KR101765242B1 - Method for preparing hydrogel pack containing even porous silica particle for skin whitening and anti-wrinkle - Google Patents
Method for preparing hydrogel pack containing even porous silica particle for skin whitening and anti-wrinkle Download PDFInfo
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Abstract
(A) obtaining a silica suspension containing silica particles, a whitening agent and an anti-wrinkle agent having a particle size of 1000 to 2000 nm, which contains pores having a size of 7 to 10 nm, into a water to provide a whitening agent and a wrinkle- (b) recovering the whitening agent and the anti-wrinkle agent-supported silica particles from the suspension of step (a); (c) mixing the recovered silica particles and the water-soluble polymer with water, and then gelling the water-soluble polymer, wherein the silica particles and the water-soluble polymer are recovered in step (b) .
The silica particles having uniform pore sizes formed according to the present invention are uniformly sized to form pores so that the whitening agent and the wrinkle removing agent can be stably carried in the silica particles and the whitening agent and the wrinkle removing agent are continuously discharged And can be effectively used in the manufacture of a pack.
Description
The present invention relates to a method for producing a whitening and wrinkle-improving hydrogel pack comprising silica particles having pores of uniform size.
A hydrogel is a hydrophilic polymer prepared by using water as a dispersion medium and capable of maintaining a three-dimensional shape without dissolving or dissociating in a sufficient amount of water.
The hydrogel has a structure very similar to an extra cellular matrix, which is a natural tissue of the human body, has excellent biocompatibility and viscoelastic properties, and has advantages such as superior permeation of oxygen and nutrients. Have been manufactured and used.
Conventional hydrogel packs mainly used water-soluble polymers and polyhydric alcohols as raw materials. However, when water-soluble polymers are dried on the skin, they form a thin film to give a feeling of skin to the skin, and polyhydric alcohols There is a tendency to take away moisture that is present in the skin rather than the skin.
In recent years, in order to solve the above problems, a hydrogel pack containing a lipid-soluble substance or an emulsion has been produced based on a water-soluble polymer, and in particular, a hydrogel pack having a stable and effective A method of producing a hydrogel using silica particles to form a bonding force has been disclosed.
For example, Patent Document 1 discloses a technical content of a cosmetic composition containing a mesoporous silica composite powder in which a chitosan-lipase aggregate is collected.
However, the silica particles disclosed in Document 1 have a disadvantage in that the size of the pores is not uniform and it is difficult to stably carry the active ingredient in the silica, and it is difficult to expect the continuous release effect of the active ingredient.
Therefore, there is a need for research on a method for producing a hydrogel pack containing silica having a uniform pore size.
The inventors of the present invention have been studying a hydrogel pack containing porous silica. When a hydrogel pack is prepared by using silica particles having pores of uniform size, a hydrogel pack having improved stability and moisturizing properties of the active ingredient I know I can do it.
Accordingly, it is an object of the present invention to provide a technical content of a method for producing a whitening and wrinkle-improving hydrogel pack containing silica particles having pores of uniform size.
In order to accomplish the above-mentioned object, the present invention provides a method for producing a silica gel, comprising the steps of: (a) adding silica particles, a whitening agent and a wrinkle reducing agent having a particle size of 1000 to 2000 nm including pores having a size of 7 to 10 nm, To obtain a suspended silica suspension; (b) recovering the whitening agent and the anti-wrinkle agent-supported silica particles from the suspension of step (a); (c) mixing silica particles and a water-soluble polymer recovered in step (b) with water to cause gelation; and (d) to provide.
In one embodiment, the silica particle preparation of step (a) may be prepared in a drop fashion.
In one embodiment, the whitening agent of step (a) is selected from the group consisting of mulberry extract, oil soluble licorice extract, bilberry extract, bark extract, arbutin, ethyl ascorbyl ether, ascorbyl glucoside, niacinamide, alpha-bisabolol, At least one member selected from the group consisting of isopropyl palmitate, isopropyl palmitate, isopropyl palmitate, isobutyric acid, isobutyric acid, isobutyric acid, isobutyric acid, isobutyric acid, isobutyric acid, isobutyric acid, isobutyric acid, The anti-wrinkle agent may be at least one selected from the group consisting of retinyl palmitate, retinol, adenosine, acetyl hexapeptide, human oligopeptide, dibenzoylmethane, benzotriazole derivative, ginseng extract, .
In one embodiment, the suspension of step (a) is selected from the group consisting of sodium lactate, hyaluronic acid, trehalose, ceramide, allantoin, lactitol, inositol, hydroxyproline, glucamine, glucuronolactone, stearyl behenate, At least one moisturizing agent selected from the group consisting of aloe vera extract, aloe vera extract, pinose, menthyl phosaccharide, mineral salt, mung bean, seaweed extract, Boi tea extract, kidney bean extract and chaga mushroom extract.
In one embodiment, the water soluble polymer of step (b) may be at least one selected from the group consisting of carrageenan, xanthan gum, carboplatin gum, guar gum and agar.
In one embodiment, the silica particles of step (c) may be included in an amount of 10 to 20% by weight based on the total weight of the hydrogel.
According to one aspect of the present invention, there is provided a hydrogel pack prepared by the above-described method.
In one embodiment, the hydrogel pack may be a mask pack, an eye patch, a nail patch, a lip patch, a body patch, an elbow patch, or a partial patch applied to a particular site.
The silica particles having uniform pore sizes formed according to the present invention are uniformly sized to form pores so that the whitening agent and the wrinkle removing agent can be stably carried in the silica particles and the whitening agent and the wrinkle removing agent are continuously discharged And can be effectively used in the manufacture of a pack.
In addition, the prepared whitening and wrinkle improving hydrogel packs can be more effectively used as a mask pack for skin improvement, because the filling ratio and moisturizing property of the hydrogel mask packs are improved compared to the hydrogel mask packs prepared using only conventional water-soluble polymer components.
Fig. 1 is a process diagram showing each step of the method for producing a hydrogel pack according to the present invention.
2 is a graph showing moisture evaporation amount of the hydrogel pack.
3 is a photograph of (a) the hydrogel according to Example 1 and (b) the hydrogel according to Comparative Example 1. Fig.
As shown in FIG. 1, the method for producing a whitening and wrinkle-improving hydrogel pack containing silica having pores of uniform size according to the present invention comprises: (a) Silica particles having a size of 1000 to 2000 nm, a whitening agent and a wrinkle-reducing agent in water to obtain a silica suspension having a whitening agent and a wrinkle-reducing agent carried thereon; (b) recovering the whitening agent and the anti-wrinkle agent-supported silica particles from the suspension of step (a); (c) mixing the recovered silica particles and the water-soluble polymer with water, and then gelling the water-soluble polymer; and (c) .
(A) silica particles having a particle size of 1000 to 2000 nm including pores having a size of 7 to 10 nm; The silica particles, the whitening agent and the wrinkle-reducing agent are put into water to obtain a silica suspension carrying a whitening agent and a wrinkle-reducing agent.
In this step, the silica particles containing pores having a size of 7 to 10 nm as described above can be prepared by various known methods, and preferably silica particles are added to a mixed solution containing a surfactant, water and an acid, The precursor may be dropwise subjected to droplet dripping to form silica particles having pores of uniform size.
More specifically, in order to produce silica particles having pores of uniform size, a silica precursor is dropwise added to a mixed solution in which a surfactant is mixed with water and an acid is added thereto, and then aged to form pores having a uniform size Silica particles can be produced.
The surfactant reacts with the silica precursor to form pores and is configured to control the amount of the surfactant to a concentration higher than the critical micelle concentration required for forming micelles in the aqueous solution state, As shown in FIG.
The surfactant is preferably a polyblock copolymer, and Pluronic P123 is a representative example.
The acid serves as a catalyst for forming silica pores having uniform pores and can be configured to control the addition amount of the acid according to the amount of the surfactant to be added.
The pH of the mixed solution may be maintained in the range of 1.0 to 2.0 in order to serve as a catalyst by the acid. To this end, a strong acid such as hydrochloric acid may be added.
The mixed solution containing the surfactant, acid, and water may be configured to be stirred for a sufficient time to allow the micelles to be homogeneously formed. For example, the micelles may be stirred at 40 ° C for at least 8 hours, To prepare a mixed solution.
In addition, the mixed solution may be further added with other catalyst components, such as ammonium fluoride (NH 4 F), to uniformly form pores in the silica particles to be produced.
In addition, the pore-expanding agent may be added to the mixed solution so that the pore size of the silica particles to be produced may be increased. Preferably, the pore-expanding agent may be added before the addition of the silica precursor.
In this step, various silica precursors known as silica precursors can be used. Preferably, tetra-ethyl-ortho-silicate (TEOS) can be used.
The TEOS is dissolved in the hydrophobic portion of the micelle formed by the surfactant to form hydrolysis and micropores. Since the TEOS is in a liquid state at room temperature, TEOS is dropped into the mixed solution by dropping, As shown in FIG.
When TEOS is added and stirred, it is preferable that the reaction is carried out by stirring at 40 DEG C for 8 hours or more.
As described above, the agitated silica solution can be aged at a high temperature. Since the silica solution is subjected to a hydrothermal synthesis reaction during aging, silica particles having a more uniform pore size can be produced Preferably overnight at 120 < 0 > C.
In this step, the aged silica solution is filtered, washed with water and dried at room temperature to obtain precipitated silica particles, and the impurities contained in the silica particles can be removed. The dried silica particles are calcined Silica particles having micropores of uniform size can be produced.
For this, it is preferable to dry at 25 to 30 ° C for 24 to 36 hours, and calcined at 550 ° C to produce silica particles.
The silica particles prepared according to the above method have pores of uniform size and high thermal stability, and can serve as a support capable of stably supporting the active ingredient.
Further, in this step, the silica particles, the whitening agent and the wrinkle remover prepared as described above are put into water to obtain a silica suspension carrying a whitening agent and a wrinkle remover.
In this step, the whitening agent is selected from the group consisting of mulberry extract, oil soluble licorice extract, bark extract, bark extract, arbutin, ethyl ascorbyl ether, ascorbyl glucoside, niacinamide, alpha-bisabolol, ascorbyl tetraisopalmitate, Phosphate, sodium ascorbyl phosphate, vitamin C, vitamin E, catechin, hydroquinone, kojic acid, berberine, succinic acid or a mixture thereof.
The mulberry extract has an effect of inhibiting the formation of melanin pigment on the skin and inhibiting the formation of spots and freckles, and thus can be included in the whitening agent. In order to achieve a whitening effect, the extract can be contained in an amount of preferably 2% Usability The licorice extract is involved in alleviating the skin hypersensitivity reaction, and has a skin moisturizing and whitening effect, and may preferably contain 0.05% or more.
In addition, arbutin inhibits the activity of tyrosinase in the melanin pigment production step, thereby inhibiting the production of excessive melanin pigment. The albutin may be included in the whitening agent, and is preferably contained in an amount of 2 to 5% can do.
The above-mentioned ethyl ascorbyl ether and ascorbyl tetraisopalmitate have the effect of inhibiting the oxidation of the tyrosine stimulated by the tyrosinase enzyme and can be included in the whitening agent. .
The above-mentioned ascorbyl glucoside promotes collagen synthesis, inhibits melanin synthesis, and can be contained in the active ingredient. In order to attain a whitening effect, the ascorbyl glucoside may preferably be contained in an amount of 2% or more. It inhibits the step of transferring melanin from melanocyte to keratocyte. It strengthens the skin barrier and is effective for maintaining skin health. It can be included in whitening agent, and it is preferably contained in 2 to 5% or more for whitening effect can do.
In addition, the alpha-bisabolol has the effect of alleviating skin irritation and preventing melanin pigment from depositing on the skin, and may be included in the whitening agent, and may be contained in an amount of preferably 0.5% or more for whitening effect.
In addition, in this step, the anti-wrinkle agents include retinyl palmitate, retinol, adenosine, acetyl hexapeptide, human oligopeptide, dibenzoylmethane, benzotriazole derivatives, ginseng extract, herring root extract, can do.
The retinyl palmitate and retinol prevent the oxidative damage of the skin, promote the synthesis of collagen and elastin to improve the wrinkles of the skin and improve the elasticity, and can be included in the wrinkle-improving agent. Preferably at least 2,500 IU / g, respectively.
In addition, adenosine may be included in the anti-wrinkle agent because it has the effect of enhancing the elasticity on the skin by progressing the aging process and improving the anti-wrinkle effect and the vitality to the skin, and is preferably 0.04% or more As shown in FIG.
Furthermore, the above-mentioned active ingredient can be used as a moisturizing agent which can be used as a cosmetic preparation, such as sodium lactate, hyaluronic acid, trehalose, ceramide, allantoin, lactitol, inositol, hydroxyproline, glucamine, glucuronolactone, stearyl behenate, Osseum, menthyl pinea, mineral salt, mung bean, seaweed extract, Boi tea extract, kidney bean extract and chaga mushroom extract.
The sodium lactate is a natural moisturizing ingredient. It exhibits a higher moisture-holding power than a polyhydric alcohol, has a property of fixing water and has an effect of maintaining skin moisturizing ability and can be included in an active ingredient. The hyaluronic acid is contained in the skin dermis layer It is effective for supplying moisture and attracting moisture from the outside to form a moisturizing film, which can be included in the moisturizing agent.
In addition, the trehalose has an effect of preventing water loss by binding itself with moisture and having a moisturizing function, and can be included in the active ingredient. The ceramide is a substance that constitutes the lipid layer of the skin, and a hydrophilic group and a lipophilic group It has the effect of preventing the moisture of the skin from evaporating and can be included in the moisturizing agent.
The allantoin improves the moisturizing function of the skin, calms the irritated skin, and can be included in the moisturizing agent without toxicity and irritation and exhibiting its effect even at a low concentration.
The above-described whitening agent and anti-wrinkle agent can be supported in the silica particle pores.
Preferably, the whitening agent and the wrinkle-reducing agent and the silica particles are immersed in water for 24 hours, and then dried at room temperature for 3 days to obtain a whitening agent and a wrinkle-removing agent It can be supported on silica particles.
The step (b) is a step of recovering the silica particles bearing the whitening agent and the anti-wrinkle agent from the suspension. In this step, only the silica particles carrying the whitening agent and the anti-wrinkle agent can be recovered by filtering the suspension.
The silica particles can be filtered by performing various known methods such as suction filtration or pressure filtration, and desirably, only silica particles can be collected by gravity filtration using a filter paper.
Step (c) is a step of mixing the silica particles and the water-soluble polymer recovered in step (b) with water and then gelling the mixture.
The water-soluble polymer may be prepared by adding carrageenan, xanthan gum, carnauba bean gum, guar gum and agar to prepare a hydrogel pack.
Carrageenan is a polysaccharide which has an antibacterial action and an immunity enhancing action and is effective as a gelling agent, a stabilizer for a medicine or a cosmetic, and has almost no viscosity change due to the above-mentioned xanthan gum black acid, alkali and salts etc. and has effects of filming, gelation and moisturizing And can be used for the production of hydrogels.
It can be used in hydrogels because it has the effect of imparting a black oil stabilizer, a water-soluble thickener and a fragrance, and the guar gum and agar have an effect of increasing viscosity, improving emulsion stability and improving physical properties and feel, ≪ / RTI >
In addition, in the present step, the hydrogel may include silica particles in an amount of 0.10 to 10% by weight based on the total weight of the hydrogel.
The silica particles contained in the hydrogel pack are preferably contained in an amount of 0.1 to 10% by weight, more preferably 0.1 to 5% by weight, and most preferably 0.1 to 0.8% by weight based on the total weight of the hydrogel, Gel can be produced.
As described above, the addition amount of the silica particles is limited because, when the silica particles are used in an amount of less than 0.1% by weight, it is difficult to expect the effect of the whitening agent and the wrinkle improving agent on the retention and moisturizing properties. And the silica particles may be added in such a composition range.
In addition, the hydrogel may further include an additive such as a surfactant, a preservative, and a pH adjuster to further improve the physical properties of the hydrogel.
In this step, an aqueous solution containing the silica particles and the water-soluble polymer may further include polyvinyl alcohol or a cross-linking agent for improving viscosity and improving physical properties.
The polyvinyl alcohol is effective as a binder, a film-forming agent, and a water-soluble thickener, and can be additionally included in the production of a hydrogel.
The crosslinking agent is capable of producing a chemically stable hydrogel having elasticity and can be additionally included in the production of hydrogel.
Examples of the cross-linking agent include acrylic cross-linked polymers, styrene-based copolymers, and mixtures thereof.
The hydrogel manufactured through the above method may be molded into a desired shape to produce a cosmetic mask pack or a partial patch, and the step of sealing to produce a final product.
As described above, according to the method for producing a whitening and wrinkle-improving hydrogel pack containing silica having pores of uniform size according to the present invention, it is possible to effectively produce silica particles having pores of uniform size, The silica particles having a uniform size can form a plurality of pores to stably carry the whitening agent and the wrinkle-reducing agent in the silica particles, and the whitening agent and the wrinkle-reducing agent can be continuously discharged, .
The present invention provides a hydrogel pack prepared by the above-described method.
The hydrogel pack may be a mask pack, an eye patch, a nail patch, a lip patch, a body patch, an elbow patch, or a partial patch applied to a specific site.
The hydrogel pack can be manufactured to be applied to the entire face or a specific area.
For example, a hydrogel patch can be manufactured with an eye patch applied around the eyes, or a nose pack applied around the nose.
The whitening and wrinkle-improving hydrogel pack according to the present invention contains silica particles uniformly formed with pores, and thus has a higher retention and moisturizing property than the hydrogel packs prepared using only conventional water-soluble polymer components, An excellent effect can be expected.
Hereinafter, the present invention will be described in more detail with reference to preferred embodiments. The embodiments presented are only a concrete example of the present invention and are not provided for the purpose of limiting the scope of the present invention.
Example 1. Preparation of hydrogel pack
The hydrogel pack according to the present invention was produced through the following steps.
4 g of surfactant P123, 120 g of 2 M HCl and 30 g of H 2 O were stirred at 40 ° C for 8 hours. 8.5 g of TEOS was dropwise added to the above solution, and the mixture was stirred at 8O < 0 > C for 8 hours. After aging at 120 ° C. overnight, the aged solution was filtered and dried at room temperature, calcined at 550 ° C. to obtain silica particles having a uniform pore size of 7 to 10 nm and a particle size of 1000 to 2000 nm .
The obtained silica particles were immersed in a solution containing 2% of niacinamide and 2% of adenosine for 24 hours, followed by filtration and drying at room temperature for 3 days to obtain silica particles impregnated with the active ingredient.
0.9 g of carrageenan, 0.7 g of xanthan gum, 0.814 g of carnauba gum, 0.07 g of guar gum, 0.07 g of agar, and 96.611 g of purified water were stirred at 60 캜. The homogenized solution was molded into a mold, cooled at room temperature, and aged for 13 hours to prepare a hydrogel pack as shown in Fig. 3 (a).
Example 2.
A hydrogel pack was prepared in the same manner as in Example 1, except that uniform pores having a size of 7 to 10 nm were formed and 0.5 g of silica particles having a particle size of 1000 to 2000 nm were contained.
Comparative Example 1
2 g of niacinamide, 2 g of adenosine, 0.935 g of carrageenan, 0.7 g of xanthan gum, 0.814 g of carob bean gum, 0.07 g of guar gum, 0.07 g of agar and 93.411 g of purified water were stirred at 60 캜. The homogenized solution was molded into a mold, cooled at room temperature, and aged for 13 hours to prepare a hydrogel pack as shown in Fig. 3 (b).
Comparative Example 2
A hydrogel pack was prepared in the same manner as in Example 1, except that silica particles (pore size < 2 nm) purchased from Grace were used.
Test Example 1. Analysis of water retention ability of the hydrogel pack
To analyze the water holding ability of the hydrogel pack according to Example 1, Comparative Example 1 and Comparative Example 2, the water evaporation amount over time was measured.
The prepared hydrogel pack was cut into a size of 45 x 10 x 1 mm and the initial weight of the specimen was measured. The specimens were dried in an oven at 45 ° C and weighed after 10 minutes, 30 minutes, 60 minutes, 150 minutes, and overnight.
The moisture evaporation amount of the hydrogel pack was calculated using the following formula 1, and the results are shown in Table 1 and FIG.
[Formula 1]
As shown in Table 1 and FIG. 2, the hydrogel pack according to the present invention had a smaller moisture evaporation amount over time than the hydrogel packs of Comparative Example 1 and Comparative Example 2, Can be confirmed.
Test Example 2. Analysis of Effluent Flow Rate of Hydrogel Pack
A dissolution test was carried out according to the paddle-over-disk method in order to examine the elution amount of the active ingredient of the hydrogel pack according to Example 1 and Comparative Example 1.
The prepared hydrogel packs were adhered to the disc assembly with the adhesive side facing the net side and the back side was coated with an adhesive tape to prevent release of the active ingredient and then subjected to a dissolution test according to the paddle test method Respectively. At this time, 500 mL of water was poured into the elution vessel of the elution apparatus, the test temperature was 32 ± 0.5 ° C, and the rotation speed of the paddle was 50 rpm.
Separate 1.2 mL of the eluate each at 5, 10, 15, 20, 25, and 30 minutes after elution began, and filter the solution beforehand. When the eluate is collected, add 1.2 mL To quantitate the eluted adenosine in the eluate, 20 μl of sample was taken from the sample solution, and the absorbance was measured at 235 nm and repeated twice. The results are shown in Table 2.
As shown in Table 2, it can be confirmed that the hydrogel pack according to the present invention provides and maintains a humid environment at the initial stage after application and gradually releases the active ingredient contained in the hydrogel pack.
Test Example 3. Analysis of whitening effect of hydrogel pack
In order to analyze the whitening effect of the hydrogel pack according to Example 1 and Comparative Example 1 of the present invention, the number of melanin in the base layer of the facial skin was measured.
The hydrogel prepared according to Example 1 and Comparative Example 1 was adhered to the face of the subject for 30 minutes each day and then removed to measure the number of melanins per 1 × 1 cm area of the skin.
The measurement was carried out for six weeks at intervals of one week using Mexameter MX-16. The measured values are shown in Table 3.
As shown in Table 3, it can be seen that the hydrogel pack according to the present invention contains silica particles having pores of uniform size impregnated with niacinamide, and thus the skin is effective in delivering and whitening the active ingredient.
Test Example 4. Analysis of wrinkle improvement effect of hydrogel pack
In order to analyze the effect of improving the wrinkles of the hydrogel pack according to Example 1 and Comparative Example 1 of the present invention, the wrinkles of the skin were measured before the use of the hydrogel, after 4 weeks of use and after 8 weeks of use.
The degree of wrinkles was measured by dividing the face into half of the subject's left eye and the right eye.
To measure the degree of wrinkles, subjects wash the measurement site with water, and then stabilize them in a waiting room at room temperature of 20 to 25 ° C and a humidity of 40 to 60% for 30 minutes to adjust skin surface temperature and humidity to the environment of the measurement space And water intake during rest was limited. For the objective measurement, one researcher measured it, and the same part was measured at each measurement.
The skin surface analysis was performed on the areas applied before, after and 4 weeks after use of the hydrogel pack according to Example 1 and Comparative Example 1 using a skin image analyzer, and the results are shown in Table 4 .
As shown in Table 4, the hydrogel pack according to the present invention includes silica particles having adenosine-impregnated uniform size pores formed therein, and the wrinkle value is decreased according to the period of use, and the skin delivery and wrinkle- Can be confirmed to be excellent.
Claims (8)
(b) recovering the whitening agent and the anti-wrinkle agent-supported silica particles from the suspension of step (a); And
(c) mixing the recovered silica particles and the water-soluble polymer in water with water, followed by gelation,
Wherein the silica particles of step (a) are prepared by dropwise dropping a silica precursor to a mixed solution comprising a surfactant, water and an acid and aging the mixture. A process for producing a hydrogel pack for whitening and wrinkle improvement comprising silica.
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