Hair growth cosmetics, cosmetic raw materials, cosmetics, and methods for manufacturing the same.
Patent Information
- Application Number
- JP2023556371
- Authority / Receiving Office
- JP · JP
- Patent Type
- Patents
- Current Assignee / Owner
- Priority Date
- 2021-10-26
- Filing Date
- 2022-10-20
- Publication Date
- 2026-09-04
- Estimated Expiration
- 2042-10-20
AI Technical Summary
【0029】 本発明によれば、以下のような優れた効果を有する育毛用化粧料を提供することができる。 (1)シモンコライト結晶が毛髪の伸長を促進するため、毛髪の健やかな成長が維持され、健康な毛髪が得られる。 (2)効果持続期間が長いため、使用頻度を少なくすることができる。 (3)有効成分であるシモンコライト結晶をナノ粒子とすることにより、シモンコライト結晶によるざらつき感や白色の肌残りが生じなくなるため、滑らかな使用感と使用後においても美容上好ましい外観を呈する。 (4)分散剤を配合することにより、シモンコライト結晶が凝集し難くなり、保存安定性が高まると共に容易に再分散可能となるため、取り扱いも容易である。
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Abstract
Description
[Technical Field]
[0001] This invention relates to cosmetic raw materials and cosmetics, and more particularly to cosmetic raw materials and cosmetics used for hair growth or scalp care. [Background technology]
[0002] Simoncholyte is a zinc chloride hydroxide hydrate composed of zinc, hydroxyl groups, and chlorine, and its chemical formula is Zn5(OH)8Cl2·(H2O). n Simoncolite is a compound represented by [formula]. It is a white crystalline powder insoluble in water and organic solvents, and is also called basic zinc chloride or zinc hydroxide chloride. Simoncolite, which is also a natural mineral, was announced as a new mineral in 1985 and named after Werner Simon and Kurt Kolle, who collected mineral samples of Simoncolite. To date, Simoncolite has been mainly used as a main component of tetrabasic zinc chloride (TBZC), an animal feed additive, and is considered a desirable nutritional supplement for animals.
[0003] In recent years, research and development have been progressing on new applications and industrial manufacturing methods for simoncolite. For example, Patent Document 1 reports a technology for using simoncolite as a treatment for skin wounds or skin irritation, and Patent Document 2 reports a method for manufacturing simoncolite that can be used as a pharmaceutical ingredient.
[0004] On the other hand, the efficacy of zinc-containing compounds has been reported in the field of hair care and scalp care. For example, Patent Document 3 reports that zinc salts such as zinc gluconate, zinc chloride, and zinc sulfate have trypsin inhibitory activity and are therefore useful in preventing or reducing hair loss. Patent Document 4 describes a hair growth composition containing scutellaria baicalensis extract, a hair nourishing and hair growth ingredient, along with zinc gluconate and bisethoxyglycol cyclohexanedicarboxylic acid, and states that zinc gluconate has the effect of giving hair firmness and body. Furthermore, Non-Patent Document 1 reports the results of a study on the effect of zinc pyrithione, a zinc complex compound, on hair density and hair thickness. [Prior art documents] [Patent Documents]
[0005] [Patent Document 1] Patent No. 6185215 [Patent Document 2] International Publication No. 2018 / 105738 [Patent Document 3] Special Publication No. 2016-540806 [Patent Document 4] Patent No. 6797673 [Non-patent literature]
[0006] [Non-Patent Document 1] RS Berger et al., “The effects of minoxidil, 1% pyrithione zinc and a combination of both on hair density: a randomized controlled trial”, British Journal of Dermatology, Vol. 149, No.2, 2003, p.354-362 [Overview of the project] [Problems that the invention aims to solve]
[0007] Zinc salts such as zinc gluconate, zinc chloride and zinc sulfate reported in Patent Documents 3 and 4 are substances with high solubility in water, which dissolve in water and rapidly generate zinc ions. These zinc ions exert the effects of preventing or reducing hair loss and imparting firmness and body to hair. As if to support this, Non-Patent Document 1 reports that although the effect of zinc pyrithione, which has extremely low solubility in water, on hair density and hair thickness was examined, zinc pyrithione was observed to have only less than half the effect of minoxidil, which is a positive control. Similar to zinc pyrithione, simonkolleite also elutes only a very small amount of zinc ions into water, so simonkolleite has not been expected to have the efficacy as reported in Patent Documents 3 and 4. Therefore, the use of simonkolleite for hair care and scalp care has not been studied so far, and its effectiveness was completely unknown.
[0008] On the other hand, the simonkolleite crystals used in the aforementioned Patent Document 1 and produced by the production method introduced in Patent Document 2, as well as other generally commercially available simonkolleite crystals, have a primary particle diameter of about 10 μm (D 50 : median diameter), which is large, and it was also found that the crystals have aggregability. When the inventors of the present application dispersed these simonkolleite crystals in a dispersion medium such as water or ethanol and blended them with other commonly used cosmetic raw materials to attempt preparing a cosmetic, they faced the problem that irreversible aggregated precipitates that cannot be easily redispersed are formed.
[0009] Furthermore, since simonkolleite crystals are white powder with a large particle diameter, "roughness" is perceived and white "residue on the skin" occurs not only when used as-is, but also when dispersed in a dispersion medium such as water or ethanol and applied to the skin. Such physical properties are highly likely to be disfavored by users, and are a major drawback particularly for use as a raw material for cosmetics. In particular, when simonkolleite is incorporated into a scalp care cosmetic, when applied to the scalp, the white "residue on the skin" derived from simonkolleite crystals is extremely different from the color of hair, thus it stands out among the hair and may be confused with "dandruff", resulting in an extremely cosmetically undesirable condition.
[0010] Accordingly, the present invention has been made in view of the above points, and an object thereof is to provide a new use of simonkolleite.
[0011] Another object of the present invention is to provide a cosmetic raw material containing simonkolleite crystals and a cosmetic, which can be easily redispersed without aggregation even when dispersed in a dispersion medium such as water or ethanol, and is easy to handle.
[0012] Another object of the present invention is to provide a cosmetic raw material containing simonkolleite crystals and a cosmetic, in which "roughness" during use and white "residue on the skin" are reduced, providing a smooth feeling of use and a cosmetically favorable appearance even after use. [Means for Solving the Problem]
[0013] The inventors of the present application studied various uses for simonkolleite crystals, and found that simonkolleite crystals have a hair growth promoting effect that surpasses that of minoxidil. Based on this finding, the present invention has been completed. In order to solve the above problems, the hair growth cosmetic of the present invention contains simonkolleite crystals as an active ingredient. Since simonkolleite crystals promote hair elongation in hair follicle tissue, the healthy growth of hair is maintained, and healthy hair can be obtained.
[0014] Furthermore, it is preferable that the amount of simoncolite crystals in the hair growth cosmetic composition of the present invention be between 0.001% and 10% by weight. This allows for the selection of a concentration of simoncolite crystals that provides excellent hair growth effects.
[0015] Furthermore, the simoncolite crystals of the hair growth cosmetic of the present invention have a 90% cumulative particle size (D) in the volume-based particle size distribution measured by laser diffraction scattering. 90 It is also preferable that the nanoparticles are 800 nm or smaller. Simoncolite crystals are D 90 By using nanoparticles of 800 nm or less, when applied to the scalp, the rough feeling caused by the insoluble simoncolite crystals, which are the active ingredient, is eliminated, and no white residue remains on the skin. As a result, a hair growth cosmetic is obtained that has a smooth feel and a cosmetically desirable appearance even after use.
[0016] Furthermore, the hair growth cosmetic of the present invention preferably further contains a dispersion medium and a dispersant, wherein the dispersant is at least one compound selected from the group consisting of polyethylene glycol, polypropylene glycol, ethylene oxide-propylene oxide copolymer, hydroxypropyl cellulose, hydroxypropyl methylcellulose, and hydroxyethyl cellulose. This makes it possible to obtain a hair growth cosmetic that is easy to handle, as the simoncolite crystals are less likely to aggregate when the dosage form of the hair growth cosmetic is a slurry (suspension) in which simoncolite crystals are dispersed in the dispersion medium, thereby increasing storage stability and making it easy to redisperse.
[0017] The cosmetic raw material or cosmetic of the present invention contains nanoparticles of simoncolite crystals. This provides novel cosmetic raw materials and cosmetics that are useful as cosmetics. By using nanoparticles of simoncolite crystals, the rough feeling caused by the simoncolite crystals is reduced, and the white residue on the skin is less likely to occur, resulting in a cosmetic that has a smooth feel and a cosmetically desirable appearance even after use. In this specification, nanoparticles refer to the 90% cumulative particle diameter (D) from the smallest particle side in the volume-based particle size distribution as determined by laser diffraction scattering. 90) refers to particulate matter with a wavelength of 1 nm or more but less than 1000 nm.
[0018] Furthermore, the nanoparticles of simoncolite crystals used as raw materials for cosmetics or cosmetics according to the present invention have a 90% cumulative particle size (D) in the volume-based particle size distribution measured by laser diffraction scattering. 90 It is also preferable that the wavelength is 800 nm or less. This eliminates the rough feeling and white residue caused by simoncolite crystals when applied to the skin, resulting in a cosmetic product that has a smoother feel and a more aesthetically pleasing appearance even after use.
[0019] Furthermore, the nanoparticles of simoncolite crystals used as raw materials for cosmetics or cosmetics according to the present invention have a 50% cumulative particle size (D) in the volume-based particle size distribution measured by laser diffraction scattering. 50 It is also preferable that the wavelength is 250 nm or less. This eliminates the rough feeling and white residue caused by simoncolite crystals when applied to the skin, resulting in a cosmetic product that has an even smoother feel and a cosmetically desirable appearance even after use.
[0020] Furthermore, the cosmetic raw material or cosmetic of the present invention further contains water, a water-miscible organic solvent, or a combination thereof as a dispersion medium. This yields a slurry (suspension) type cosmetic raw material or cosmetic.
[0021] Furthermore, the cosmetic raw material or cosmetic of the present invention may also preferably contain a dispersant. This makes it less likely for the simoncholite crystals contained in the slurry to aggregate, improving storage stability and allowing for easy redispersion, thus resulting in a cosmetic raw material or cosmetic that is easy to handle.
[0022] Furthermore, it is preferable that the dispersant described above is at least one compound selected from the group consisting of polyethylene glycol, polypropylene glycol, ethylene oxide-propylene oxide copolymer, hydroxypropyl cellulose, hydroxypropyl methylcellulose, and hydroxyethyl cellulose. This allows for the selection of a compound suitable as a dispersant.
[0023] Furthermore, the amount of simoncolite crystals in the cosmetic raw material or cosmetic of the present invention is preferably 0.001% to 30% by weight. This allows for the selection of a suitable concentration of simoncolite crystals for use as a cosmetic raw material or cosmetic.
[0024] Furthermore, the cosmetic raw material or cosmetic of the present invention is preferably for hair growth or scalp care. Simoncolite crystals have the effect of promoting hair elongation in hair follicle tissue and maintaining healthy hair growth, so suitable uses as a cosmetic raw material or cosmetic can be selected.
[0025] The present invention provides a method for producing a cosmetic raw material or cosmetic product, comprising: a mixing step of mixing simoncolite crystals and a dispersion medium to obtain a suspension; a stirring step of stirring the suspension for at least one hour; and a micronization step of introducing the suspension after the stirring step into an atomizing device and micronizing the simoncolite crystals contained in the suspension to a nanoscale size. By stirring the suspension of simoncolite crystals and the dispersion medium for at least one hour to allow the two to blend, clogging of the flow channels and nozzles in the atomizing device becomes less likely, and the micronization process of the simoncolite crystals becomes easier, thus providing a cosmetic raw material or cosmetic product in which the simoncolite crystals are micronized to a nanoscale size.
[0026] Furthermore, the method for producing a cosmetic raw material or cosmetic of the present invention is also preferably characterized by further mixing a dispersant into the suspension during the mixing or stirring step. By adding a dispersant to the mixing or stirring step and allowing the simoncolite crystals and dispersant to blend into the dispersion medium, the micronization process of the simoncolite crystals by a micronization device becomes easier, and a cosmetic raw material or cosmetic is obtained in which the simoncolite crystals are less likely to aggregate and the dispersibility is improved.
[0027] The present invention provides a method for producing a cosmetic raw material or cosmetic, comprising: a mixing step of mixing simoncolite crystals with a dispersion medium having a water-miscible organic solvent to obtain a suspension; a micronization step of introducing the suspension into an atomizer and micronizing the simoncolite crystals contained in the suspension to a nanoscale size; and a step of distilling off the water-miscible organic solvent contained in the suspension after the micronization process. By using a water-miscible organic solvent as the dispersion medium, clogging of channels and nozzles in the atomizer is less likely to occur, so the suspension of both can be introduced into the atomizer and micronized without performing a stirring step to mix the dispersion medium and the simoncolite crystals. At this time, by distilling off the water-miscible organic solvent from the obtained suspension, the water-miscible organic solvent can be replaced with another solvent, specifically the water-miscible organic solvent, so that a cosmetic raw material or cosmetic consisting of a water suspension (slurry) of micronized simoncolite crystals can be obtained.
[0028] Furthermore, in the method for producing cosmetic raw materials or cosmetics of the present invention, it is also preferable to further mix in a dispersant during the mixing step to obtain a suspension. By adding a dispersant, a cosmetic raw material or cosmetic can be obtained in which the simoncolite crystals are less likely to aggregate and the dispersibility is improved. [Effects of the Invention]
[0029] According to the present invention, it is possible to provide a hair growth cosmetic composition having the following excellent effects. (1) Simoncolite crystals promote hair elongation, thus maintaining healthy hair growth and resulting in healthy hair. (2) Because the effect lasts for a long time, the frequency of use can be reduced. (3) By using simoncolite crystals, which are the active ingredient, as nanoparticles, the rough feeling and white residue left on the skin caused by the simoncolite crystals are eliminated, resulting in a smooth feel and a cosmetically desirable appearance even after use. (4) By incorporating a dispersant, the simoncolite crystals become less likely to aggregate, improving storage stability and making them easily redispersible, thus simplifying handling.
[0030] Furthermore, according to the present invention, it is possible to provide a cosmetic raw material or cosmetic, and a method for producing the same, which have the following excellent effects. (1) By using simoncolite crystals as nanoparticles, the rough feeling caused by the simoncolite crystals is reduced, and the white residue on the skin is less likely to occur, resulting in a cosmetic product that has a smooth feel and a cosmetically desirable appearance even after use. (2) By incorporating a dispersant, the simoncolite crystals in the slurry are less likely to aggregate, improving storage stability and allowing for easy redispersion, thus making it possible to obtain a cosmetic raw material or cosmetic that is easy to handle. (3) Simoncolite crystals have the effect of promoting hair elongation and maintaining healthy hair growth, and can therefore be suitably used as a raw material for hair growth or scalp cosmetics or as a cosmetic product. (4) Simoncolite crystals can be easily refined to nanoscale size to obtain a slurry-like cosmetic raw material or cosmetic product. [Brief explanation of the drawing]
[0031] [Figure 1] This graph shows hair elongation in rat whisker follicles using the organ culture method in Example 4. [Figure 2] This graph shows the change in particle size distribution of the simoncolite crystal over time in Example 6. [Figure 3] This graph shows hair elongation in rat hair follicles using the organ culture method in Example 9. [Modes for carrying out the invention]
[0032] The following describes the hair growth cosmetic, cosmetic raw materials, and cosmetic products of the present invention, as well as methods for producing them.
[0033] The simoncolite crystal used in the hair growth cosmetic, cosmetic raw material, or cosmetic of the present invention is Zn5(OH)8Cl2·(H2O) nrefers to the white crystalline powder of zinc hydroxide chloride hydrate represented by the above formula. Simonkolleite crystals that are industrially produced by the method described in the above-mentioned Patent Document 2 and the like are generally commercially available. As an example, simonkolleite manufactured by JFE Mineral Co., Ltd. is preferably used, but it is also possible to use simonkolleite obtained by other production methods or simonkolleite derived from natural minerals.
[0034] The simonkolleite crystals blended in the hair growth cosmetic of the present invention are preferably nanoparticles in order to reduce the rough feeling caused by the simonkolleite crystals when applied to the scalp and the residual white color on the skin after application. In the present specification, the term "nanoparticles" refers to particles whose 90% cumulative particle diameter from the small particle side in a volume-based particle size distribution measured by laser diffraction scattering method is D 90 which is a particulate substance having a particle size of 1 nm or more and less than 1000 nm. In the present invention, from the viewpoint of further eliminating the rough feeling caused by simonkolleite crystals and the residual white color on the skin, it is preferable that the 90% cumulative particle diameter D 90 of the simonkolleite crystals is 800 nm or less, more preferably the 50% cumulative particle diameter D 50 is 250 nm or less, still more preferably the 50% cumulative particle diameter D 50 is 150 nm or less, and particularly preferably the 90% cumulative particle diameter D 90 is 550 nm or less and the 50% cumulative particle diameter D 50 is 150 nm or less.
[0035] The hair growth use in the present invention, that is, the hair growth cosmetic or the cosmetic raw material for hair growth, refers to a cosmetic or cosmetic raw material having an effect of promoting hair growth in hair follicle tissue, and means a cosmetic or cosmetic raw material that can promote hair growth in hair follicle tissue compared to a control in which the hair growth cosmetic or cosmetic raw material of the present invention is not applied or added. The promotion level of hair growth in hair follicle tissue can be measured by a known method such as an organ culture method using rat whisker hair follicles, for example.
[0036] The amount of simoncolite crystals contained in the hair growth cosmetic composition of the present invention can be appropriately set depending on the target hair growth effect, formulation and dosage form, method and frequency of use, etc., but from the viewpoint of its effect, 0.001% to 10% by weight is preferred, 0.005% to 5% by weight is more preferred, and 0.01% to 3% by weight is even more preferred.
[0037] On the other hand, the simoncolite crystals incorporated into the cosmetic raw material or cosmetic of the present invention are nanoparticles. This reduces the roughness caused by the simoncolite crystals when applied to the skin, and the white residue left on the skin after application. Specifically, in terms of the particle size of the nanoparticles, from the viewpoint of further eliminating the roughness and white residue left on the skin caused by the simoncolite crystals, the simoncolite crystals are given a 90% cumulative particle size (D 90 It is preferable that the nanoparticles have a diameter of 800 nm or less, and the 50% cumulative particle size (D 50 It is more preferable that the nanoparticles have a diameter of 250 nm or less, and the 50% cumulative particle size (D 50 It is even more preferable that the nanoparticles have a diameter of 150 nm or less, and the 90% cumulative particle size (D 90 ) is 550 nm or less and the 50% cumulative particle size (D 50 ) However, it is particularly preferable that the nanoparticles be 150 nm or smaller.
[0038] The hair growth cosmetic, cosmetic raw material, or cosmetic of the present invention is preferably a suspension (slurry) obtained by dispersing simoncolite crystals in a dispersion medium, from the viewpoint of ease of handling. As the dispersion medium, water, a water-miscible organic solvent, or a combination thereof can be used. Examples of water-miscible organic solvents include alcohols such as ethanol and propanol, ethers such as tetrahydrofuran, esters such as methyl acetate, or ketones such as acetone, but from the viewpoint of safety, ethanol is preferably used.
[0039] Furthermore, when hair growth cosmetics, cosmetic raw materials, or cosmetics are made into a suspension (slurry), it is preferable to include a dispersant to prevent the formation of aggregated precipitates in the suspension that do not easily redisperse the simoncolite crystals. Examples of dispersants include ethylene oxide polymers, ethylene oxide-propylene oxide copolymers, cellulose derivatives, or combinations thereof. Specifically, although not particularly limited, polyethylene glycol, polypropylene glycol, ethylene oxide-propylene oxide copolymer, hydroxypropyl cellulose, hydroxypropyl methylcellulose, or hydroxyethyl cellulose are preferably used. Of these, hydroxypropyl cellulose, hydroxypropyl methylcellulose, polyethylene glycol 6000, or combinations thereof are more preferably used from the viewpoint of further improving the dispersibility of simoncolite crystals in the suspension. From the viewpoint of improving dispersibility, the amount of dispersant added to the suspension is preferably 0.05% to 10% by weight, and more preferably 0.1% to 5% by weight.
[0040] The concentration of simoncolite crystals contained in the cosmetic raw material of the present invention is preferably 1% to 30% by weight, and more preferably 5% to 20% by weight, from the viewpoint of improving the circulation of the cosmetic raw material and ease of handling during manufacturing. On the other hand, the concentration of simoncolite crystals contained in the cosmetic composition of the present invention can be appropriately set depending on the intended use (function) and effect, formulation and dosage form, method of use, etc. Specifically, although not particularly limited, as an example, 0.001% to 10% by weight is preferred, 0.005% to 5% by weight is more preferred, and 0.01% to 3% by weight is even more preferred.
[0041] As mentioned above, the Simoncolite crystal has hair growth-promoting effects, and therefore can be used for hair growth or scalp care. Furthermore, it can be used as a cosmetic ingredient or cosmetic to exhibit other functions of the Simoncolite crystal.
[0042] Next, the hair growth cosmetic, cosmetic raw material, or method for producing the cosmetic of the present invention will be described. The simoncolite crystals incorporated in these are nanoparticles, and the simoncolite crystals that are generally available on the market have an average particle size (D 50 The size of the crystals is quite large, approximately 10 μm. Therefore, it is necessary to reduce these simoncolite crystals to a nanoscale size. For this reduction process, wet grinding is used because it is excellent at reducing crystals to a nanoscale size. The details are explained below.
[0043] (Mixing process) First, the simoncolite crystals and the dispersion medium are mixed to obtain a suspension. As mentioned above, water, a water-miscible organic solvent, or a combination thereof can be used as the dispersion medium. It is also preferable to add the dispersant mentioned above during this mixing step to include the dispersant in the suspension. This is because by including the dispersant in the suspension containing the simoncolite crystals and then introducing the suspension into a micronizer to micronize the simoncolite crystals, a slurry with improved dispersibility can be obtained.
[0044] (Agitation process) Next, the suspension obtained by mixing the simoncolite crystals with the dispersion medium is stirred. This stirring step allows the simoncolite crystals in the suspension to adapt to the dispersion medium, making it less likely for the flow channels and nozzles in the atomizing device to become clogged during the atomizing process, thus facilitating the atomizing of the simoncolite crystals. The stirring method is not particularly limited as long as it can stir the entire suspension, but for example, a propeller-type stirrer or a magnetic stirrer can be used. The stirring time is preferably 1 hour or more, and more preferably 2 hours or more, in order to allow the dispersion medium and simoncolite crystals to adapt. It is also preferable to add the above-mentioned dispersant during this stirring step to include the dispersant in the suspension. If a water-miscible organic solvent such as ethanol is selected as the dispersion medium, it is possible to perform the atomizing process without stirring.
[0045] (Miniaturization process) In the micronization process, the suspension is introduced into a micronizer to micronize the simoncolite crystals in the suspension to a nanoscale size. A wet micronizer is used as the micronizer, for example, a high-pressure homogenizer type wet micronizer or a bead mill type wet micronizer is used. The micronization process reduces the simoncolite crystals to a 90% cumulative particle size (D 90 It is preferable to perform the procedure so that the nanoparticles have a diameter of 800 nm or less, and the 50% cumulative particle size (D 50 It is more preferable to perform the procedure so that the nanoparticle size (D) is 250 nm or less, and the 50% cumulative particle size (D) 50 It is even more preferable that the nanoparticles have a diameter of 150 nm or less, and the 90% cumulative particle size (D 90 ) is 550 nm or less and the 50% cumulative particle size (D 50 It is particularly preferable to perform the process so that the nanoparticle size (D) is 150 nm or less. In the micronization process, in the case of a high-pressure homogenizer type apparatus, there are micronization conditions such as the chamber used, pressure, nozzle diameter, number of passes, or processing time, and in the case of a bead mill type apparatus, there are micronization conditions such as the material of the beads used, bead diameter, or processing time, but these processing conditions can be appropriately set based on the specifications of the apparatus used and the desired level of micronization. Furthermore, in this micronization process, a preliminary grinding process may be performed to roughly grind the simoncolite crystals in the suspension beforehand, and then a micronization process may be performed to further refine the crystals. For the preliminary grinding process, the same apparatus as the micronization apparatus described above can be used, and the simoncolite crystals in the suspension are roughly ground by reducing the processing time, number of passes, pressure, etc., or by increasing the nozzle diameter of the chamber used or the bead diameter used, etc., compared to the conditions for the main micronization process. 50 This allows for the stable production of simoncolite crystals with small ) and uniform nanoparticle sizes.
[0046] (Solvent removal process) Furthermore, if a water-miscible organic solvent such as ethanol is selected as the dispersion medium, the dispersion medium can be replaced with another dispersion medium, specifically water, by distilling off the water-miscible organic solvent contained in the water-miscible organic solvent slurry after the micronization treatment. Specifically, as an example, water is added to the ethanol slurry after the micronization treatment, and a reduced-pressure environment is created, followed by steam distillation. This removes the ethanol, and a water slurry containing dispersed micronized simoncolite crystals can be obtained.
[0047] The slurry obtained by the above-described micronization process or distillation process can be used as is as a slurry in hair growth cosmetics, cosmetic raw materials, or cosmetics. In addition, concentrated liquids obtained by concentration treatment and fine powders obtained by drying treatment can also be used in hair growth cosmetics, cosmetic raw materials, or cosmetics.
[0048] Furthermore, if the simoncolite crystals in the formulation are not to be in the form of nanoparticles, it is also possible to obtain a hair growth cosmetic by adding simoncolite crystals and, if necessary, a dispersant to a dispersion medium and dispersing them.
[0049] The cosmetic raw material of the present invention can be used as a raw material for hair growth, scalp care, and topical skin preparations to promote hair elongation in hair follicle tissue, maintain healthy hair growth, and obtain healthy hair.
[0050] The amount of the hair growth cosmetic composition of the present invention used varies depending on the desired hair elongation effect, method of use, age, and hair condition, and therefore cannot be specified in general terms. However, as simoncolite crystals, the amount per epidermal unit area (1 cm²) is... 2 ) Per unit: 0.01~1000 μg / cm³ 2 It is preferable to use a daily dose of 0.1 to 500 μg / cm³. 2 It is preferable to use "day".
[0051] The hair growth cosmetic, cosmetic raw material, or cosmetic of the present invention can be applied to various topical formulations by conventional methods, as a dosage form typically applied to the scalp or skin. Examples include liquid formulations such as slurries and low-viscosity liquids, gels, emulsions, pastes, creams, foams, ointments, or powders. The hair growth cosmetic, cosmetic raw material, or cosmetic of the present invention can be applied to cosmetics, quasi-drugs, or pharmaceuticals. Specific products are not particularly limited, but examples include hair tonics, scalp lotions, shampoos, conditioners, treatments, hair styling products, soaps, lotions, cosmetic creams, cosmetic emulsions, serums, cosmetic packs, cosmetic cleansers, bath additives, or makeup cosmetics.
[0052] Furthermore, the hair growth cosmetic, cosmetic raw material, or cosmetic of the present invention may contain various components commonly used in cosmetics and topical preparations, to the extent that they do not impair the effects of the present invention. Examples include vasodilators, blood circulation promoters, surfactants, antihistamines, anti-inflammatory agents, thickeners, vitamins, amino acids, humectants, preservatives, antibacterial agents, fragrances, and pigments. It is also possible to incorporate hair growth and hair regeneration components other than simoncolite crystals. Examples of other hair growth and hair regeneration components include minoxidil, adenosine, or Swertia japonica extract. [Examples]
[0053] The present invention will be described in more detail below with reference to examples and comparative examples. The method for measuring the particle size of simoncolite crystals in each sample prepared in the following examples and comparative examples, and the method for evaluating each sample, are as follows.
[0054] (1) Particle size The particle size distribution of the samples obtained in the examples and comparative examples was measured using a laser diffraction scattering particle size distribution analyzer (model: Partica LA-960, manufactured by Horiba, Ltd.). The refractive index parameter of the simoncolite crystal was set to 1.700-0.000i, and the measurement was performed using deionized water or anhydrous ethanol in which the simoncolite crystal was dispersed as the dispersion medium for each sample. From the obtained particle size distribution, the 90% cumulative particle size (D) in the volume-based particle size distribution was determined. 90 ) and 50% cumulative particle size (D 50 ) was sought.
[0055] (2) roughness For each sample obtained in the examples and comparative examples, evaluation samples were prepared by diluting them with the same dispersion medium (ion-exchanged water or anhydrous ethanol) used in the original sample so that the concentration of simoncolite crystals reached 5 wt%. 50 μL of each evaluation sample was taken, dropped onto the inner forearm, and gently spread over a 4 cm diameter area with a finger. The perceived roughness was evaluated according to the following criteria. ◎: I don't feel any roughness at all. ○: Slightly rough texture. △: Feels slightly rough. ×: Feels very rough.
[0056] (3) Skin residue In the evaluation of "(2) roughness" described above, the evaluation sample liquid applied to the inner forearm was tested for the presence or absence of a white residue on the skin after it had dried on the skin, according to the evaluation criteria below. ◎: No white residue on the skin was observed at all. ○: Almost no white residue of skin is observed. △: Slight traces of white skin remain in some areas. ×: A clear white residue of skin is visible throughout.
[0057] (4) Dispersibility Each evaluation sample, diluted to a concentration of 5 wt% simoncolite crystals, was taken in 8 mL portions and placed in 10 mL vials (Mighty Vial No. 3, Maruemu Co., Ltd.). The vials were shaken to disperse the simoncolite crystals in the evaluation samples, and then left to stand at room temperature for 18 hours. After 18 hours, the dispersibility of the simoncolite crystals was evaluated according to the following evaluation criteria. ◎: The dispersion state of the simoncolite crystals is maintained, or the simoncolite crystals disperse simply by gently shaking the vial a few times. ○: Shaking the vial disperses the simoncolite crystals. △: By vigorously shaking the vial, the simoncolite crystals are dispersed. ×: Even when the vial is shaken vigorously, some simoncolite crystals remain at the bottom of the vial and are difficult to disperse.
[0058] Table 1 shows the specifications of the ingredients used in the following examples and comparative examples.
[0059] [Table 1]
[0060] [Example 1] 1. Preparation of Simoncolite aqueous slurry Simoncolite (JFE Mineral Co., Ltd., Lot No.: S1C231) was sieved through a 32-mesh sieve to obtain 5 g of sieved Simoncolite. Deionized water was added to this as a dispersion medium to make 100 mL, and then ultrasonic irradiation was performed for 2 minutes to obtain 100 mL of Simoncolite aqueous slurry (aqueous suspension). The particle size of the Simoncolite crystals in this slurry was the 90% cumulative particle size (D 90 ) is 9458nm, 50% cumulative particle size (D 50 The wavelength was 5600 nm.
[0061] [Example 2] 2. Preparation of aqueous slurry of simoncolite nanocrystals (1) 160g of Simoncolite (JFE Mineral Co., Ltd., Lot No.: TOL81) was added to 840g of deionized water and mixed. The mixture was then stirred using a propeller-type stirrer at a stirring speed of 300-500 rpm for 4 hours and 30 minutes. The resulting aqueous slurry (aqueous suspension) of Simoncolite crystals was introduced into a high-pressure homogenizer-type wet atomization device (Starburst Lab, manufactured by Sugino Machine Co., Ltd.). The device was subjected to a micronization process under the following conditions: chamber: ball impact chamber, chamber nozzle diameter: 0.14 mm, pressure: 245 MPa, number of passes: 30. As a result, an aqueous slurry was obtained in which Simoncolite crystals were micronized to nanoscale size. The particle size of the Simoncolite crystals in this slurry was the 90% cumulative particle size (D 90 ) is 401nm, 50% cumulative particle size (D 50 The wavelength was 133 nm.
[0062] [Example 3] 3. Preparation of aqueous slurry of simoncolite nanocrystals (2) 62.5 g of the aqueous slurry obtained in Example 2 was mixed with deionized water to make a total volume of 200 mL, and the mixture was shaken well to prepare a diluted slurry with a simoncolite crystal concentration of 5 w / v% in the slurry.
[0063] [Comparative Example 1] 4. Preparation of the supernatant of the aqueous slurry of Simoncholyte nanocrystals Although simoncolite is insoluble in water, it is believed that very small amounts of zinc ions dissolve into the water. Therefore, to investigate the effect of zinc ions dissolving into the aqueous slurry of simoncolite nanocrystals, a supernatant of the aqueous slurry was prepared. Specifically, the aqueous slurry with a simoncolite crystal concentration of 5 w / v%, obtained in Example 3, was centrifuged at 1830 × g for 30 minutes (model number: AX-521, manufactured by Tommy Seiko Co., Ltd.). The supernatant was collected and filtered through a membrane filter with a pore size of 0.22 μm (Millex®-GV filter, manufactured by Merck), and a colorless, clear filtrate was obtained as the supernatant of the aqueous slurry.
[0064] Table 2 below shows the formulation, manufacturing conditions, particle size, and various evaluations of the samples prepared in Examples 1-3 and Comparative Example 1.
[0065] [Table 2]
[0066] [Example 4] 5. Investigation of the hair growth effect of Simoncolite crystals (1) The hair growth promoting effect of Simoncolite was investigated by organ culture of rat whisker hair follicles using the samples prepared in Examples 1 and 3 and Comparative Example 1. The test was carried out as follows: Male SD rats (SLC Japan Co., Ltd.) that were 7 weeks old and weighed 210-230 g were anesthetized, and the whisker skin was aseptically excised. From the first and second rows of whisker hair on the excised skin, hair follicles with two hairs growing from a single follicle (growing hair follicles) were selected and isolated under a stereomicroscope. The isolated hair follicles were washed with a culture medium (Thermo Fisher Scientific Co., Ltd.) supplemented with penicillin G (100 IU / mL), streptomycin (100 μg / mL), and amphotericin B (0.25 μg / mL). Next, culture media were prepared by adding the samples prepared in Examples 1, 3, and Comparative Example 1, as well as minoxidil as the positive control, to 10% FBS-containing DMEM medium. As shown in Table 3 below, the samples and minoxidil shown in Table 3 below were added to 10% FBS-containing DMEM medium (negative control) to the predetermined concentrations to prepare culture media for each test group (Tests 4a to 4e).
[0067] Cell culture inserts (Millicell®, Merck product) were placed in 6-well cell culture plates, and the membranes were moistened from below with 2 mL of the culture medium for each test group (tests 4a-4e). Twenty hair follicles immersed in PBS were randomly selected from each test group, transferred to the membrane using tweezers, and placed in a CO2 incubator (Napco 7100) at 37°C under 5% CO2 conditions. The culture was carried out for 7 days, and hair elongation was observed and recorded under a stereomicroscope, measuring the change in the total length from the starting point of the black tissue of the hair root to the point of hair transection, and the change in the length of the exposed hair portion from the skin surface to the point of hair transection. The results are shown in Figure 1.
[0068] [Table 3]
[0069] As shown in Figure 1, all test groups showed similar hair elongation until the fourth day from the start of the test. However, after the fourth day, only the Simoncolite test group of Example 1 (4b) and the Simoncolite nanocrystal test group of Example 3 (4c) showed significant hair elongation. This elongation effect was outstanding not only compared to the negative control test group (4a) but also to the positive control test group of minoxidil (4e). Notably, no such outstanding effect was observed in the Simoncolite supernatant test group of Comparative Example 1 (4d). These findings indicate that the remarkable hair elongation effect shown by the Simoncolite test group of Example 1 (4b) and the Simoncolite nanocrystal test group of Example 3 (4c) is not simply due to the effect of zinc ions dissolved in the aqueous phase in equilibrium with Simoncolite, but rather is an effect specific to Simoncolite crystals, which are a water-insoluble powder.
[0070] [Example 5] 6. Investigation of the dispersibility of simoncolite nanocrystalline slurry (1) The particle size distribution of unprocessed simoncolite (Example 1) is D 50 5.6 μm, D 90The particles are large, measuring 9.5 μm. Therefore, when applied to the skin as a cosmetic, a rough texture due to the crystals is felt, and a white residue remains on the applied area after application, which is undesirable from a cosmetic standpoint. Furthermore, although the simoncolite nanocrystalline slurry obtained in Examples 2 and 3 is a nanoparticle, eliminating the rough texture and white residue on the skin, aggregation and precipitation of simoncolite crystals occur. When using it, the container must be shaken vigorously until the simoncolite crystals are redispersed, which is time-consuming. Therefore, in order to obtain a simoncolite nanocrystalline slurry with improved dispersibility from un-micronized simoncolite, various samples were prepared using the formulations and manufacturing conditions shown in Tables 4 and 5 below, and dispersants were investigated.
[0071] (Exam 5-1) 103 g of Japanese Pharmacopoeia anhydrous ethanol was dissolved in 2 g of hydroxypropyl cellulose as a dispersant. 20 g of simoncolite (JFE Mineral Co., Ltd., Lot No.: TOL81) was added to this solution to obtain a suspension. This suspension was introduced into a high-pressure homogenizer-type wet atomization apparatus (Starburst Mini, manufactured by Sugino Machine Co., Ltd.), and atomized under the following conditions: chamber: ball impact chamber, chamber nozzle diameter: 0.1 mm, pressure: 200 MPa, number of passes: 10 passes, to obtain an ethanol slurry. The particle size of the simoncolite crystals in this slurry sample was measured, and various evaluations of the sample were performed. The results are shown in Table 4.
[0072] (Exam 5-2) An ethanol slurry was obtained in the same manner as in Test 5-1, except that the amount of anhydrous ethanol was changed to 101 g, the amount of hydroxypropyl cellulose to 4 g, and the number of passes in the micronization process was changed to 20 passes. The particle size of the simoncolite crystals and various evaluations of the sample were performed on this slurry sample. The results are shown in Table 4.
[0073] (Exam 5-3) 48 g of hydroxypropyl cellulose was dissolved in 1212 g of Japanese Pharmacopoeia anhydrous ethanol as a dispersant. 240 g of simoncolite (JFE Mineral Co., Ltd., Lot No.: S1C231, 30-mesh sieved) was added to this solution to obtain a suspension. This suspension was introduced into a high-pressure homogenizer-type wet atomization apparatus (Starburst Lab, manufactured by Sugino Machine Co., Ltd.), and atomized under the following conditions: chamber: ball impact chamber, chamber nozzle diameter: 0.14 mm, pressure: 200 MPa, number of passes: 30 passes, to obtain an ethanol slurry. The particle size of the simoncolite crystals and various evaluations of the slurry sample were performed. The results are shown in Table 4.
[0074] (Exam 5-4) 80.8 g of Japanese Pharmacopoeia anhydrous ethanol was dissolved in 3.2 g of hydroxypropyl cellulose as a dispersant. 16 g of simoncolite (JFE Mineral Co., Ltd., Lot No.: TOL81) was added to this solution to obtain a suspension. This suspension was introduced into a high-pressure homogenizer-type wet atomization apparatus (Starburst Mini, manufactured by Sugino Machine Co., Ltd.), and atomized under the following conditions: chamber: slit chamber, chamber nozzle diameter: equivalent to 0.16 mm, pressure: 175 MPa, number of passes: 20 passes, to obtain an ethanol slurry. The particle size of the simoncolite crystals and various evaluations of the slurry sample were performed. The results are shown in Table 4.
[0075] (Exam 5-5) An ethanol slurry was obtained in the same manner as in Test 5-4, except that the number of passes in the refinement process was changed to 30 passes. The particle size of the simoncolite crystals and various evaluations of the sample were performed on this slurry sample. The results are shown in Table 4.
[0076] (Exam 5-6) 82.4 g of Japanese Pharmacopoeia anhydrous ethanol was dissolved in 1.6 g of hydroxypropyl methylcellulose as a dispersant. 16 g of simoncolite (JFE Mineral Co., Ltd., Lot No.: TOL81) was added to this solution to obtain a suspension. This suspension was introduced into a high-pressure homogenizer-type wet atomization apparatus (Starburst Mini, manufactured by Sugino Machine Co., Ltd.), and atomized under the following conditions: chamber: slit chamber, chamber nozzle diameter: equivalent to 0.16 mm, pressure: 175 MPa, number of passes: 30 passes, to obtain an ethanol slurry. The particle size of the simoncolite crystals in this slurry sample was measured, and various evaluations of the sample were performed. The results are shown in Table 4.
[0077] (Exam 5-7) An ethanol slurry was obtained in the same manner as in Test 5-6, except that the dispersant was changed to polyethylene glycol 6000 (PEG-6000P, product of Sanyo Chemical Industries, Ltd.). The particle size of the simoncolite crystals and various evaluations of the sample were performed on this slurry sample. The results are shown in Table 5.
[0078] (Exam 5-8) Japanese Pharmacopoeia anhydrous ethanol was mixed with polyethylene glycol 6000 (PEG6000, product of Kishida Chemical Co., Ltd.) at a concentration of 0.8 wt% and simoncolite (JFE Mineral Co., Ltd., lot number: T0I71-A5) at a concentration of 16 wt% to obtain a suspension. This suspension was introduced into a bead mill type wet atomizer (Labostar Mini LMZ015, product of Ashizawa Finetech Co., Ltd.) and ground for 150 minutes using 0.2 mm diameter PSZ beads. Then, polyethylene glycol 6000 was added to a final concentration of 1.6 wt%, and the 0.2 mm diameter PSZ beads were changed to 0.05 mm diameter PSZ beads, and the mixture was ground for a further 120 minutes to perform a finer atomization process. The resulting ethanol slurry sample was subjected to measurement of the particle size of simoncolite crystals and various evaluations of the sample. The results are shown in Table 5.
[0079] (Exam 5-9) An ethanol slurry was prepared in the same manner as in Test 5-1, except that the amount of anhydrous ethanol was changed to 101 g and the dispersant was changed to polyethylene glycol 400 and its amount to 4 g. The particle size of the simoncolite crystals and various evaluations of the sample were performed on this slurry sample. The results are shown in Table 5.
[0080] (Exam 5-10) An ethanol slurry was obtained in the same manner as in Test 5-1, except that the dispersant was changed to polyethylene glycol 1000. The particle size of the simoncolite crystals and various evaluations of the sample were performed on this slurry sample. The results are shown in Table 5.
[0081] (Exam 5-11) An ethanol slurry was prepared in the same manner as in Test 5-1, except that the amount of anhydrous ethanol was changed to 152 g, the dispersant was changed to a mixture of polyethylene glycol 1000 and propylene glycol 1-methoxy-2-acetate (weight ratio PEG1000:PGMA=8:2) and its amount was changed to 8 g, and the amount of simoncolite was changed to 40 g. The particle size of the simoncolite crystals and various evaluations of the sample were performed on this slurry sample. The results are shown in Table 5.
[0082] (Exam 5-12) An ethanol slurry was prepared in the same manner as in Test 5-1, except that the amount of anhydrous ethanol was changed to 78 g and the dispersant was changed to propylene glycol 1-methoxy-2-acetate and its amount to 2 g. The particle size of the simoncolite crystals and various evaluations of the sample were performed on this slurry sample. The results are shown in Table 5.
[0083] (Exam 5-13) An ethanol slurry was prepared in the same manner as in Test 5-1, except that the amount of anhydrous ethanol was changed to 78 g and the dispersant was changed to ethoxyethyl acetate and its amount to 2 g. The particle size of the simoncolite crystals and various evaluations of the sample were performed on this slurry sample. The results are shown in Table 5.
[0084] [Table 4]
[0085] [Table 5]
[0086] The results in Table 4 show that using hydroxypropylcellulose and hydroxypropylmethylcellulose, which are cellulose derivatives, as dispersants improved dispersibility and eliminated the grittiness and white residue found in simoncolite nanocrystalline slurry. Furthermore, the results in Table 5 show that polyethylene glycol is also suitably used as a dispersant, and that polyethylene glycol 6000 (PEG6000) in particular is suitable for improving dispersibility and eliminating grittiness and white residue. On the other hand, when polyethylene glycol 1000, propylene glycol 1-methoxy-2-acetate, and ethoxyethyl acetate were used as dispersants, not only was there no improvement in dispersibility, but the refinement of simoncolite crystals was also insufficient, making it difficult to refine to the nanoscale.
[0087] Furthermore, from the results in Tables 4 and 5, the simoncolite crystal was found to have a 90% cumulative particle size (D 90 It was revealed that by miniaturizing the particles to nanoparticles of 800 nm or less, the roughness and white residue on the skin are reduced, resulting in a slurry with a superior feel. Furthermore, the 90% cumulative particle size (D 90 ) is 550 nm or less and the 50% cumulative particle size (D 50It was shown that by miniaturizing the material to nanoparticles of 150 nm or less, the rough texture and white residue on the skin are eliminated, resulting in a slurry with an excellent feel for use as a cosmetic.
[0088] Furthermore, when a high-pressure homogenizer type atomizer was used as the atomization treatment condition, little influence was observed due to the difference in chamber type, and atomization to a similar level was achieved in both the ball-impact type chamber and the slit type chamber. It was also confirmed that atomization to a smaller size was achieved as the number of passes increased. In addition, it was shown that not only high-pressure homogenizer type atomizers but also bead mill type atomizers can be suitably used as atomizers (Test 5-8).
[0089] [Example 6] 7. Investigation of the dispersibility of simoncolite nanocrystalline slurry (2) The particle size distribution of simoncolite crystals was measured immediately after sample preparation and after the samples were stored at room temperature for one week, for both samples containing a dispersant and samples without a dispersant. The sample containing the dispersant was the ethanol slurry obtained in Test 5-3 of Example 5 (dispersant: hydroxypropyl cellulose), and the sample without the dispersant was the water slurry obtained in Example 2. The results are shown in Figure 2.
[0090] As is clear from Figure 2, in the sample of Example 2, which did not contain a dispersant, after one week, almost no particles smaller than 200 nm were observed, and the simoncolite particles had aggregated into 10 μm particles. On the other hand, in the slurry sample of Test 5-3 of Example 5, which contained hydroxypropyl cellulose as a dispersant, there was almost no change in the particle size distribution of simoncolite nanoparticles, and the particle size distribution was maintained at the same level as immediately after sample preparation. From this, it became clear that the dispersant not only improves the dispersibility of the slurry, but also has a significant effect on maintaining the nanoscale size of simoncolite particles and improving storage stability.
[0091] [Example 7] 8. Investigation of a method for producing aqueous slurry of simoncolite nanocrystals (1) In this invention, when water is selected as the dispersion medium for simoncolite crystals, it has been found that difficulties in micronizing the simoncolite particles tend to occur, as shown in Test 7-1 below. Therefore, various methods for producing a water slurry of simoncolite nanocrystals when water is selected as the dispersion medium were investigated.
[0092] (Exam 7-1) 840g of deionized water was mixed with 160g of Simoncolite (JFE Mineral Co., Ltd., lot number: TOL81), and the mixture was stirred for 3 minutes at a stirring speed of 300-400 rpm using a propeller-type agitator. The resulting aqueous slurry (aqueous suspension) of Simoncolite crystals was then introduced into a high-pressure homogenizer-type wet atomization device (Starburst Lab, manufactured by Sugino Machine Co., Ltd.). An attempt was made to perform atomization under the following conditions: chamber: ball impact chamber, chamber nozzle diameter: 0.14 mm, pressure: 245 MPa. However, clogging such as adhesion occurred in the pipeline, and atomization could not be performed. The results are shown in Table 6.
[0093] (Exam 7-2) 4.8 g of hydroxypropyl cellulose was dissolved in 121.2 g of deionized water as a dispersant, and 24 g of simoncolite (JFE Mineral Co., Ltd., lot number: TOL81) was added to this solution to obtain a suspension. This suspension was stirred for 2 hours using a propeller-type stirrer at a stirring speed of 500-1000 rpm. The aqueous slurry (aqueous suspension) of simoncolite crystals after stirring was introduced into a high-pressure homogenizer-type wet atomization device (Starburst Mini, manufactured by Sugino Machine Co., Ltd.), and atomization was performed under the following conditions: chamber: ball impact chamber, chamber nozzle diameter: 0.1 mm, pressure: 245 MPa, number of passes: 30 passes, to obtain an aqueous slurry. The particle size of the simoncolite crystals and various evaluations of the sample were performed on this slurry sample. The results are shown in Table 6.
[0094] (Exam 7-3) 24 g of Simoncolite (JFE Mineral Co., Ltd., Lot No.: TOL81) was added to 121.2 g of deionized water to obtain a suspension. This suspension was stirred with a magnetic stirrer for 4 hours, then allowed to stand overnight to acclimate to water. 4.8 g of polyethylene glycol 6000 (PEG-6000P, Sanyo Chemical Industries, Ltd.) was added to this suspension as a dispersant, and the mixture was stirred for 3 hours at a stirring speed of 500-1000 rpm using a propeller-type stirrer. The aqueous slurry (aqueous suspension) of Simoncolite crystals after stirring was subjected to micronization treatment under the same conditions and methods as in Test 7-2 to obtain an aqueous slurry. The particle size of Simoncolite crystals and various evaluations of the sample were performed on this slurry sample. The results are shown in Table 6.
[0095] (Exam 7-4) 2.56 g of polyethylene glycol 6000 (PEG-6000P, Sanyo Chemical Industries, Ltd.) was dissolved in 168 g of deionized water as a dispersant. 32 g of Simoncolite (JFE Mineral Corporation, lot number: TOL81) was added to this solution to obtain a suspension. This suspension was introduced into a high-pressure homogenizer-type wet atomization device (Starburst Mini, Sugino Machine Co., Ltd.), and an attempt was made to perform atomization under the following conditions: chamber: ball impact chamber, chamber nozzle diameter: 0.1 mm, pressure: 245 MPa. However, clogging such as adhesion occurred in the tubing, and atomization could not be performed. The results are shown in Table 6.
[0096] (Exam 7-5) 2.56 g of polyethylene glycol 400 was dissolved in 168 g of deionized water as a dispersant, and 32 g of Simoncolite (JFE Mineral Co., Ltd., lot number: TOL81) was added to this solution to obtain a suspension. This suspension was introduced into a high-pressure homogenizer type wet atomization device (Starburst Mini, manufactured by Sugino Machine Co., Ltd.), and an attempt was made to perform atomization under the following conditions: chamber: ball impact chamber, chamber nozzle diameter: 0.1 mm, pressure: 245 MPa. However, clogging such as adhesion occurred in the pipeline, and atomization could not be performed. The results are shown in Table 6.
[0097] (Exam 7-6) 760 g of deionized water was dissolved in 40 g of hydroxypropyl cellulose as a dispersant. 200 g of simoncolite (JFE Mineral Co., Ltd., lot number: S1J201) was added to this solution to obtain a suspension. This suspension was stirred for 5.5 hours using a propeller-type stirrer at a stirring speed of 500-1000 rpm. This aqueous slurry (aqueous suspension) of simoncolite crystals was introduced into a high-pressure homogenizer-type wet atomization apparatus (Starburst Lab, manufactured by Sugino Machine Co., Ltd.), and the mixture was atomized under the following conditions: chamber: slit-type chamber, chamber nozzle diameter: 0.16 mm, pressure: 150 MPa, number of passes: 50 passes, to obtain an aqueous slurry. The particle size of the simoncolite crystals and various evaluations of the slurry sample were performed. The results are shown in Table 7.
[0098] (Exam 7-7) 40 g of hydroxypropyl cellulose was dissolved in 1760 g of deionized water as a dispersant. 200 g of simoncolite (JFE Mineral Co., Ltd., lot number: S1J201) was added to this solution to obtain a suspension. This suspension was stirred using a propeller-type stirrer at a stirring speed of 500-1000 rpm for 3 hours and then allowed to stand overnight. This simoncolite crystal aqueous slurry (aqueous suspension) was introduced into a high-pressure homogenizer-type wet atomization device (Starburst Lab, manufactured by Sugino Machine Co., Ltd.), and preliminary grinding was performed under the following conditions: chamber: slit-type chamber, chamber nozzle diameter: 0.16 mm, pressure: 150 MPa, number of passes: 5. After preliminary grinding, the chamber of the wet atomization device was changed to another slit-type chamber (model number: ESC-101, the nozzle diameter is presumed to be smaller than the chamber used in the preliminary grinding), and fine grinding was performed under the following conditions: pressure: 150 MPa, number of passes: 50, to obtain an aqueous slurry. The particle size of the simoncolite crystals and various other evaluations of the sample were performed on this slurry sample. The results are shown in Table 7.
[0099] (Exams 7-8) 765.6 g of deionized water was mixed with 17.4 g of polyethylene glycol 6000 (PEG-6000P, Sanyo Chemical Industries, Ltd.) as a dispersant, and 87 g of simoncolite (JFE Mineral Co., Ltd., lot number: S1J201) was added to obtain a suspension. This suspension was stirred for 2 hours using a propeller-type stirrer at a stirring speed of 500-1000 rpm. The aqueous slurry (aqueous suspension) of simoncolite crystals after stirring was subjected to preliminary grinding and micronization treatment under the same conditions and methods as in Test 7-7 to obtain an aqueous slurry. The particle size of the simoncolite crystals and various evaluations of the sample were performed on this slurry sample. The results are shown in Table 7.
[0100] (Exam 7-9) 880 g of deionized water was mixed with 10 g of hydroxypropyl cellulose and 10 g of polyethylene glycol 6000 (PEG-6000P, Sanyo Chemical Industries, Ltd.) as dispersants, and 100 g of simoncolite (JFE Mineral Co., Ltd., lot number: S1J201) was added to obtain a suspension. This suspension was stirred for 2 hours using a propeller-type stirrer at a stirring speed of 500-1000 rpm. The aqueous slurry (aqueous suspension) of simoncolite crystals after stirring was subjected to preliminary grinding and micronization treatment under the same conditions and methods as in Test 7-7 described above, except that the number of passes in the micronization treatment was set to 40 passes, to obtain an aqueous slurry. The particle size of the simoncolite crystals and various evaluations of the sample were performed on this slurry sample. The results are shown in Table 7.
[0101] (Tests 7-10) 1043 g of deionized water was dissolved with 56 g of hydroxypropyl cellulose as a dispersant and 21 g of phenoxyethanol as a preservative. 280 g of simoncolite (JFE Mineral Co., Ltd., lot number: S1J201) was added to obtain a suspension. This suspension was stirred for 3 hours using a propeller-type stirrer at a stirring speed of 500-1000 rpm. The resulting aqueous slurry (aqueous suspension) of simoncolite crystals was subjected to preliminary grinding and micronization treatments under the same conditions and methods as in Test 7-9 to obtain an aqueous slurry. The particle size of the simoncolite crystals and various evaluations of the slurry sample were performed. The results are shown in Table 7.
[0102] [Table 6]
[0103] [Table 7]
[0104] Table 6 also shows the results of Example 2. As shown in Table 6, in tests 7-1, 7-4, and 7-5, which did not include a stirring step, adhesion occurred in the high-pressure homogenizer, presumably due to simoncolite crystals, resulting in a state where micronization treatment could not be performed. On the other hand, as shown in Tables 6 and 7, it became clear that by including a stirring step in which a suspension containing simoncolite crystals and water is stirred for a predetermined time before the micronization treatment step, the simoncolite crystals can be smoothly micronized to nanoscale size even when water is selected as the dispersion medium (Example 2, Tests 7-2 and 7-3, Tests 7-6 to 7-10). Furthermore, even when a dispersant was added, the micronization device operated without problems and the simoncolite crystals were micronized to nanoscale size after going through the stirring step (Tests 7-2 and 7-3, Tests 7-6 to 7-10). Furthermore, even when water was selected as the dispersion medium, it was confirmed that high-pressure homogenizer type atomizers could atomize particles to a good level regardless of whether a ball-impact type chamber or a slit-type chamber was used. In addition, by performing a rough pulverization process with a small number of passes as a preliminary grinding treatment, and then performing the finer pulverization treatment, the 50% cumulative particle size (D 50 It was revealed that the size of the simoncolite crystals became stably smaller (150 nm or less), and a slurry with excellent evaluation in terms of roughness, skin residue, and dispersibility was obtained (Tests 7-7 to 7-10). Furthermore, even when phenoxyethanol, a preservative, was added to the slurry, it did not affect the level of refinement of the simoncolite crystals, and the various evaluations remained excellent (Test 7-10).
[0105] [Example 8] 9. Investigation of a method for producing aqueous slurry of simoncolite nanocrystals (2) We investigated whether a water slurry of simoncolite nanocrystals could be produced by changing the dispersion medium of the ethanol slurry of simoncolite nanocrystals to water. First, 32 g of deionized water was added to 20 g of the ethanol slurry obtained in Test 5-3 of Example 5. Ethanol was removed by steam distillation under reduced pressure in a rotary evaporator to obtain 27.11 g of water slurry. Deionized water was added to this to make 32 g, and a water slurry containing 10 w / w% simoncolite nanocrystals was obtained. 25 g of this product was diluted with deionized water to make 50 mL, and a water slurry containing 5 w / v% simoncolite nanocrystals and 1 w / v% hydroxypropyl cellulose was obtained (Table 8).
[0106] [Table 8]
[0107] As shown in Table 8, it was demonstrated that the dispersion medium can be converted from ethanol to water by steam distillation of the ethanol in the ethanol slurry of simoncolite nanocrystals. Since stirring is unnecessary when ethanol is selected as the dispersion medium, a manufacturing method can be proposed in which the simoncolite nanocrystal slurry is prepared as an ethanol slurry, and then, if necessary, a water slurry is prepared by ethanol distillation.
[0108] [Example 9] 10. Investigation of the hair growth effect of Simoncolite crystals (2) Using samples containing the dispersant prepared in Example 8, organ cultures of rat hair follicles were performed to investigate the hair growth promoting effect of Simoncolite. The test was conducted in the same manner as in Example 4 described above. The culture solutions used in each test group (Tests 1-3) are shown in Table 9 below. The culture was performed for 7 days, and hair elongation was observed and recorded under a stereomicroscope, measuring the change in the total length from the starting point of the black tissue in the hair root to the hair cutting point, and the length of the exposed hair portion from the skin surface to the hair cutting point. The results are shown in Figure 3.
[0109] [Table 9]
[0110] Similar to the results in Figure 1 of Example 4, as shown in Figure 3, from the 5th day after the start of the test, only the test group (Test 2) to which the sample containing simoncolite nanocrystals and dispersant of Example 8 was added showed significant hair elongation. This elongation effect was outstanding not only compared to the negative control test group (Test 1) but also to the positive control test group of minoxidil (Test 3). These results indicate that, similar to Example 4, simoncolite nanocrystals also have a hair elongation effect.
[0111] [Example 10] 11. Preparation of hair growth cosmetics Simoncolite nanocrystalline slurry obtained in Test 5-8 of Example 5: 12.5% by weight, Ethanol: 5% by weight, Dipropylene glycol: 10% by weight, Propylene glycol-10 methyl glucose: 2% by weight, Butylene glycol: 20% by weight, Bisglyceryl ascorbate: 1% by weight, 1,2-Hexanediol: 1% by weight, Glycine: 1% by weight, Arginine: 1% by weight, Glycerin: 0.5% by weight, Hydrate Roxyethylcellulose: 0.5% by weight, Dextran: 0.5% by weight, Phenoxyethanol: 0.5% by weight, Yuzu fruit extract: 0.2% by weight, Rehmannia glutinosa root extract: 0.2% by weight, Acetyl tetrapeptide-3: 0.2% by weight, Trifolium pratense flower extract: 0.2% by weight, Biotin: 0.2% by weight, Riboflavin: 0.2% by weight, Pyridoxine HCl: 0.2% by weight, Dipotassium glycyrrhizate: 0.2% by weight Sodium acetylated hyaluronate: 0.2% by weight, Hydrolyzed elastin: 0.2% by weight, Cholesterol: 0.2% by weight, PEG-40 Hydrogenated Castor Oil: 0.2% by weight, Polyglyceryl-10 Myristate: 0.2% by weight, Diphenyl Dimethicone: 0.2% by weight, Bergamot Fruit Oil: 0.05% by weight, Frankincense Oil: 0.05% by weight, Lime Juice: 0.05% by weight, Orange Juice: 0.05% by weight, Lemon Juice: Mixing 0.05% by weight of hawthorn extract, 0.05% by weight of jujube fruit extract, 0.05% by weight of grapefruit fruit extract, 0.05% by weight of apple fruit extract, and the remainder with water, a slightly viscous, refreshing, slightly peach-white suspension hair growth lotion was obtained (component content as simoncolite nanocrystals in the lotion: 2% by weight, component content of polyethylene glycol 6000: 0.2% by weight).
[0112] The present invention is not limited to the embodiments or examples described above, and its technical scope also includes various design modifications that do not depart from the gist of the invention as described in the claims. [Industrial applicability]
[0113] The hair growth cosmetic, cosmetic raw materials, and cosmetic products of the present invention have excellent hair growth effects, as well as superior usability, ease of handling, and stability, and are therefore widely used in the fields of beauty and hair care.
Claims
1. A hair growth cosmetic containing simoncolite crystals as an active ingredient, The simoncolite crystal is a hair growth cosmetic characterized by being a nanoparticle with a 90% cumulative particle size (D90) of 800 nm or less in the volume-based particle size distribution measured by laser diffraction scattering.
2. The hair growth cosmetic composition according to claim 1, characterized in that the amount of simoncolite crystals included is 0.001% by weight to 10% by weight.
3. Furthermore, it contains a dispersion medium and a dispersant, The hair growth cosmetic composition according to claim 1 or 2, characterized in that the dispersant is at least one compound selected from the group consisting of polyethylene glycol, polypropylene glycol, ethylene oxide / propylene oxide copolymer, hydroxypropyl cellulose, hydroxypropyl methylcellulose, and hydroxyethyl cellulose.
4. A cosmetic ingredient or cosmetic characterized by containing nanoparticles of simoncolite crystals.
5. The nanoparticles of the simoncolite crystal have a 90% cumulative particle size (D) in the volume-based particle size distribution measured by laser diffraction scattering. 90 The cosmetic raw material or cosmetic according to claim 4, characterized in that the wavelength is 800 nm or less.
6. The nanoparticles of the simoncolite crystal have a 50% cumulative particle size (D) in the volume-based particle size distribution measured by laser diffraction scattering. 50 The cosmetic raw material or cosmetic according to claim 4, characterized in that the n is 250 nm or less.
7. Furthermore, the cosmetic raw material or cosmetic according to any one of claims 4 to 6 is characterized by containing water, a water-miscible organic solvent, or a combination thereof as a dispersion medium.
8. Furthermore, the cosmetic raw material or cosmetic according to claim 7, characterized in that it contains a dispersant.
9. The cosmetic raw material or cosmetic according to claim 8, characterized in that the dispersant is at least one compound selected from the group consisting of polyethylene glycol, polypropylene glycol, ethylene oxide / propylene oxide copolymer, hydroxypropyl cellulose, hydroxypropyl methylcellulose, and hydroxyethylcellulose.
10. The cosmetic raw material or cosmetic according to any one of claims 4 to 6, characterized in that the amount of simoncolite crystals blended is 0.001% by weight to 30% by weight.
11. A cosmetic ingredient or cosmetic according to any one of claims 4 to 6, characterized in that it is for hair growth or scalp care.
12. A mixing step to obtain a suspension by mixing simoncolite crystals and a dispersion medium, A stirring step of stirring the suspension for one hour or more, A method for producing a cosmetic raw material or cosmetic, characterized by comprising a micronization step of introducing the suspension after the stirring step into a micronization device and micronizing the simoncolite crystals contained in the suspension to a nanoscale size.
13. The method for producing a cosmetic raw material or cosmetic according to claim 12, characterized in that a dispersant is further mixed into the suspension in the mixing step or the stirring step.
14. A mixing step to obtain a suspension by mixing simoncolite crystals with a dispersion medium having a water-miscible organic solvent, A micronization process is performed by introducing the suspension into an atomizing device and micronizing the simoncolite crystals contained in the suspension to a nanoscale size. A method for producing a raw material for cosmetics or a cosmetic product, characterized by comprising the step of distilling off the water-miscible organic solvent contained in the suspension after the micronization treatment.
15. The method for producing a cosmetic raw material or cosmetic according to claim 14, characterized in that a dispersant is further mixed in the mixing step to obtain a suspension.
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