloe extract, 1-5 parts of lycium ruthenicum extract and 0.5-1 part of citric acid. According to the invention, the modified cyclodextrin metal organic framework material is added as an adsorption material, and the porous structure and the large specific surface area of the adsorption material can enable the mask to have good oil control and cleaning effects; the rose essential oil is included in the cyclodextrin metal organic framework material and is connected with the retinal through an acetal structure, and the rose essential oil and the retinal are released in the using process of the facial mask, so that the facial mask also has the effects of moistening and moisturizing, pore refining, skin smoothing, whitening and wrinkle resisting, and the using performance of the cleaning facial mask is improved.
Description
Technical Field
The invention relates to the technical field of cleaning masks, in particular to moistening and astringing type deep cleaning mask powder.
Background
With the development of society and the improvement of living standard, the problem of environmental pollution is more and more serious, and more people are used to daily makeup, and pollutants such as dust and cosmetics and the residue of cosmetics on the face can cause the pore blockage of the face skin, so that the water and oil secretion of skin oil is disordered, and the puzzling skin problems such as acne, comedo and blackhead are caused. Therefore, the cleaning mask is used regularly to remove dirt remained on the surface of the skin and clean pores, and the generation of skin problems can be effectively reduced.
The cleaning facial mask in the prior art is generally divided into a tearing type cleaning facial mask and a smearing type cleaning facial mask, the tearing type cleaning facial mask is fully contacted and bonded with skin, when the facial mask is torn away from the skin, blackheads, aged cutin, grease and the like on the skin are stripped by means of the adhesion capacity of the tearing type cleaning facial mask, although the cleaning facial mask has a good cleaning effect, the skin is easy to loose, pores are large and skin allergy is caused due to the fact that the tearing force is strong, the use comfort is not good, and the skin is damaged greatly.
The smearing type cleaning mask is in a paste shape, the main components are clay components and mineral powder components such as kaolin, bentonite and perlite, and the like, and the components have excellent adsorption effect and can adsorb redundant grease on the skin, so that the smearing type cleaning mask has a good cleaning effect, is less in damage to the skin and is widely popular with consumers. But the skin cleansing cream has stronger adsorption and cleaning capabilities, and can also absorb moisture and oil in the skin, so that the skin is often pulled dry and tight after the cleansing cream is used, and the skin is even sensitive and reddened or even allergic under the condition that the skin is lack of water; and the pores cannot be timely converged and closed after being cleaned, so that the pores are easily large, and the cleaned skin is rough.
In order to avoid the skin from becoming dry, sensitive and rough after the facial mask is used, plant essential oil and other components are added into a part of the facial mask to improve the moisturizing and skin-tendering effects of the facial mask, but the addition of the plant essential oil and other components can reduce the content of adsorption components such as kaolin and the like, and the plant essential oil can be adsorbed on the surface of the kaolin to reduce the oil adsorption capacity of the kaolin, so that the oil control and cleaning capacity of the facial mask can be reduced. Therefore, the existing cleaning mask is difficult to give consideration to both the oil control cleaning effect and the moisturizing and skin-tendering effect, and cannot meet the requirements of consumers.
Disclosure of Invention
The invention provides moistening and astringing type deep cleaning mask powder for overcoming the problems that a cleaning mask in the prior art cannot meet the requirements of consumers because the oil control cleaning effect and the moistening and moisturizing skin-tendering effect are difficult to be considered at the same time, and the requirements of the consumers cannot be met; the rose essential oil is included in the cyclodextrin metal organic framework material and is connected with the retinal through an acetal structure, and the rose essential oil and the retinal are released in the using process of the facial mask, so that the facial mask also has the effects of moistening and moisturizing, pore refining, skin smoothing, whitening and wrinkle resisting, and the using performance of the cleaning facial mask is improved.
In order to achieve the purpose, the invention adopts the following technical scheme:
a moistening and astringing type deep cleaning mask powder comprises the following raw materials in parts by weight: 20-30 parts of a modified cyclodextrin metal organic framework material, 10-15 parts of kaolin, 1-5 parts of trehalose, 3-5 parts of sodium hyaluronate, 3-5 parts of sorbitol powder, 1-5 parts of aloe extract, 1-5 parts of lycium ruthenicum extract and 0.5-1 part of citric acid;
the preparation method of the modified cyclodextrin metal-organic framework material comprises the following steps:
A) dissolving gamma-cyclodextrin and KOH in water to prepare reaction mother liquor, adding methanol into the reaction mother liquor, uniformly mixing, heating to 50-60 ℃, and stirring for reacting for 5-6 hours; cooling to room temperature, adding hexadecyl trimethyl ammonium bromide, uniformly mixing, standing for 3-5 h, and separating, washing and drying a product to obtain the cyclodextrin metal organic framework material;
B) adding the cyclodextrin metal organic framework material into an ethanol solution of glacial acetic acid, stirring for reaction, separating, washing and drying a product to obtain a neutralized cyclodextrin metal organic framework material;
C) dispersing the neutralized cyclodextrin metal organic framework material in ethanol, adding retinene and p-toluenesulfonic acid, uniformly stirring, reacting at 60-70 ℃ for 18-24 h, separating and drying a product to obtain a retinene modified cyclodextrin metal organic framework material;
D) adding the retinal-modified cyclodextrin metal-organic framework material into an ethanol solution of rose essential oil, stirring and reacting for 3-5 h, and separating, washing and freeze-drying a product to obtain the modified cyclodextrin metal-organic framework material.
The modified cyclodextrin metal organic framework material and kaolin are used as an adsorbent together, and are compounded with moisturizing components such as sodium hyaluronate, sorbitol and the like and plant components such as aloe, lycium ruthenicum extract and the like to prepare the cleansing mask powder; the modified cyclodextrin metal organic framework material and kaolin can effectively adsorb grease in pores, so that the mask has the effect of deep cleaning; the aloe extract has good water replenishing, moisturizing and anti-inflammatory properties, and has a certain treatment effect on acne and acne marks; the lycium ruthenicum extract is rich in anthocyanin and procyanidine, has strong free radical scavenging and oxidation resisting performances, and enables the mask to have anti-wrinkle and anti-aging effects. When the facial mask powder is used, the facial mask powder is added into water, stirred into paste, smeared on the face for a period of time, and washed off, so that the facial mask powder is convenient to use and carry.
In the preparation process of the modified cyclodextrin metal-organic framework material, the gamma-cyclodextrin and the K are used in the step A)+The cyclodextrin metal organic framework material prepared by coordination self-assembly is a porous cubic crystal material, has ultrahigh specific surface area and porosity, has stronger adsorption performance, and can effectively adsorb residues and redundant grease in skin pores after being smeared on the face, so that the mask achieves the effect of deep cleaning. Since K + is introduced by KOH, step A) produces a cyclodextrin metal-organic framework materialThe mask is strong in alkalinity and easy to cause irritation and damage to the skin, so that the mask is subjected to neutralization modification by using acetic acid in the step B), and is mild and non-irritating to the skin when in use. In order to further improve the moistening, moisturizing and astringing effects of the mask and avoid the phenomena of dryness, tightness, large pores and the like after use, the invention also utilizes the acetalization reaction of retinene and hydroxyl on gamma-cyclodextrin in the step C) to connect the retinene to a cyclodextrin metal organic framework material through an acetal structure, and because the acetal structure is unstable and easy to decompose under acidic conditions, after the mask powder is stirred by adding water, the acetal bond can be broken under the acidic conditions provided by citric acid to release the retinene again, the retinene has biological activity similar to that of retinoic acid, can stimulate skin cells to accelerate renewal, can accelerate the generation of dermal collagen, and can effectively inhibit the generation of epidermal melanin, so the mask has the effects of skin care, skin tendering, wrinkle resistance and skin tolerance which are obviously superior to that of the retinoic acid, however, retinal is poorly soluble in water and easily oxidized, thus limiting its use in cosmetics; the invention connects retinene on cyclodextrin metal organic framework material through acetal structure, which improves the storage stability, and makes it release effectively in acid solution, and be absorbed and utilized by skin, solves the solubility problem, realizes controlled release, and improves the using effect of the facial mask. Finally, the rose essential oil is included in the cyclodextrin through the step D), when the facial mask is used, the modified cyclodextrin metal organic framework material is added into water, the inclusion effect of the cyclodextrin and the rose essential oil can be influenced by strong-polarity water molecules and other components in the facial mask, the rose essential oil is subjected to inclusion removal and is continuously released, the rose essential oil has a very good beautifying effect on dry skin, sensitive skin and aging skin, the skin water deficiency state can be improved, the skin can recover the water and luster, the activity of elastic fibers of the skin is enhanced, the skin immunity is enhanced, and the moistening effect of the facial mask is improved; the invention includes the rose essential oil in the cyclodextrin in the modified cyclodextrin metal organic framework material, can avoid the volatilization of the rose essential oil in the storage process, and simultaneously can also avoid the volatilization of the rose essential oil in the storage processThe influence on the oil control and cleaning performance of the facial mask caused by directly mixing the essential oil and the kaolin is avoided.
Preferably, the molar ratio of the gamma-cyclodextrin to the KOH in the reaction mother liquor in the step A) is 1: 8-8.5.
Preferably, the concentration of the gamma-cyclodextrin in the reaction mother liquor in the step A) is 30-35 mg/mL, and the volume ratio of the added methanol to the reaction mother liquor is 1: 8-12; the concentration of the added hexadecyl trimethyl ammonium bromide in the system is 7-9 mg/mL.
Preferably, the volume ratio of the glacial acetic acid to the ethanol in the glacial acetic acid ethanol solution in the step B) is 1: 10-20, and the mass volume ratio of the cyclodextrin metal-organic framework material to the glacial acetic acid ethanol solution is 1g: 10-20 mL.
Preferably, the stirring reaction time in the step B) is 1-3 h.
Preferably, the mass ratio of the neutralized cyclodextrin metal-organic framework material in the step C) to the retinene to the p-toluenesulfonic acid is 8-10: 1: 0.5-0.6.
Preferably, the volume ratio of the rose essential oil to the ethanol in the ethanol solution of the rose essential oil in the step D) is 1: 10-20; the mass-volume ratio of the retinal-modified cyclodextrin metal-organic framework material to the ethanol solution of the rose essential oil is 1g: 20-50 mL.
The invention also provides a preparation method of the cleaning mask powder, which comprises the following steps:
(1) drying and pulverizing Aloe and Lycium ruthenicum Murr respectively, and soaking in petroleum ether for defatting; filtering, washing, drying, adding the degreased powder into an ethanol solution, performing reflux extraction, extracting for 2-4 times, combining filtrates, concentrating under reduced pressure, and freeze-drying to obtain an aloe extract and a lycium ruthenicum extract;
(2) drying the rest raw materials, mixing with the aloe extract and the lycium ruthenicum extract, stirring uniformly, sterilizing and packaging to obtain the cleaning mask powder.
Preferably, the mass ratio of the aloe or the lycium ruthenicum mill to the petroleum ether during soaking and degreasing in the step (1) is 1: 8-10, and the soaking and degreasing time is 18-36 h; the mass concentration of the ethanol solution is 60-70% during reflux extraction, the mass ratio of the degreased powder to the ethanol solution is 1: 6-8, the reflux extraction temperature is 45-50 ℃, and the extraction time is 1-3 h.
Therefore, the invention has the following beneficial effects:
(1) the modified cyclodextrin metal organic framework material is added as an adsorption material, and the porous structure and the large specific surface area of the adsorption material can enable the mask to have good oil control and cleaning effects; the rose essential oil is included in the cyclodextrin metal organic framework material and is connected with the retinal through an acetal structure, so that the storage stability of the rose essential oil and the retinal is improved, and meanwhile, the rose essential oil and the retinal are released in the using process of the mask, so that the mask also has the effects of moistening and moisturizing, refining pores, smoothing skin, whitening and resisting wrinkles, and the using performance of the cleaning mask is improved;
(2) the lycium ruthenicum extract is added into the mask powder, and the lycium ruthenicum extract is rich in anthocyanin and procyanidine, has strong free radical scavenging and oxidation resisting performances, and improves the anti-wrinkle and anti-aging effects of the mask.
Detailed Description
The invention is further described with reference to specific embodiments.
In the present invention, all the equipment and materials are commercially available or commonly used in the art, and the methods in the following examples are conventional in the art unless otherwise specified.
Example 1:
a moistening and astringing type deep cleaning mask powder comprises the following raw materials in parts by weight: 25 parts of modified cyclodextrin metal organic framework material, 12 parts of kaolin, 3 parts of trehalose, 4 parts of sodium hyaluronate, 4 parts of sorbitol powder, 3 parts of aloe extract, 3 parts of lycium ruthenicum extract and 0.6 part of citric acid.
The preparation method of the modified cyclodextrin metal-organic framework material comprises the following steps:
A) dissolving gamma-cyclodextrin and KOH with the molar ratio of 1:8.1 in water to prepare reaction mother liquor with the concentration of the gamma-cyclodextrin being 32 mg/mL; adding methanol into the reaction mother liquor in a volume ratio of 1:10, oscillating, mixing uniformly, heating to 55 ℃, and stirring for reaction for 5.5 hours; cooling to room temperature, adding hexadecyl trimethyl ammonium bromide to enable the concentration of the hexadecyl trimethyl ammonium bromide in the system to be 8mg/mL, stirring and mixing uniformly, standing for 4 hours, and separating, washing and drying the product to obtain the cyclodextrin metal organic framework material;
B) adding the cyclodextrin metal organic framework material into a glacial acetic acid ethanol solution with the volume ratio of glacial acetic acid to ethanol being 1:15, wherein the mass volume ratio of the cyclodextrin metal organic framework material to the glacial acetic acid ethanol solution is 1g:15mL, stirring for reacting for 2h, and separating, washing and drying a product to obtain a neutralized cyclodextrin metal organic framework material;
C) dispersing a neutralized cyclodextrin metal organic framework material in ethanol, wherein the mass volume ratio of the neutralized cyclodextrin metal organic framework material to the ethanol is 1g:20mL, then adding retinene and p-toluenesulfonic acid, wherein the mass ratio of the neutralized cyclodextrin metal organic framework material to the retinene to the p-toluenesulfonic acid is 9:1:0.55, stirring uniformly, heating to 65 ℃, reacting for 20h, separating and drying a product to obtain a retinene modified cyclodextrin metal organic framework material;
D) adding the retinene modified cyclodextrin metal-organic framework material into an ethanol solution of rose essential oil with the volume ratio of the rose essential oil to the ethanol of 1:15, wherein the mass volume ratio of the retinene modified cyclodextrin metal-organic framework material to the ethanol solution of the rose essential oil is 1g:30mL, stirring and reacting for 4h, separating the product, washing with ethanol, and freeze-drying to obtain the modified cyclodextrin metal-organic framework material.
The preparation method of the cleaning mask powder comprises the following steps:
(1) drying and crushing aloe and lycium ruthenicum, and then adding into petroleum ether for soaking and degreasing for 24 hours, wherein the mass ratio of the aloe or lycium ruthenicum to the petroleum ether is 1: 9; filtering, washing, drying, extracting the defatted powder with 65 wt% ethanol solution at 47 deg.C under reflux for 2 hr, filtering, extracting the residue with the same method again, extracting for 3 times, mixing filtrates, concentrating under reduced pressure, and freeze drying to obtain Aloe extract and Lycium ruthenicum Murr extract;
(2) drying the rest raw materials, mixing with Aloe extract and Lycium ruthenicum Murr extract at a certain proportion, stirring, performing ultraviolet sterilization, placing the sterilized cleaning facial mask powder in PVC packaging bag, sealing, and storing.
Example 2:
a moistening and astringing type deep cleaning mask powder comprises the following raw materials in parts by weight: 20 parts of modified cyclodextrin metal organic framework material, 15 parts of kaolin, 5 parts of trehalose, 3 parts of sodium hyaluronate, 5 parts of sorbitol powder, 1 part of aloe extract, 5 parts of lycium ruthenicum extract and 0.5 part of citric acid.
The preparation method of the modified cyclodextrin metal-organic framework material comprises the following steps:
A) dissolving gamma-cyclodextrin and KOH with the molar ratio of 1:8 in water to prepare reaction mother liquor with the concentration of the gamma-cyclodextrin being 30 mg/mL; adding methanol with the volume ratio of 1:8 to the reaction mother liquor, oscillating, mixing uniformly, heating to 50 ℃, and stirring for reaction for 6 hours; cooling to room temperature, adding hexadecyl trimethyl ammonium bromide to enable the concentration of the hexadecyl trimethyl ammonium bromide in the system to be 7mg/mL, stirring and mixing uniformly, standing for 3h, and separating, washing and drying the product to obtain the cyclodextrin metal organic framework material;
B) adding the cyclodextrin metal organic framework material into a glacial acetic acid ethanol solution with the volume ratio of glacial acetic acid to ethanol being 1:10, wherein the mass volume ratio of the cyclodextrin metal organic framework material to the glacial acetic acid ethanol solution is 1g:20mL, stirring for reacting for 1h, and separating, washing and drying a product to obtain a neutralized cyclodextrin metal organic framework material;
C) dispersing a neutralized cyclodextrin metal organic framework material in ethanol, wherein the mass volume ratio of the neutralized cyclodextrin metal organic framework material to the ethanol is 1g:20mL, then adding retinene and p-toluenesulfonic acid, wherein the mass ratio of the neutralized cyclodextrin metal organic framework material to the retinene to the p-toluenesulfonic acid is 8:1:0.5, stirring uniformly, heating to 60 ℃, reacting for 24h, separating and drying a product to obtain a retinene modified cyclodextrin metal organic framework material;
D) adding the retinene modified cyclodextrin metal-organic framework material into an ethanol solution of rose essential oil with the volume ratio of the rose essential oil to the ethanol of 1:10, wherein the mass volume ratio of the retinene modified cyclodextrin metal-organic framework material to the ethanol solution of the rose essential oil is 1g:50mL, stirring and reacting for 3h, separating the product, washing with ethanol, and freeze-drying to obtain the modified cyclodextrin metal-organic framework material.
The preparation method of the cleaning mask powder comprises the following steps:
(1) drying and crushing aloe and lycium ruthenicum, and then adding into petroleum ether for soaking and degreasing for 18h, wherein the mass ratio of the aloe or the lycium ruthenicum to the petroleum ether is 1: 10; filtering, washing, drying, extracting the defatted powder with 60 wt% ethanol solution at 45 deg.C under reflux for 3 hr, filtering, extracting the residue with the same method again, extracting for 2 times, mixing filtrates, concentrating under reduced pressure, and freeze drying to obtain Aloe extract and Lycium ruthenicum Murr extract;
(2) drying the rest raw materials, mixing with Aloe extract and Lycium ruthenicum Murr extract at a certain proportion, stirring, performing ultraviolet sterilization, placing the sterilized cleaning facial mask powder in PVC packaging bag, sealing, and storing.
Example 3:
a moistening and astringing type deep cleaning mask powder comprises the following raw materials in parts by weight: 30 parts of modified cyclodextrin metal organic framework material, 10 parts of kaolin, 1 part of trehalose, 5 parts of sodium hyaluronate, 3 parts of sorbitol powder, 5 parts of aloe extract, 1 part of lycium ruthenicum extract and 1 part of citric acid.
The preparation method of the modified cyclodextrin metal-organic framework material comprises the following steps:
A) dissolving gamma-cyclodextrin and KOH with the molar ratio of 1:8.5 in water to prepare reaction mother liquor with the concentration of the gamma-cyclodextrin being 35 mg/mL; adding methanol with the volume ratio of 1:12 to the reaction mother liquor, oscillating, mixing uniformly, heating to 60 ℃, and stirring for reaction for 5 hours; cooling to room temperature, adding hexadecyl trimethyl ammonium bromide to enable the concentration of the hexadecyl trimethyl ammonium bromide in the system to be 9mg/mL, stirring and mixing uniformly, standing for 5 hours, and separating, washing and drying the product to obtain the cyclodextrin metal organic framework material;
B) adding the cyclodextrin metal organic framework material into a glacial acetic acid ethanol solution with the volume ratio of glacial acetic acid to ethanol being 1:20, wherein the mass volume ratio of the cyclodextrin metal organic framework material to the glacial acetic acid ethanol solution is 1g:10mL, stirring for reacting for 3h, and separating, washing and drying a product to obtain a neutralized cyclodextrin metal organic framework material;
C) dispersing a neutralized cyclodextrin metal organic framework material in ethanol, wherein the mass volume ratio of the neutralized cyclodextrin metal organic framework material to the ethanol is 1g:20mL, then adding retinene and p-toluenesulfonic acid, wherein the mass ratio of the neutralized cyclodextrin metal organic framework material to the retinene to the p-toluenesulfonic acid is 10:1:0.6, stirring uniformly, heating to 70 ℃, reacting for 18h, and separating and drying a product to obtain a retinene modified cyclodextrin metal organic framework material;
D) adding the retinene modified cyclodextrin metal-organic framework material into an ethanol solution of rose essential oil with the volume ratio of the rose essential oil to the ethanol of 1:20, wherein the mass volume ratio of the retinene modified cyclodextrin metal-organic framework material to the ethanol solution of the rose essential oil is 1g:20mL, stirring and reacting for 5h, separating the product, washing with ethanol, and freeze-drying to obtain the modified cyclodextrin metal-organic framework material.
The preparation method of the cleaning mask powder comprises the following steps:
(1) drying and crushing aloe and lycium ruthenicum, and then adding into petroleum ether for soaking and degreasing for 36 hours, wherein the mass ratio of the aloe or lycium ruthenicum to the petroleum ether is 1: 8; filtering, washing, drying, extracting the defatted powder with 70 wt% ethanol solution at 50 deg.C under reflux for 1 hr, filtering, extracting the residue with the same method again, extracting for 4 times, mixing filtrates, concentrating under reduced pressure, and freeze drying to obtain Aloe extract and Lycium ruthenicum Murr extract;
(2) drying the rest raw materials, mixing with Aloe extract and Lycium ruthenicum Murr extract at a certain proportion, stirring, performing ultraviolet sterilization, placing the sterilized cleaning facial mask powder in PVC packaging bag, sealing, and storing.
Comparative example 1 (without addition of modified cyclodextrin metal organic framework material):
a moistening and astringing type deep cleaning mask powder comprises the following raw materials in parts by weight: 37 parts of kaolin, 3 parts of trehalose, 4 parts of sodium hyaluronate, 4 parts of sorbitol powder, 3 parts of aloe extract, 3 parts of lycium ruthenicum extract and 0.6 part of citric acid. The preparation method is the same as in example 1.
Comparative example 2 (no retinaldehyde attached to modified cyclodextrin metal organic framework material):
the preparation method of the modified cyclodextrin metal-organic framework material in the comparative example 2 comprises the following steps:
A) dissolving gamma-cyclodextrin and KOH with the molar ratio of 1:8.1 in water to prepare reaction mother liquor with the concentration of the gamma-cyclodextrin being 32 mg/mL; adding methanol into the reaction mother liquor in a volume ratio of 1:10, oscillating, mixing uniformly, heating to 55 ℃, and stirring for reaction for 5.5 hours; cooling to room temperature, adding hexadecyl trimethyl ammonium bromide to enable the concentration of the hexadecyl trimethyl ammonium bromide in the system to be 8mg/mL, stirring and mixing uniformly, standing for 4 hours, and separating, washing and drying the product to obtain the cyclodextrin metal organic framework material;
B) adding the cyclodextrin metal organic framework material into a glacial acetic acid ethanol solution with the volume ratio of glacial acetic acid to ethanol being 1:15, wherein the mass volume ratio of the cyclodextrin metal organic framework material to the glacial acetic acid ethanol solution is 1g:15mL, stirring for reacting for 2h, and separating, washing and drying a product to obtain a neutralized cyclodextrin metal organic framework material;
C) adding the neutralized cyclodextrin metal-organic framework material into an ethanol solution of the rose essential oil, wherein the volume ratio of the rose essential oil to the ethanol is 1:15, the mass volume ratio of the neutralized cyclodextrin metal-organic framework material to the ethanol solution of the rose essential oil is 1g:30mL, stirring for reacting for 4h, separating a product, washing with ethanol, and freeze-drying to obtain the modified cyclodextrin metal-organic framework material.
The rest is the same as in example 1.
Comparative example 3 (modified cyclodextrin metal organic framework material does not include rose essential oil):
the preparation method of the modified cyclodextrin metal-organic framework material in the comparative example 3 comprises the following steps:
A) dissolving gamma-cyclodextrin and KOH with the molar ratio of 1:8.1 in water to prepare reaction mother liquor with the concentration of the gamma-cyclodextrin being 32 mg/mL; adding methanol into the reaction mother liquor in a volume ratio of 1:10, oscillating, mixing uniformly, heating to 55 ℃, and stirring for reaction for 5.5 hours; cooling to room temperature, adding hexadecyl trimethyl ammonium bromide to enable the concentration of the hexadecyl trimethyl ammonium bromide in the system to be 8mg/mL, stirring and mixing uniformly, standing for 4 hours, and separating, washing and drying the product to obtain the cyclodextrin metal organic framework material;
B) adding the cyclodextrin metal organic framework material into a glacial acetic acid ethanol solution with the volume ratio of glacial acetic acid to ethanol being 1:15, wherein the mass volume ratio of the cyclodextrin metal organic framework material to the glacial acetic acid ethanol solution is 1g:15mL, stirring for reacting for 2h, and separating, washing and drying a product to obtain a neutralized cyclodextrin metal organic framework material;
C) dispersing the neutralized cyclodextrin metal organic framework material in ethanol, wherein the mass volume ratio of the neutralized cyclodextrin metal organic framework material to the ethanol is 1g:20mL, then adding retinene and p-toluenesulfonic acid, wherein the mass ratio of the neutralized cyclodextrin metal organic framework material to the retinene to the p-toluenesulfonic acid is 9:1:0.55, stirring uniformly, heating to 65 ℃, reacting for 20h, separating a product, washing with ethanol, and drying to obtain the modified cyclodextrin metal organic framework material.
The rest is the same as in example 1.
Comparative example 4 (retinal is not attached via an acetal linkage):
the preparation method of the modified cyclodextrin metal-organic framework material in the comparative example 4 comprises the following steps:
A) dissolving gamma-cyclodextrin and KOH with the molar ratio of 1:8.1 in water to prepare reaction mother liquor with the concentration of the gamma-cyclodextrin being 32 mg/mL; adding methanol into the reaction mother liquor in a volume ratio of 1:10, oscillating, mixing uniformly, heating to 55 ℃, and stirring for reaction for 5.5 hours; cooling to room temperature, adding hexadecyl trimethyl ammonium bromide to enable the concentration of the hexadecyl trimethyl ammonium bromide in the system to be 8mg/mL, stirring and mixing uniformly, standing for 4 hours, and separating, washing and drying the product to obtain the cyclodextrin metal organic framework material;
B) adding the cyclodextrin metal organic framework material into a glacial acetic acid ethanol solution with the volume ratio of glacial acetic acid to ethanol being 1:15, wherein the mass volume ratio of the cyclodextrin metal organic framework material to the glacial acetic acid ethanol solution is 1g:15mL, stirring for reacting for 2h, and separating, washing and drying a product to obtain a neutralized cyclodextrin metal organic framework material;
C) dispersing the neutralized cyclodextrin metal organic framework material in an ethanol solution of retinene, wherein the mass-volume ratio of the neutralized cyclodextrin metal organic framework material to the retinene to the ethanol is 9g:1g:180mL, uniformly dispersing, stirring for reaction for 20h, and separating and drying a product to obtain the retinene modified cyclodextrin metal organic framework material;
D) adding the retinene modified cyclodextrin metal-organic framework material into an ethanol solution of rose essential oil with the volume ratio of the rose essential oil to the ethanol of 1:15, wherein the mass volume ratio of the retinene modified cyclodextrin metal-organic framework material to the ethanol solution of the rose essential oil is 1g:30mL, stirring and reacting for 4h, separating the product, washing with ethanol, and freeze-drying to obtain the modified cyclodextrin metal-organic framework material.
The rest is the same as in example 1.
Comparative example 5 (rose essential oil and retinal added directly):
a moistening and astringing type deep cleaning mask powder comprises the following raw materials in parts by weight: 25 parts of modified cyclodextrin metal organic framework material, 12 parts of kaolin, 3 parts of trehalose, 4 parts of sodium hyaluronate, 4 parts of sorbitol powder, 3 parts of aloe extract, 3 parts of lycium ruthenicum extract, 0.6 part of citric acid, 5 parts of rose essential oil and 3 parts of retinal.
The preparation method of the modified cyclodextrin metal-organic framework material comprises the following steps:
A) dissolving gamma-cyclodextrin and KOH with the molar ratio of 1:8.1 in water to prepare reaction mother liquor with the concentration of the gamma-cyclodextrin being 32 mg/mL; adding methanol into the reaction mother liquor in a volume ratio of 1:10, oscillating, mixing uniformly, heating to 55 ℃, and stirring for reaction for 5.5 hours; cooling to room temperature, adding hexadecyl trimethyl ammonium bromide to enable the concentration of the hexadecyl trimethyl ammonium bromide in the system to be 8mg/mL, stirring and mixing uniformly, standing for 4 hours, and separating, washing and drying the product to obtain the cyclodextrin metal organic framework material;
B) adding the cyclodextrin metal organic framework material into a glacial acetic acid ethanol solution with the volume ratio of glacial acetic acid to ethanol being 1:15, wherein the mass volume ratio of the cyclodextrin metal organic framework material to the glacial acetic acid ethanol solution is 1g:15mL, stirring for reacting for 2h, and separating, washing and drying a product to obtain the modified cyclodextrin metal organic framework material.
The preparation method of the cleaning mask powder comprises the following steps:
(1) drying and crushing aloe and lycium ruthenicum, and then adding into petroleum ether for soaking and degreasing for 24 hours, wherein the mass ratio of the aloe or lycium ruthenicum to the petroleum ether is 1: 9; filtering, washing, drying, extracting the defatted powder with 65 wt% ethanol solution at 47 deg.C under reflux for 2 hr, filtering, extracting the residue with the same method again, extracting for 3 times, mixing filtrates, concentrating under reduced pressure, and freeze drying to obtain Aloe extract and Lycium ruthenicum Murr extract;
(2) drying the other raw materials except for the rose essential oil, mixing the dried raw materials with the aloe extract and the lycium ruthenicum extract in proportion, uniformly stirring, spraying the rose essential oil into the powder, performing ultraviolet sterilization, placing the cleaning mask powder into a PVC packaging bag, and sealing for storage.
The storage stability and release property of retinal and rose essential oil in the facial mask powders prepared in the above examples and comparative examples were measured, and the results are shown in table 1. The test method comprises the following steps: placing the PVC packaging bag containing the cleaning facial mask powder in a constant temperature oven at 37 deg.C for 6 months, taking 1g sample every 2 months, dissolving with 15mL mixed solvent of water and ethanol (volume ratio 7:3) for 20min, and measuring the content of retinene and citronellol (main volatile component in rose essential oil) in the solution by high performance liquid chromatography.
Table 1: results of the storage stability and release of retinal and rose essential oils.
The respective use properties of the mask powders prepared in the above examples and comparative examples were tested, and the results are shown in table 2. The evaluation method of each performance comprises the following steps: selecting 120 subjects with large pores in the T area, dividing the subjects into 6 groups of 20 subjects, using the cleaning facial mask powder in the embodiment 1 and the comparative examples 1-5 respectively for each group, using the cleaning facial mask powder once a week, and continuously using the cleaning facial mask powder for three months; the use method of the cleaning mask powder comprises the following steps: mixing the mask powder with water according to the mass ratio of 1:5, stirring into uniform paste, smearing the paste on the face after face cleaning, smearing the paste with the thickness of 2-3 mm, and washing with clear water after 20 min.
The pore refining effect evaluation method comprises the following steps: the average area of the skin pores on the face of the subject was measured using a VisioFace facial image analyzer before use and after the three month test period was completed, respectively, and the shrinkage of the facial pores was calculated from the ratio of the area after use to the area before use, and the average was taken.
The evaluation method of the acne removing effect comprises the following steps: and (3) testing the number of facial acnes of the subject by using a VisioFace facial image analyzer before use and after the three-month test period is finished, calculating the reduction rate of the acnes, and taking an average value.
The rest performances are the average value of the scoring results of the subjects, each full performance score is 10, and the higher the score is, the better the corresponding performance is.
Table 2: and (5) testing the service performance of the combined product.
| Item | Example 1 | Comparative example 1 | Comparative example 2 | Comparative example 3 | Comparative example 4 | Comparative example 5 |
| Pox reduction (%) | 72.3 | 26.7 | 61.6 | 69.2 | 63.7 | 56.8 |
| Pore shrinkage (%) | 23.2 | 8.5 | 14.3 | 18.5 | 15.0 | 13.8 |
| Oil control effect (minute) | 8.9 | 7.7 | 8.7 | 8.5 | 8.8 | 7.9 |
| Moistening property (fen) | 8.5 | 5.5 | 8.0 | 6.1 | 8.2 | 6.7 |
| Cleaning power (score)) | 9.1 | 9.3 | 8.8 | 9.0 | 8.6 | 8.5 |
As can be seen from tables 1 and 2, the concentrations of retinene and rose essential oil of the cleaning facial mask powder prepared by the raw materials and the method in the invention in the examples 1-3 are not obviously reduced after 6 months of storage, and the storage stability is good; and has good moistening, oil controlling and cleaning abilities, and good effects of removing acnes and shrinking pores.
In the comparative example 1, the modified cyclodextrin metal organic framework material is not added into the mask powder, and only kaolin is used as an adsorbent, so that the oil control and the moisturizing performance of the mask are remarkably reduced, and the effects of removing acnes and shrinking pores are also remarkably reduced, possibly because retinaldehyde and rose essential oil components are absent in the mask when the modified cyclodextrin metal organic framework material is not added, the moisturizing performance of the mask is reduced due to the absence of the rose essential oil, and the skin is easy to pull dry and tighten after use, so that the water and oil imbalance of the skin is caused, the secretion of oil and fat is accelerated, and the oil control effect is further reduced; the lack of retinene can reduce the capability of the mask for astringing pores, and the imbalance of water and oil can cause excessive secreted oil to be accumulated in the pores, so that the pores cannot be closed and the acne is easy to grow.
In comparative example 2, no retinal was attached to the modified cyclodextrin metal organic framework material, and the anti-acne and pore-astringing effects of the mask were reduced; in the comparative example 3, the rose essential oil is not added into the modified cyclodextrin metal organic framework material, so that the moistening performance of the mask is reduced, and the acne removing and pore astringing effects are reduced.
In comparative example 4, the retinal is not connected to the cyclodextrin metal organic framework material through an acetal reaction, but is directly loaded on the surface of the cyclodextrin metal organic framework material through an adsorption method, and the release of the retinal cannot be effectively controlled; as can be seen from table 1, the amount of retinal released was small after the facial mask powder was dissolved in water for 20 minutes, and thus the pore astringency and the acne removing effect of the facial mask were significantly reduced as compared to those of example 1.
In comparative example 5, the rose essential oil and the retinal are directly blended with other components in other mask powder without being modified on the cyclodextrin metal organic framework material, so that the retinal and the rose essential oil are more oxidized and volatilized during the storage process, and the storage stability is poor; therefore, the moistening performance and the acne removing and pore astringing effects of the mask are reduced; furthermore, since retinal has poor solubility in water, retinal that is not oxidized when the retinal is directly blended is not easily dissolved and absorbed by the skin, and the acne removing and pore astringing effects of the mask are also reduced.
Claims (9)
1. The moistening and astringing type deep cleaning mask powder is characterized by comprising the following raw materials in parts by weight: 20-30 parts of a modified cyclodextrin metal organic framework material, 10-15 parts of kaolin, 1-5 parts of trehalose, 3-5 parts of sodium hyaluronate, 3-5 parts of sorbitol powder, 1-5 parts of aloe extract, 1-5 parts of lycium ruthenicum extract and 0.5-1 part of citric acid;
the preparation method of the modified cyclodextrin metal-organic framework material comprises the following steps:
A) dissolving gamma-cyclodextrin and KOH in water to prepare reaction mother liquor, adding methanol into the reaction mother liquor, uniformly mixing, heating to 50-60 ℃, and stirring for reacting for 5-6 hours; cooling to room temperature, adding hexadecyl trimethyl ammonium bromide, uniformly mixing, standing for 3-5 h, and separating, washing and drying a product to obtain the cyclodextrin metal organic framework material;
B) adding the cyclodextrin metal organic framework material into an ethanol solution of glacial acetic acid, stirring for reaction, separating, washing and drying a product to obtain a neutralized cyclodextrin metal organic framework material;
C) dispersing the neutralized cyclodextrin metal organic framework material in ethanol, adding retinene and p-toluenesulfonic acid, uniformly stirring, reacting at 60-70 ℃ for 18-24 h, separating and drying a product to obtain a retinene modified cyclodextrin metal organic framework material;
D) adding the retinal-modified cyclodextrin metal-organic framework material into an ethanol solution of rose essential oil, stirring and reacting for 3-5 h, and separating, washing and freeze-drying a product to obtain the modified cyclodextrin metal-organic framework material.
2. The moisturizing and astringent deep cleansing facial mask powder according to claim 1, wherein the molar ratio of the gamma-cyclodextrin to the KOH in the reaction mother solution in the step A) is 1: 8-8.5.
3. The moistening and astringing type deep cleaning mask powder as claimed in claim 1 or 2, wherein the concentration of the gamma-cyclodextrin in the reaction mother liquor in the step A) is 30-35 mg/mL, and the volume ratio of the added methanol to the reaction mother liquor is 1: 8-12; the concentration of the added hexadecyl trimethyl ammonium bromide in the system is 7-9 mg/mL.
4. The moistening and astringing deep cleaning facial mask powder as claimed in claim 1, wherein the volume ratio of the glacial acetic acid to the ethanol in the glacial acetic acid solution in the step B) is 1: 10-20, and the mass volume ratio of the cyclodextrin metal organic framework material to the ethanol solution of the glacial acetic acid is 1g: 10-20 mL.
5. The moisturizing and astringent deep cleansing facial mask powder according to claim 1 or 4, wherein the stirring reaction time in the step B) is 1-3 h.
6. The moisturizing and astringent deep cleansing facial mask powder as claimed in claim 1, wherein the mass ratio of the neutralized cyclodextrin metal organic framework material, the retinal and the p-toluenesulfonic acid in step C) is 8-10: 1: 0.5-0.6.
7. The moisturizing and astringent deep cleansing mask powder as claimed in claim 1, wherein the volume ratio of the rose essential oil to the ethanol in the ethanol solution of the rose essential oil in the step D) is 1: 10-20; the mass-volume ratio of the retinal-modified cyclodextrin metal-organic framework material to the ethanol solution of the rose essential oil is 1g: 20-50 mL.
8. A method for preparing the cleansing facial mask powder according to any one of claims 1 to 7, which is characterized by comprising the following steps:
(1) drying and pulverizing Aloe and Lycium ruthenicum Murr respectively, and soaking in petroleum ether for defatting; filtering, washing, drying, adding the degreased powder into an ethanol solution, performing reflux extraction, extracting for 2-4 times, combining filtrates, concentrating under reduced pressure, and freeze-drying to obtain an aloe extract and a lycium ruthenicum extract;
(2) drying the rest raw materials, mixing with the aloe extract and the lycium ruthenicum extract, stirring uniformly, sterilizing and packaging to obtain the cleaning mask powder.
9. The preparation method of the cleansing facial mask powder according to claim 8, wherein the mass ratio of aloe or lycium ruthenicum mill to petroleum ether during soaking and degreasing in the step (1) is 1: 8-10, and the soaking and degreasing time is 18-36 h; the mass concentration of the ethanol solution is 60-70% during reflux extraction, the mass ratio of the degreased powder to the ethanol solution is 1: 6-8, the reflux extraction temperature is 45-50 ℃, and the extraction time is 1-3 h.
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