US20030072805A1 - Microgel and external compositions containing the same - Google Patents
Microgel and external compositions containing the same Download PDFInfo
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- US20030072805A1 US20030072805A1 US09/936,317 US93631701A US2003072805A1 US 20030072805 A1 US20030072805 A1 US 20030072805A1 US 93631701 A US93631701 A US 93631701A US 2003072805 A1 US2003072805 A1 US 2003072805A1
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- gel
- microgel
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
- A61K8/04—Dispersions; Emulsions
- A61K8/042—Gels
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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- A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
- A61K47/30—Macromolecular organic or inorganic compounds, e.g. inorganic polyphosphates
- A61K47/36—Polysaccharides; Derivatives thereof, e.g. gums, starch, alginate, dextrin, hyaluronic acid, chitosan, inulin, agar or pectin
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- A—HUMAN NECESSITIES
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- A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
- A61K47/30—Macromolecular organic or inorganic compounds, e.g. inorganic polyphosphates
- A61K47/42—Proteins; Polypeptides; Degradation products thereof; Derivatives thereof, e.g. albumin, gelatin or zein
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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- A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
- A61K8/0212—Face masks
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- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
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- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/40—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing nitrogen
- A61K8/44—Aminocarboxylic acids or derivatives thereof, e.g. aminocarboxylic acids containing sulfur; Salts; Esters or N-acylated derivatives thereof
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/64—Proteins; Peptides; Derivatives or degradation products thereof
- A61K8/65—Collagen; Gelatin; Keratin; Derivatives or degradation products thereof
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- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/67—Vitamins
- A61K8/676—Ascorbic acid, i.e. vitamin C
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- A—HUMAN NECESSITIES
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- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
- A61K8/73—Polysaccharides
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- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
- A61K8/81—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
- A61K8/8141—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
- A61K8/8147—Homopolymers or copolymers of acids; Metal or ammonium salts thereof, e.g. crotonic acid, (meth)acrylic acid; Compositions of derivatives of such polymers
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- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
- A61K8/81—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
- A61K8/8141—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
- A61K8/8152—Homopolymers or copolymers of esters, e.g. (meth)acrylic acid esters; Compositions of derivatives of such polymers
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- A61K8/81—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
- A61K8/8141—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
- A61K8/8158—Homopolymers or copolymers of amides or imides, e.g. (meth) acrylamide; Compositions of derivatives of such polymers
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- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
- A61K8/84—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions otherwise than those involving only carbon-carbon unsaturated bonds
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- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
- A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
- A61K8/9783—Angiosperms [Magnoliophyta]
- A61K8/9789—Magnoliopsida [dicotyledons]
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- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
- A61K8/98—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution of animal origin
- A61K8/981—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution of animal origin of mammals or bird
- A61K8/982—Reproductive organs; Embryos, Eggs
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- A61K9/0014—Skin, i.e. galenical aspects of topical compositions
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- A61Q19/00—Preparations for care of the skin
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- A61Q19/00—Preparations for care of the skin
- A61Q19/02—Preparations for care of the skin for chemically bleaching or whitening the skin
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L5/00—Compositions of polysaccharides or of their derivatives not provided for in groups C08L1/00 or C08L3/00
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L5/00—Compositions of polysaccharides or of their derivatives not provided for in groups C08L1/00 or C08L3/00
- C08L5/04—Alginic acid; Derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L5/00—Compositions of polysaccharides or of their derivatives not provided for in groups C08L1/00 or C08L3/00
- C08L5/12—Agar or agar-agar, i.e. mixture of agarose and agaropectin; Derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L89/00—Compositions of proteins; Compositions of derivatives thereof
- C08L89/04—Products derived from waste materials, e.g. horn, hoof or hair
- C08L89/06—Products derived from waste materials, e.g. horn, hoof or hair derived from leather or skin, e.g. gelatin
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- A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
- A61K2800/41—Particular ingredients further characterized by their size
- A61K2800/412—Microsized, i.e. having sizes between 0.1 and 100 microns
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- A—HUMAN NECESSITIES
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- A61Q5/06—Preparations for styling the hair, e.g. by temporary shaping or colouring
- A61Q5/065—Preparations for temporary colouring the hair, e.g. direct dyes
Definitions
- the present invention relates to a viscosity control agent which is used mainly in the fields of, for example, cosmetic compositions and drugs.
- the present invention also relates to external compositions, such as cosmetic compositions, comprising the viscosity control agent.
- Conventionally known methods for increasing the viscosity of an external composition include a method for incorporating into the composition a viscosity control agent or a thickening agent; for example, a polysaccharide such as xanthan gum, a hydrophilic synthetic polymer such as a polyacrylic acid, or a clay mineral such as bentonite.
- a viscosity control agent or a thickening agent for example, a polysaccharide such as xanthan gum, a hydrophilic synthetic polymer such as a polyacrylic acid, or a clay mineral such as bentonite.
- the composition When a polysaccharide such as xanthan gum is incorporated, as a viscosity control agent, into an external composition, the composition involves problems in terms of sensation during use; for example, the composition provides a sticky sensation during use, although such a polysaccharide exhibits excellent stability in the composition into which a pharmaceutical ingredient or a salt is incorporated.
- a hydrophilic synthetic polymer such as polyacrylic acid
- the composition provides good sensation during use; i.e., the composition provides no sticky sensation during use, but provides a refreshing sensation during use.
- such a hydrophilic synthetic polymer has low resistance to a salt or an ionic substance.
- the composition when a large amount of a salt or a pharmaceutical ingredient such as a whitening ingredient; for example, L-ascorbic acid (i.e., vitamin C) or arbutin, is incorporated into the composition, the composition involves problems including lowering of the viscosity of the composition.
- a clay mineral such as bentonite is incorporated, as a viscosity control agent, into an external composition, the composition involves problems in terms of sensation during use; for example, the composition provides a frictional sensation during use.
- An object of the present invention is to provide a new type of viscosity control agent which, when incorporated as an ingredient into an external composition, imparts the composition with excellent sensation during use; i.e., free of sticky sensation or frictional sensation. Furthermore, even when a large amount of a salt or a pharmaceutical ingredient such as a whitening ingredient is incorporated into the composition, the viscosity of the composition is not lowered, the composition exhibits long-term stability, and separation of water does not occur. Another object of the present invention is to provide an external composition comprising the viscosity control agent.
- the present inventors have performed extensive studies in order to attain the aforementioned objects, and have found that, when a compound capable of forming a gel, such as agar which is conventionally used as a gelation agent, is formed into a gel, the resultant gel is pulverized into a microgel, and then the resultant microgel is incorporated, as a viscosity control agent, into an external composition, the composition provides no sticky sensation during use, and the viscosity of the composition is not lowered even when a large amount of pharmaceutical ingredient such as a whitening ingredient or large amounts of various salts are incorporated into the composition.
- the present invention has been accomplished on the basis of this finding.
- the present invention provides a microgel having a mean particle size of 0.1-1,000 ⁇ m, the microgel being produced from a gel which is formed by use of a hydrophilic compound capable of forming a gel (hereinafter the microgel may be referred to as “the present microgel”).
- the present microgel may be produced through a process comprising dissolving, in an aqueous solvent, a hydrophilic compound capable of forming a gel; forming a gel; and pulverizing the gel into a microgel having a mean particle size of 0.1-1,000 ⁇ m (hereinafter the process may be referred to as “the present production process”).
- the present invention also provides an external composition comprising the present microgel (hereinafter the composition may be referred to as “the present external composition”).
- the composition may be referred to as “the present external composition”.
- a salt or a pharmaceutical ingredient such as a whitening ingredient may be incorporated intentionally.
- the term “external composition” refers to a composition which is applied onto the skin (including the scalp and hair) .
- the composition can be used to prepare, for example, cosmetic compositions, hair-dyes, external drugs, and external quasi-drugs.
- hydrophilic compound capable of forming a gel which is used for producing the present microgel, so long as the compound is a water-soluble soluble compound capable of forming a gel and can be incorporated into an external composition.
- the hydrophilic compound include hydrophilic proteins capable of forming a gel, such as gelatin and collagen; and hydrophilic polysaccharides such as agar, curdlan, scleroglucan, schizophyllan, gellan gum, alginic acid, carrageenan, mannan, pectin, and hyaluronic acid.
- gelatin agar, curdlan, gellan gum, alginic acid, or carrageenan is particularly preferred, since such a compound is not easily affected by a salt or an ionic substance in the composition, and enables to provide a stable gel.
- gel-formable hydrophilic compounds may be used.
- the present microgel may be produced through, for example, the below-described process (i.e., the present production process).
- any of the aforementioned hydrophilic compounds capable of forming a gel is dissolved in an aqueous solvent such as water, and is allowed to form a gel.
- the hydrophilic compound may be dissolved in an aqueous solvent through a customary method; for example, through mixing or heating.
- Gelation (solidification) is preferably carried out by stopping heating of the resultant mixture after dissolving, and then allowing the mixture to stand still until the temperature of the mixture becomes lower than the gelation temperature (solidification temperature).
- the aqueous solvent is not particularly limited, so long as the solvent can be incorporated into an external composition.
- the aqueous solvent include water; glycols such as 1,3-butylene glycol and propylene glycol; and lower alcohols such as ethanol and propanol.
- One or more of such aqueous solvents may be used.
- Water or a mixture of water and another aqueous solvent is preferably used.
- the aqueous solvent may contain a water-soluble ingredient other than the aqueous solvent, which ingredient can be incorporated into an external composition.
- a water-soluble ingredient include, but are not limited to, chelating agents such as metaphosphates and edetates; pH-adjusting agents; preservatives; water-soluble pharmaceutical ingredients; and salts.
- the gel strength of the aforementioned gel is not particularly limited, so long as the gel can maintain its shape and the gel can be subjected to the subsequent procedure to thereby form a microgel.
- a gel having a very high gel strength for example, a gel having a high jelly strength (as measured according to the official method of Japanese Association of Agar) of up to 1,000 g/cm 2 or thereabouts, can be used.
- a gel having a very low jelly strength i.e., a jelly strength of 30 g/cm 2 or thereabouts
- a gel having a jelly strength of 100 g/cm 2 or thereabouts is preferred.
- a viscosity increasing compound incapable of forming a gel may be incorporated into the present external composition in addition to the aforementioned hydrophilic compound capable of forming a gel.
- hydrophilic viscosity increasing compounds including hydrophilic synthetic polymers such as polyacrylic acid, polyethylene glycol, polyacrylamide, polyalkylacrylamide/polyacrylamide copolymers, carboxymethyl cellulose, cationized cellulose, and pluronic; hydrophilic naturally-occurring polymers such as xanthan gum, succinoglycan, guar gum, and locust bean gum; and hydrophilic clay minerals such as laponite, bentonite, and smectite.
- the gel strength of the resultant gel can be arbitrarily regulated.
- the viscosity increasing compound incapable of forming a gel is particularly preferably xanthan gum, succinoglycan, polyacrylic acid, polyethylene glycol, polyacrylamide, or a polyalkylacrylamide/polyacrylamide copolymer.
- a salt of the viscosity increasing compound is also preferably used.
- One or more of the viscosity increasing compounds incapable of forming a gel may be used.
- the incorporation amount of the hydrophilic viscosity increasing compound incapable of forming a gel varies with intended use of the resultant viscosity control agent.
- the viscosity increasing compound incapable of forming a gel may be incorporated in an amount of about 1-100 mass % based upon the hydrophilic compound capable of forming a gel.
- the gel formed as described above is pulverized (crushed) by means of, for example, a homogenizer, a high speed mixer, or a mechanical stirrer, to thereby obtain a desired microgel.
- the mean particles size of the microgel is preferably about 0.1-1,000 ⁇ m, more preferably about 1-300 ⁇ m, much more preferably about 10-200 ⁇ m.
- the degree of pulverization of the gel may be regulated in accordance with use of the microgel. When the microgel is required to have a smooth sensation during use, the gel is sufficiently pulverized through high-speed stirring, to thereby obtain a microgel having a very small particle size. When an intrinsic tactile sensation of the microgel is required, the degree of pulverization of the gel is decreased through low-speed or brief stirring, to thereby obtain a microgel having a slightly large particle size.
- the viscosity of the thus-obtained microgel varies in accordance with use or need of the microgel.
- the viscosity of the resultant microgel (agar content: about 0.5-2%) is preferably about 2,000-1,000,000 mPa ⁇ s, the viscosity being measured by use of a B-type viscometer (revolution number: 0.6 rpm, at 25° C.).
- the microgel produced by the present invention is incorporated, as a viscosity control agent, into an external composition, improvement of sensation during use of the composition (i.e., suppression of a sticky sensation during use) can be attained.
- a pharmaceutical ingredient, salt, etc. is incorporated into the external composition in a large amount; for example, in an amount of about 20 mass % of the total of the composition, the viscosity of the composition is not lowered; i.e., the viscosity of the composition can be maintained.
- the composition exhibits long-term stability, and separation of water does not occur.
- the amount of a pharmaceutical ingredient or a salt incorporated into the composition is preferably about 0.1 mass % or more of the total of the composition, in order to obtain the intended effects of incorporation of such an ingredient.
- the present external composition may contain a water-soluble or oil-soluble pharmaceutical ingredient or salt.
- a pharmaceutical ingredient is incorporated into the external composition in order to impart effective pharmaceutical activity to the composition.
- Most pharmaceutical ingredients have a variety of active groups, and assume a salt form. Therefore, when a large amount of such a pharmaceutical ingredient is incorporated into the composition, the stability of a composition may be impaired.
- Examples of the pharmaceutical ingredient which may be incorporated into the composition include vitamins, anti-inflammatory agents, antibacterial agents, and whitening ingredients.
- the pharmaceutical ingredient include vitamins and derivatives thereof, such as vitamin B, vitamin P, water-soluble vitamin A, and water-soluble vitamin D; pantothenyl ethyl ether; calcium pantothenate; glycyrrhizic acid; glycyrrhizinates; glycyrrhetic acid; glycyrrhetinates; royal jelly; polyphenol; nicotinic acid and derivatives thereof (e.g., nicotinamide); resorcin; sulfur; salicylic acid and derivative thereof; urea; xylitol; trehalose; and caffeine.
- vitamins and derivatives thereof such as vitamin B, vitamin P, water-soluble vitamin A, and water-soluble vitamin D
- pantothenyl ethyl ether pantothenate
- glycyrrhizic acid glycyrrhizinates
- glycyrrhetic acid glycyr
- Preferred examples of the whitening ingredient include L-ascorbic acid and derivatives thereof; arbutin; glutathione; tranexamic acid and derivatives thereof; placenta extract; and vegetable extracts exhibiting whitening effects (e.g., chamomile extract, Scutellaria root extract, and Saxifraga extract).
- L-ascorbic acid is generally called “vitamin C,” exhibits cell respiration effects, enzyme activation effects, and collagen formation effects, due to its strong reducing effects, and exhibits melanin-reducing effects.
- L-ascorbic acid derivatives include L-ascorbic acid monoalkyl esters such as L-ascorbyl monostearate, L-ascorbyl monopalmitate, and L-ascorbyl monooleate; L-ascorbic acid monoesters such as L-ascorbyl monophosphate and L-ascorbyl-2-sulfate; L-ascorbic acid dialkyl esters such as L-ascorbyl distearate, L-ascorbyl dipalmitate, and L-ascorbyl dioleate; L-ascorbic acid diesters such as L-ascorbyl diphosphate; L-ascorbic acid trialkyl esters such as L-ascorbyl tristearate, L
- L-ascorbic acid L-ascorbic acid, L-ascorbyl phosphate, L-ascorbyl-2-sulfate, L-ascorbic acid 2-glucoside, or a salt thereof is preferably used.
- tranexamic acid derivatives include dimers of tranexamic acid (e.g., trans-4-(trans-aminomethylcyclohexanecarbonyl) aminomethylcyclohexanecarboxylic acid hydrochloride); esters of tranexamic acid and hydroquinone (e.g., 4′-hydroxyphenyl trans-4-aminomethylcyclohexanecarboxylate); esters of tranexamic acid and gentisic acid (e.g., 2-(trans-4-aminomethylcyclohexylcarbonyloxy)-5-hydroxybenzoic acid and salts thereof); and amides of tranexamic acid (e.g., trans-4-aminomethylcyclohexanecarboxylic acid methylamide and salts thereof, trans-4-(P-methoxybenzoyl) aminomethylcyclohexanecarboxylic acid and salts thereof, and trans-4-guanidinomethylcyclohexan
- one or more of the whitening ingredients may be used.
- the amount of the whitening ingredient incorporated into the present external composition is preferably about 0.1-20 mass %, more preferably about 0.5-5 mass %, of the total of the composition.
- Examples of salts include a variety of pharmaceutically acceptable organic acid salts, amino acid salts, and inorganic salts.
- organic acid salts include hydrochlorides, metallic salts (e.g., sodium salts and potassium salts), and amine salts of organic acids such as citric acid, lactic acid, oxalic acid, and sulfonic acid.
- the amino acid salts include hydrochlorides, metallic salts (e.g., sodium salts and potassium salts), and amine salts of amino acids such as glycine, alanine, proline, lysine, aspartic acid, and glutamic acid.
- inorganic salts include sodium salts, potassium salts, magnesium salts, calcium salts, carbonates, phosphates, nitrates, borates, sulfates, sulfites, and halogen compounds (e.g., sodium chloride and potassium chloride).
- the present external composition exhibits excellent resistance to a salt. Therefore, even when a large amount of the aforementioned salt or a salt of the aforementioned pharmaceutical ingredient is incorporated into the composition, the stability of the composition is not impaired, and the composition provides an excellent sensation during use as described above.
- a compound capable of forming a gel such as agar, carrageenan, curdlan, or gelatin
- a viscosity control agent has been used as a viscosity control agent.
- such a compound is heated and dissolved in an external composition, and the resultant mixture is gradually cooled under stirring, to thereby obtain a viscous composition without solidification (gelation) of the compound (e.g., Japanese Patent Application Laid-Open (kokai) No. 11-209262).
- the external composition containing the compound capable of forming a gel is gradually cooled under stirring as described in the conventional method, to thereby increase the viscosity of the composition, the degree of increase in the viscosity of the composition is limited.
- a pharmaceutical ingredient or a salt is incorporated into the external composition, the viscosity of the composition is prone to decrease.
- the gelled compound is pulverized into a microgel, and the resultant microgel is used as a viscosity control agent.
- the present microgel obtained as described above differs from a polysaccharide viscosity control agent or a synthetic polymer viscosity control agent which is conventionally used in an external composition such as a cosmetic composition, in that the present microgel exerts the viscosity increasing effect not through entanglement of molecules but through friction of the microgel particles yielded from pulverization of the gel.
- the present microgel does not exhibit spinnability that is unique to polymer solutions, and an external composition containing the microgel provides a very refreshing sensation during use. Also, as contrasted to polymer solutions, which in some cases are affected by a pharmaceutical ingredient or salt incorporated therein to thereby lower the viscosity and impose limitations on incorporation of the pharmaceutical ingredient or salt, the present invention is free from such problems, permitting a variety of external compositions, including cosmetic compositions, to be formulated.
- a water-soluble pharmaceutical ingredient or salt when a water-soluble pharmaceutical ingredient or salt is used, after the aforementioned hydrophilic ingredient capable of forming a gel is dissolved in an aqueous solvent, the resultant mixture is allowed to stand and cool, for example, to thereby form a gel, and subsequently, a microgel obtained by pulverizing the resultant gel may be mixed with the pharmaceutical ingredient or salt.
- the resultant mixture is allowed to stand and cool, for example, to thereby form a gel, and subsequently the resultant gel may be pulverized into a microgel.
- the resultant mixture is allowed to stand and cool, for example, to thereby form a gel, and subsequently, the resultant gel may be pulverized into a microgel.
- the oil-soluble pharmaceutical ingredient or salt and another oil ingredient are preferably preliminarily emulsified in an aqueous system, and the resultant emulsion is mixed with the above-obtained microgel, and the resultant mixture is emulsified.
- the present external composition containing the present microgel may appropriately contain an ingredient which is generally incorporated into an external composition such as a cosmetic composition, such as a humectant, a preservative, powder, a colorant, a perfume, or a pH-adjusting agent, so long as the ingredient does not impede the purposes and the effects of the present invention.
- a cosmetic composition such as a humectant, a preservative, powder, a colorant, a perfume, or a pH-adjusting agent
- the present microgel may be incorporated into an aqueous external composition, or, similar to the case of a usual polymer viscosity control agent, may be incorporated into an emulsified external composition such as a milky lotion or a cream.
- the present microgel may be incorporated into an external composition even when the product form of the composition is a hair-setting agent, a hair cream, a body-care product, or hair dye.
- the present microgel is incorporated into an acidic hair dye, the stability, the adhesive property, and the usability of the hair dye can be enhanced.
- the present microgel per se can be used as a gel-type external composition.
- Examples 1 through 10 A hydrophilic compound capable of forming a gel and a viscosity increasing compound incapable of forming a gel were added to water, mixed, heated to 90° C., dissolved, and then allowed to stand at room temperature, to thereby form a gel. Subsequently, the gel was pulverized with a homogenizer, to thereby yield a microgel having a mean particle size of 100 ⁇ m. The microgel was mixed with the remaining ingredients, and the resultant mixture was stirred, to thereby yield the external compositions of Examples 1 through 10.
- Comparative Examples 1 through 4 The ingredients were mixed, and then allowed to stand for 12 hours at room temperature, to thereby yield external compositions of Comparative Examples 1 through 4.
- the viscosity of the above-obtained sample was measured by use of a B-type viscometer (number of revolution: 0.6 rpm, at 25° C.), to thereby evaluate the viscosity increasing property of the sample.
- A very excellent viscosity increasing property (viscosity: 50,000 mPa ⁇ s or more)
- C poor viscosity increasing property (viscosity: 500 to 5,000 mPa ⁇ s)
- the present external composition containing the present microgel contains a large amount of a whitening ingredient, the viscosity of the composition is not lowered.
- the present external composition exhibits excellent viscosity increasing property, provides good sensation during use; i.e., provides no sticky sensation during use, and exhibits excellent whitening effect and long-term stability.
- an external composition of each of Examples 11 through 24 was prepared in manner similar to that of the external composition of each of Examples 1 through 10, and an external composition of each of Comparative Examples 5 through 11 was prepared in manner similar to that of the external composition of each of Comparative Examples 1 through 4.
- Examples 25 and 26 Ingredients were mixed, heated to 90° C., dissolved, and then allowed to stand at room temperature, to thereby form a gel. The gel was pulverized with a homogenizer, to thereby yield a microgel (mean particle size: 100 ⁇ m).
- Comparative Examples 12 and 13 Ingredients were mixed at 90° C., heating of the resultant mixture was stopped, and then the mixture was allowed to stand at room temperature.
- Viscosity increasing agent A 50 mass %), ascorbic acid 2-glucoside (2 mass %), and emulsion part A (48 mass %) were mixed under stirring for emulsification, to thereby yield an O/W cream of Example 27.
- compositional system which contains a pharmaceutical ingredient (whitening ingredient) and which fails to be thickened by a conventional viscosity control agent can be successfully thickened by the addition of the microgel of the present invention.
- ingredients (9), (10), and (12) through (16) were dissolved at 90° C., and subsequently, the resultant mixture was cooled to form a gel.
- the thus-obtained gel was thoroughly pulverized with a homogenizing mixer, to thereby yield a microgel (mean particle size: 70 ⁇ m)
- the microgel was added to the above-prepared emulsion part, and the resultant mixture was subjected to stirring, deaeration, filtration, and cooling, to thereby yield a massage cream (O/W).
- Viscosity increasing agent A prepared in Example 27 (48 mass %), NaCl (2 mass %), and emulsion part A prepared in Example 27 (48 mass %) were mixed under stirring for emulsification, to thereby yield an O/W cream of Example 33.
- the viscosity (25° C.) of each of the O/W creams prepared in Example 33 and Comparative Example 15 was measured by use of a B-type viscometer.
- the viscosity of the O/W cream of Example 33 and that of Comparative Example 15 were found to be 400,000 mPa ⁇ s and 18,000 mPa ⁇ s, respectively.
- Ingredient (1) was dispersed in a mixture consisting of ingredient (3) and a portion of ingredient (12) so as to form a dispersion.
- Ingredient (2), a portion of ingredient (4), ingredient (6), and ingredients (9) through (11) were dissolved in the remaining portion of ingredient (12), and the resultant mixture was added to the above-prepared dispersion, yielding a mixed solution.
- Ingredient (7) was dissolved in the remaining portion of (4), ingredient (8) was added thereto and dissolved therein, and the mixture was neutralized with ingredient (5).
- the resultant neutral solution was added to the aforementioned mixed solution, and heated at 80° C. for 10 minutes. Subsequently, the formed gel was subjected to pulverizing with a homogenizer (mean particle size: 80 ⁇ m), filtration, deaeration, and cooling, to thereby yield a hair-setting gel.
- a homogenizer mean particle size: 80 ⁇ m
- an emulsified product which had been prepared through addition of ingredient (11) to a homogeneously dispersed mixture of ingredients (7) through (9), and (13) in the remaining portion of ingredient (1) followed by a treatment with a homogenizing mixer to obtain a homogeous emulsion was added, and subsequently, the thus-obtained mixture was subjected to homogeneous dispersion, to thereby yield a moisturizing cream.
- Agent 1 Ethanol and benzyl alcohol were mixed with purified water. To the resultant mixture, glycolic acid and sodium lactate were dissolved, and the colorant was added thereto and caused to dissolve, to thereby yield an agent 1.
- Agent 2 Agar was dissolved in purified water (75° C.). Methylparaben and ethanol were added to the resultant solution, and the mixture was allowed to stand for 12 hours at room temperature. The thus-solidified agar gel was pulverized with a high speed mixer (mean particle size: 70 ⁇ m, to thereby yield an agent 2 (an agar microgel).
- the acid hair dye prepared from mixing the agents 1 and 2 was found to exhibit satisfactory viscosity stability and adhesion, and was also found to have excellent sensation during use.
- Agar was dissolved in a portion of purified water (75° C.). The solution was allowed to cool to 60° C., followed by addition of 1,3-butylene glycol, benzyl alcohol, glycolic acid, and hydroxyethylcellulose thereto. The mixture was caused to dissolve, and subsequently the resultant solution was allowed to stand for 12 hours at room temperature. The solidified agar gel was pulverized with a high speed mixer until a microgel having a mean particle size of 50 ⁇ m was yielded.
- the acid hair dye prepared in Example 46 was found to exhibit high viscosity stability and adhesion, and was found to be endowed with excellent sensation during use.
- the microgel of the present invention does not exhibit even slightest spinnability, which is unique to polymer solutions conventionally used as viscosity control agents, and an external composition containing the microgel provides a very refreshing sensation during use.
- polymer solutions may in some cases be affected by a pharmaceutical ingredient or salt incorporated therein, to thereby cause a reduced viscosity and limitation in terms of pharmaceutical ingredients or salts which can be incorporated, the microgel of the present invention does not involve such problems, and a broad range of external compositions, including cosmetic compositions, can be prepared by use of the microgel.
Priority Applications (1)
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US12/082,130 US8367082B2 (en) | 2000-01-11 | 2008-04-09 | Microgel and external compositions containing the same |
Applications Claiming Priority (8)
Application Number | Priority Date | Filing Date | Title |
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JP2000-2611 | 2000-01-11 | ||
JP2000002610 | 2000-01-11 | ||
JP2000002611 | 2000-01-11 | ||
JP2000-2610 | 2000-03-30 | ||
JP2000-94308 | 2000-03-30 | ||
JP2000094308 | 2000-03-30 | ||
JP2000-94307 | 2000-03-30 | ||
JP2000094307 | 2000-03-30 |
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US12/082,130 Continuation US8367082B2 (en) | 2000-01-11 | 2008-04-09 | Microgel and external compositions containing the same |
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US20030072805A1 true US20030072805A1 (en) | 2003-04-17 |
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US12/082,130 Expired - Lifetime US8367082B2 (en) | 2000-01-11 | 2008-04-09 | Microgel and external compositions containing the same |
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US12/082,130 Expired - Lifetime US8367082B2 (en) | 2000-01-11 | 2008-04-09 | Microgel and external compositions containing the same |
Country Status (5)
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---|---|
US (2) | US20030072805A1 (fr) |
EP (1) | EP1158021B1 (fr) |
KR (1) | KR20010102550A (fr) |
TW (1) | TWI279416B (fr) |
WO (1) | WO2001051558A1 (fr) |
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Also Published As
Publication number | Publication date |
---|---|
TWI279416B (en) | 2007-04-21 |
US20090047312A1 (en) | 2009-02-19 |
EP1158021B1 (fr) | 2011-10-05 |
EP1158021A4 (fr) | 2006-04-12 |
KR20010102550A (ko) | 2001-11-15 |
EP1158021A1 (fr) | 2001-11-28 |
WO2001051558A1 (fr) | 2001-07-19 |
US8367082B2 (en) | 2013-02-05 |
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