WO2022074798A1 - 固形状組成物 - Google Patents

固形状組成物 Download PDF

Info

Publication number
WO2022074798A1
WO2022074798A1 PCT/JP2020/038183 JP2020038183W WO2022074798A1 WO 2022074798 A1 WO2022074798 A1 WO 2022074798A1 JP 2020038183 W JP2020038183 W JP 2020038183W WO 2022074798 A1 WO2022074798 A1 WO 2022074798A1
Authority
WO
WIPO (PCT)
Prior art keywords
mass
component
solid composition
less
chlorogenic acids
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/JP2020/038183
Other languages
English (en)
French (fr)
Japanese (ja)
Inventor
祐佳 江野口
陽子 杉浦
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Kao Corp
Original Assignee
Kao Corp
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Kao Corp filed Critical Kao Corp
Priority to JP2022555207A priority Critical patent/JP7727653B2/ja
Priority to PCT/JP2020/038183 priority patent/WO2022074798A1/ja
Publication of WO2022074798A1 publication Critical patent/WO2022074798A1/ja
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

Links

Classifications

    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES, NOT OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF
    • A23L33/00Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
    • A23L33/10Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
    • A23L33/105Plant extracts, their artificial duplicates or their derivatives
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES, NOT OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF
    • A23L33/00Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
    • A23L33/10Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
    • A23L33/17Amino acids, peptides or proteins
    • A23L33/175Amino acids
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K31/00Medicinal preparations containing organic active ingredients
    • A61K31/185Acids; Anhydrides, halides or salts thereof, e.g. sulfur acids, imidic, hydrazonic or hydroximic acids
    • A61K31/19Carboxylic acids, e.g. valproic acid
    • A61K31/195Carboxylic acids, e.g. valproic acid having an amino group
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K31/00Medicinal preparations containing organic active ingredients
    • A61K31/70Carbohydrates; Sugars; Derivatives thereof
    • A61K31/7028Compounds having saccharide radicals attached to non-saccharide compounds by glycosidic linkages
    • A61K31/7032Compounds having saccharide radicals attached to non-saccharide compounds by glycosidic linkages attached to a polyol, i.e. compounds having two or more free or esterified hydroxy groups, including the hydroxy group involved in the glycosidic linkage, e.g. monoglucosyldiacylglycerides, lactobionic acid, gangliosides
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00Medicinal preparations characterised by special physical form
    • A61K9/14Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00Medicinal preparations characterised by special physical form
    • A61K9/20Pills, tablets, discs, rods

Definitions

  • the present invention relates to a solid composition.
  • Chlorogenic acids are one of the polyphenols found in green coffee beans. As the physiological action of chlorogenic acids, an autonomic nerve function improving action, an indefinite complaint improving action and the like have been reported (Patent Document 1).
  • GABA gamma-aminobutyric acid
  • ⁇ -Aminobutyric acid is also contained not only in mammals but also in a wide range of organisms including other animals and plants.
  • ⁇ -Aminobutyric acid is known to have a high tranquilizing effect, and has been reported to be effective against insomnia, depression, and irritability during menopause or presenile age (Non-Patent Document 1).
  • Patent Document 2 describes tablets and granules containing a ⁇ -aminobutyric acid-containing coffee bean extract prepared from a hot water extract of Rubiaceae coffee beans. It was
  • Patent Document 1 Japanese Patent Application Laid-Open No. 2002-145765
  • Patent Document 2 Japanese Patent Application Laid-Open No. 2010-187554
  • Non-Patent Document 1 Food and Development, 2001, 36 (6): 4-6
  • the present invention contains chlorogenic acids (A) and ⁇ -aminobutyric acid (B) of 0.5% by mass or more, and the content ratio of the component (A) to the component (B) is 100: 0. It provides a solid composition which is 7 to 140.
  • the present invention relates to a solid composition containing chlorogenic acids and ⁇ -aminobutyric acid, which has improved solubility in water and suppressed hygroscopicity.
  • the solid composition of the present invention contains chlorogenic acids (A).
  • chlorogenic acids in the present specification refer to monocafe oil quinic acid of 3-cafe oil quinic acid, 4-cafe oil quinic acid and 5-cafe oil quinic acid, and 3-ferloyl quinic acid, 4 -A generic term for ferroylquinic acid and monoferloylquinic acid 5-ferloylquinic acid.
  • at least one of the above six types may be contained.
  • the chlorogenic acids include stereoisomers and analogs, and include pure stereoisomers, analogs or mixtures thereof.
  • chlorogenic acids (A) may be referred to as "component (A)" in the present specification.
  • the component (A) may be in the form of a salt or a hydrate.
  • the salt is preferably a pharmaceutically acceptable salt.
  • the salt include salts with alkali metals such as lithium, sodium and potassium; salts with alkaline earth metals such as magnesium and calcium; salts of inorganic bases such as ammonium salts; arginine, lysine, histidine, ornithine and the like. Salts with basic amino acids; salts with organic bases such as monoethanolamine, diethanolamine, triethanolamine and the like. Of these, salts with alkali metals or alkaline earth metals are preferable.
  • a commercially available reagent may be used, but a plant extract containing chlorogenic acids can also be used.
  • the plant is not particularly limited as long as it contains chlorogenic acids, but for example, sunflower seeds, immature apple fruits, coffee beans, simon leaves, Pinaceae bulbs, Pinaceae seed husks, sugar cane, and southern heavens.
  • One or more species selected from leaves, gobos, eggplant skins, plum fruits, fuquitan popo, pinaceae plants and the like can be mentioned.
  • coffee beans are preferable from the viewpoint of the content of chlorogenic acids and the like.
  • the bean seeds and production areas of coffee beans are not particularly limited.
  • the coffee beans may be raw coffee beans or roasted coffee beans, and these can be used in combination.
  • the roasted coffee beans are preferably lightly roasted coffee beans from the viewpoint of the content of chlorogenic acids.
  • the range of the L value of the lightly roasted coffee beans is preferably 27 or more, more preferably 29 or more, further preferably 35 or more, and preferably less than 62 from the viewpoint of the content of chlorogenic acids. , 60 or less is more preferable, and 55 or less is further preferable.
  • the range of the L value of the lightly roasted coffee beans is preferably 27 or more and less than 62, more preferably 29 or more and 60 or less, and further preferably 35 or more and 55 or less.
  • the "L value” in the present specification means that black is L value 0 and white is L value 100, and the brightness of roasted coffee beans is crushed and then a colorimeter (for example, Spectrophotometer SE2000, Co., Ltd.). ) Measured by Nippon Denshoku Co., Ltd.). The coffee beans attached to the extraction may be uncrushed or crushed.
  • the extraction method and extraction conditions can be appropriately selected, and can be carried out by known methods such as batch extraction, drip extraction, and column extraction using water, hot water, or a water-soluble organic solvent.
  • the water-soluble organic solvent include lower alcohols such as ethanol.
  • the extraction method for example, the methods described in JP-A-58-138347, JP-A-59-51763, JP-A-62-111671, and JP-A-5-236918 can be adopted.
  • the purification method is not particularly limited, and a known method can be adopted. For example, one type or a combination of two or more types of various chromatographies such as ion chromatography, molecular sieving chromatography, and reverse phase chromatography can be adopted. Can be done.
  • the obtained extract may be concentrated by known means such as atmospheric pressure concentration, vacuum concentration concentration, membrane concentration, etc., or the extract or concentrate may be dried. Drying can be performed by known means such as spray drying and freeze drying.
  • the form of the reagent of the component (A) and the plant extract containing the component (A) is solid (powder, granule, etc.) at room temperature (25 ° C.).
  • the content of the component (A) in the coffee bean extract is preferably 10% by mass or more, more preferably 15% by mass or more, and preferably 70% by mass or less, based on the total amount. More preferably, it is 60% by mass or less.
  • the coffee bean extract is preferably decaffeinated.
  • the mass ratio of caffeine / chlorogenic acids in the coffee bean extract is preferably 0.015 or less, more preferably 0.014 or less, still more preferably 0.010 or less, still more preferably 0.0066 or less, still more preferably 0. It is 0050 or less, more preferably 0.0020 or less, still more preferably 0.0005 or less.
  • the mass ratio of chlorogenic acids / caffeine in the coffee bean extract is preferably 65 or more, more preferably 70 or more, still more preferably 100 or more, still more preferably 150 or more, still more preferably 200 or more, still more preferably. It is 500 or more, more preferably 2000 or more.
  • the content of caffeine in the coffee bean extract is preferably 0.5% by mass or less, more preferably 0.4% by mass or less, still more preferably 0.3% by mass, based on the total amount from the viewpoint of physiological effects. Below, it is more preferably 0.2% by mass or less, further preferably 0.15% by mass or less, still more preferably 0.1% by mass or less, still more preferably 0.05% by mass or less, still more preferably the coffee.
  • the bean extract is substantially free of caffeine (eg, below the detection limit of HPLC).
  • the analysis of chlorogenic acids and caffeine shall follow the methods described in the Examples below. In the present specification, the contents of chlorogenic acids and caffeine in the coffee bean extract refer to their mass ratios in the dried coffee bean extract.
  • a method of subjecting decaffeinated coffee beans to an extraction step and a method of subjecting a coffee bean extract or a concentrate thereof to a decaffeination treatment can be mentioned.
  • a method of decaffeinating the coffee bean extract or its concentrate is preferable.
  • the coffee bean extract or its concentrate is dissolved in a mixed solution of water and an organic solvent, and then activated charcoal and / or activated clay or clay is used. It is preferable to bring it into contact with acid clay.
  • the method described in Japanese Patent Application Laid-Open No. 2011-4766 can be adopted.
  • a commercially available product may be used as the extract of coffee beans or a concentrate thereof to be subjected to the decaffeination treatment.
  • the decaffeinated coffee beans are coffee beans that have been decaffeinated.
  • a known method can be adopted, and examples thereof include a water method, a supercritical carbon dioxide extraction method, and an organic solvent extraction method.
  • the content of the component (A) is preferably 1% by mass or more, more preferably 2% by mass or more from the viewpoint of physiological activity and reduction of hygroscopicity of the solid composition. , More preferably 3% by mass or more, further preferably 5% by mass or more, and from the viewpoint of processing, preferably 99.5% by mass or less, more preferably 98% by mass or less, still more preferably 97% by mass. Below, it is more preferably 95% by mass or less.
  • the content of the component (A) in the solid composition is preferably 1 to 99.5% by mass, more preferably 2 to 98% by mass, more preferably 3 to 97% by mass, still more preferably 5 to 95% by mass. %.
  • the content of the component (A) is defined based on the total amount of the above six types unless otherwise specified.
  • the component (A) is a salt or a hydrate
  • the content of the component (A) is a value converted into chlorogenic acids which are free acids.
  • the solid composition of the present invention contains ⁇ -aminobutyric acid (B).
  • ⁇ -aminobutyric acid (B) may be referred to as “component (B)” in the present specification.
  • the component (B) can be produced by various methods, or a commercially available product (for example, GABA-S; Kyowa Hakko Bio Co., Ltd.) can be used.
  • L-aminobutyric acid-producing bacteria such as Lactobacillus plantum and Lactobacillus brevis TY414 (FERMP-16910; Japanese Patent Application Laid-Open No. 2000-210075) can be used to ferment L-aminobutyric acid.
  • Method for producing ⁇ -aminobutyric acid from glutamic acid Method for extracting from plants containing ⁇ -aminobutyric acid such as rice germ, wheat germ, and Gavalon tea; Examples thereof include a method of further purifying an extract from a plant containing butyric acid by ion exchange chromatography.
  • the component (B) may be a commercially available product or a purified product, but as long as it contains an effective amount of ⁇ -aminobutyric acid, it is a fermentation product of the above-mentioned ⁇ -aminobutyric acid-producing bacteria, ⁇ -aminobutyric acid. It may be in the form of a plant containing or an extract thereof.
  • the content of the component (B) is 0.5% by mass or more, but the effect of the present invention can be easily enjoyed, and the total amount of the solid food to be ingested can be reduced. From the viewpoint of improving the solubility of the solid composition in water, 3% by mass or more is more preferable, and from the same viewpoint, 58% by mass or less is preferable, 50% by mass or less is more preferable, and 40% by mass or less. Is even more preferable.
  • the content of the component (B) in the solid composition is 0.5% by mass or more, preferably 0.5 to 58% by mass, more preferably 3 to 58% by mass, and more preferably 3 to 50%. It is by mass, more preferably 3 to 40% by mass.
  • the analysis of ⁇ -aminobutyric acid shall follow the method described in the examples below.
  • the content ratio of the component (A) to the component (B) is 100: 0.7 to 140 in terms of mass ratio.
  • the solubility of chlorogenic acids in water can be improved in the solid composition, and the hygroscopicity of ⁇ -aminobutyric acid is lowered.
  • the content ratio of the component (A) to the component (B) is a mass ratio, preferably 100: 1 to 120, more preferably. It is 100: 5 to 100, more preferably 100: 7 to 90, still more preferably 100: 8 to 80, still more preferably 100: 10 to 70, still more preferably 100: 30 to 60.
  • the solid composition of the present invention contains minerals (eg, calcium, magnesium, iron, zinc, chromium, selenium, manganese, molybdenum, copper, iodine, as long as the effects of the present invention are not impaired.
  • minerals eg, calcium, magnesium, iron, zinc, chromium, selenium, manganese, molybdenum, copper, iodine, as long as the effects of the present invention are not impaired.
  • Phosphorus, potassium, sodium vitamins (eg, vitamin A, vitamin B1, vitamin B2, vitamin B6, vitamin B12, vitamin C, vitamin D, vitamin E, folic acid and their salts, or esters thereof), sweeteners (eg)
  • additives such as simple sugars, small sugars, sugar alcohols, synthetic sweeteners
  • acidulants e.g, sorbitol, sorbitol, sorbitol, sorbitol, sorbitol, sorbitol, sorbitol, gly
  • the solid composition of the present invention is not particularly limited as long as it is in a solid state at room temperature (25 ° C.), and specific dosage forms include, for example, capsules, granules, powders, tablets (chewable tablets, etc.). Included), oral solid preparations such as pills and troches. Among them, tablets and powders are preferable because they can be ingested in a small amount at a time and are easily ingested as food.
  • an acceptable carrier When preparing such a solid composition, an acceptable carrier can be appropriately combined and used as needed.
  • the carrier include excipients (eg, lactose, starches, crystalline cellulose, sucrose, mannitol, light anhydrous silicic acid, calcium hydrogen phosphate), binders (eg, hydroxypropylmethyl cellulose, hydroxypropyl cellulose, gelatin, etc.).
  • Alfarated starch polyvinylpyrrolidone, polyvinyl alcohol, pullulan, methylcellulose, hardened oil
  • disintegrants eg carmellose, carmellose calcium, croscarmellose sodium, crospopidone, corn starch, low substitution hydroxypropyl cellulose
  • smooth Agents eg, calcium stearate, magnesium stearate, sucrose fatty acid ester, stearyl sodium fumarate, talc
  • fluidity improvers eg, silicon dioxide
  • flavoring agents eg, stevia, aspartame
  • fragrances bulking agents.
  • the content of the carrier can be appropriately set within a range that does not impair the object of the present invention.
  • the solid composition of the present invention preferably has a dissolution time (seconds) of 200 seconds or less, further 180 seconds or less, and further 100 seconds or less by the solubility evaluation in water described in Examples described later. When this value is small, it dissolves quickly in water and can prevent a decrease in intake due to undissolved residue, so that improvement in absorption of chlorogenic acids after oral ingestion and high functional expression can be expected. Further, in the solid composition of the present invention, the amount of increase in hygroscopicity (% by mass) according to the evaluation of hygroscopicity is preferably 20% by mass or less, further 18% by mass or less, and further preferably 10% by mass or less.
  • the solid composition containing the component (A) and the component (B) in a specific mass ratio a mixture of water, the component (A) and the component (B) is present on the surface of the component (B). It is presumed that it is formed, and by inhibiting the movement of water on the surface of the component (B), the hygroscopicity is lowered and the change in appearance can be suppressed.
  • the solid composition of the present invention can be produced according to a conventional method, and an appropriate method can be adopted.
  • the component (A) and the component (B), and if necessary, the carrier and / or the additive are mixed and produced so that the mass ratio of the component (A) and the component (B) is within the above range.
  • the mixing order of each component is not particularly limited, and the components may be added in any order or at the same time.
  • an appropriate method such as stirring or shaking can be adopted, and a mixing device may be used.
  • the mixing method of the mixing device may be a container rotation type or a container fixed type.
  • the container rotation type for example, a horizontal cylinder type, a V type, a double cone type, a cube type and the like can be adopted.
  • the container fixing type for example, a ribbon type, a screw type, a conical screw type, a paddle type, a fluidized bed type, a Philips blender and the like can be adopted.
  • it may be a granulated product by a known granulation method. Examples of the granulation method include spray granulation, fluidized bed granulation, compression granulation, rolling granulation, stirring granulation, extrusion granulation, powder-coated granulation and the like.
  • the granulation conditions can be appropriately selected depending on the granulation method.
  • the granulated product may be compressed by a tableting molding machine and molded.
  • a commonly used tableting machine such as a rotary type tableting machine or a single-shot type tableting machine can be used.
  • the compression molding pressure at the time of tableting is preferably about 10 to 30 MPa from the viewpoint of maintaining the hardness of the molded product.
  • the tablet hardness is preferably a hardness that can withstand transportation, storage, and the like, and is preferably about 10N to 200N.
  • the shape of the tablet may be a circular or oval, oval, oval, quadrangular or other planar shape tablet, but is preferably circular from the viewpoint of ease of administration.
  • the diameter is preferably 3 to 30 mm, more preferably 3 to 20 mm from the viewpoint of ease of administration.
  • the tablet weighs 0.1 to 6 g per preparation from the viewpoint of convenience and effectiveness.
  • the solid composition of the present invention contains chlorogenic acids (A) and 0.5% by mass or more of ⁇ -aminobutyric acid (B) from the viewpoint of improving the solubility in water and lowering the hygroscopicity. It is preferable that the composition is a solid composition in which the content ratio of the component (A) to the component (B) is 100: 7 to 90 in mass ratio.
  • the solid composition of the present invention contains chlorogenic acids (A) and 0.5% by mass or more of ⁇ -aminobutyric acid (B) from the viewpoint of improving the solubility in water and lowering the hygroscopicity. It is preferable that the composition is a solid composition in which the content ratio of the component (A) to the component (B) is 100: 8 to 80 by mass.
  • the solid composition of the present invention contains chlorogenic acids (A) and 0.5% by mass or more of ⁇ -aminobutyric acid (B) from the viewpoint of improving the solubility in water and lowering the hygroscopicity. It is preferable that the composition is a solid composition in which the content ratio of the component (A) to the component (B) is 100: 10 to 70 in mass ratio.
  • the solid composition of the present invention contains chlorogenic acids (A) and 0.5% by mass or more of ⁇ -aminobutyric acid (B) from the viewpoint of improving the solubility in water and lowering the hygroscopicity. It is preferable that the composition is a solid composition in which the content ratio of the component (A) to the component (B) is 100: 30 to 60 in mass ratio.
  • the solid composition of the present invention comprises a coffee bean extract containing chlorogenic acids (A) and 0.5% by mass or more of ⁇ -aminobutyric acid from the viewpoint of improving the solubility in water and lowering the hygroscopicity. It is preferable that the composition contains (B) and the content ratio of the component (A) to the component (B) is 100: 7 to 90 in mass ratio.
  • the solid composition of the present invention comprises a coffee bean extract containing chlorogenic acids (A) and 0.5% by mass or more of ⁇ -aminobutyric acid from the viewpoint of improving the solubility in water and lowering the hygroscopicity. It is preferable that the composition contains (B) and the content ratio of the component (A) to the component (B) is 100: 8 to 80 by mass.
  • the solid composition of the present invention comprises a coffee bean extract containing chlorogenic acids (A) and 0.5% by mass or more of ⁇ -aminobutyric acid from the viewpoint of improving the solubility in water and lowering the hygroscopicity. It is preferable that the composition contains (B) and the content ratio of the component (A) to the component (B) is 100: 10 to 70 by mass.
  • the solid composition of the present invention comprises a coffee bean extract containing chlorogenic acids (A) and 0.5% by mass or more of ⁇ -aminobutyric acid from the viewpoint of improving the solubility in water and lowering the hygroscopicity. It is preferable that the composition contains (B) and the content ratio of the component (A) to the component (B) is 100: 30 to 60 in terms of mass ratio.
  • the present invention further discloses the following solid composition.
  • Chlorogenic acids (A) and ⁇ -aminobutyric acid (B) of 0.5% by mass or more are contained, and the content ratio of the component (A) to the component (B) is 100: 0.7 by mass.
  • a coffee bean extract containing chlorogenic acids (A) and 0.5% by mass or more of ⁇ -aminobutyric acid (B) are contained, and the content ratio of the component (A) to the component (B) is mass.
  • the L value of coffee beans is preferably 27 or more, more preferably 29 or more, still more preferably 35 or more, and preferably less than 62, more preferably 60 or less, still more preferably 55 or less.
  • the solid composition according to ⁇ 2> which is preferably 27 or more and less than 62, more preferably 29 or more and 60 or less, and further preferably 35 or more and 55 or less and less than 27 or more and less than 62.
  • the mass ratio of caffeine / chlorogenic acids in the coffee bean extract is preferably 0.015 or less, more preferably 0.014 or less, still more preferably 0.010 or less, still more preferably 0.0066 or less, and further.
  • the content of the chlorogenic acids (A) in the solid composition is preferably 1% by mass or more, more preferably 2% by mass or more, more preferably 3% by mass or more, still more preferably 5% by mass or more.
  • ⁇ -aminobutyric acid (B) in the solid composition is 0.5% by mass or more, preferably 3% by mass or more, and preferably 58% by mass or less.
  • the content ratio of the component (A) to the component (B) is a mass ratio, preferably 100: 1 to 120, more preferably 100: 5 to 100, still more preferably 100: 7 to 90, still more preferably 100. : 8 to 80, more preferably 100: 10 to 70, still more preferably 100: 30 to 60.
  • the form of the solid composition is preferably an oral solid preparation, more preferably a capsule, a granule, a powder, a tablet, a pill or a troche, and further preferably a tablet or a powder ⁇ 1.
  • Eluent B Acetonitrile [concentration gradient condition] Time (minutes) Liquid A (% (v / v)) Liquid B (% (v / v)) 0.0 100% 0% 10.0 100% 0% 15.0 95% 5% 20.0 95% 5% 22.0 92% 8% 50.0 92% 8% 52.0 10% 90% 60.0 10% 90% 60.1 100% 0% 70.0 100% 0% [Retention time of chlorogenic acids] When the retention time of chlorogenic acids was confirmed using a standard product, it was as follows.
  • caffeine was measured by the absorbance at a wavelength of 270 nm using the reagent caffeine as a standard substance.
  • Caffeine was quantified from the area ratio obtained from the peak area of 21.1 minutes.
  • Dissolution time 100 mg of the mixed powder was separated, placed in a falcon tube containing 10 mL of ion-exchanged water (25 ° C.), and rotated with Mix ROTOR (60 r / min, AS ONE Corporation). The time until the powder in the Falcon tube could not be visually confirmed was measured and used as the dissolution time (seconds).
  • (2) Judgment of undissolved residue Weigh 30 mL of ion-exchanged water (25 ° C) in a 50 mL beaker, add 100 mg of mixed powder while stirring at a constant speed with a magnetic stirrer, stir for 10 seconds, and filter (milk sediment disc black). bottom.
  • Binarization score is less than 10% of Comparative Example 1
  • B Binarization score is 10 to 25% of Comparative Example 1.
  • C Binarization score is 25 to 50% of Comparative Example 1.
  • D Binarization score is 50% or more compared to Comparative Example 1.
  • Moisture absorption increase (mass%) [(total mass after 4.5 hours-container mass) / (initial total mass-container mass)] ⁇ 100
  • Change in appearance After taking 100 mg of the mixed powder and storing it in an environment of 40 ° C. and 75% RH for 4.5 hours, visually observe the change in the appearance of the powder and judge according to the following criteria. Was done. A: Remains white, or slightly discolored B: Slightly brown but within the acceptable range of quality C: Discolored to grayish brown but within the acceptable range of quality D: Black change is observed, Or fail to deliquesce
  • Example 11 and Comparative Examples 8 to 11 Each raw material component was uniformly mixed in a mortar with the compounding composition shown in Table 2 to obtain a mixed powder.
  • the obtained mixed powder was evaluated for hygroscopicity ((1) increased amount of moisture absorption) in the same manner as in Example 1. The results are shown in Table 2.
  • Examples 1 to 10 containing the component (A) and the component (B) in a specific mass ratio have a shorter dissolution time in water and dissolve in water as compared with Comparative Example 1. There was little left. Further, as is clear from Tables 1 and 2, the amount of increase in moisture absorption increases as the amount of the component (B) increases, but Examples 1 to 1 to the example containing the component (A) and the component (B) in a specific mass ratio. In No. 11, it was confirmed that the amount of increase in moisture absorption was small and the change in appearance was also small.
  • Prescription example 1 Preparation of coffee bean extract The powder prepared by extracting the crushed raw coffee bean with hot water and then spray-drying it is dissolved in an ethanol aqueous solution, and the filtered solution obtained by filtration is used as activated charcoal and ions.
  • Raw coffee bean extract was prepared by treatment with a column using an exchange resin. This was pulverized by drying and used in the following procedure.
  • the content of chlorogenic acids (total of 3-CQA, 4-CQA, 5-CQA, 3-FQA, 4-FQA and 5-FQA) in the obtained coffee bean extract powder was 33% by mass, that of caffeine. The content was 0.006% by mass.
  • the mass ratio of caffeine / chlorogenic acids (CQA + FQA) was 0.0002.

Landscapes

  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Veterinary Medicine (AREA)
  • Pharmacology & Pharmacy (AREA)
  • Epidemiology (AREA)
  • Animal Behavior & Ethology (AREA)
  • General Health & Medical Sciences (AREA)
  • Public Health (AREA)
  • Medicinal Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Food Science & Technology (AREA)
  • Mycology (AREA)
  • Nutrition Science (AREA)
  • Polymers & Plastics (AREA)
  • Bioinformatics & Cheminformatics (AREA)
  • Proteomics, Peptides & Aminoacids (AREA)
  • Molecular Biology (AREA)
  • Botany (AREA)
  • Acyclic And Carbocyclic Compounds In Medicinal Compositions (AREA)
PCT/JP2020/038183 2020-10-08 2020-10-08 固形状組成物 Ceased WO2022074798A1 (ja)

Priority Applications (2)

Application Number Priority Date Filing Date Title
JP2022555207A JP7727653B2 (ja) 2020-10-08 2020-10-08 固形状組成物
PCT/JP2020/038183 WO2022074798A1 (ja) 2020-10-08 2020-10-08 固形状組成物

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/JP2020/038183 WO2022074798A1 (ja) 2020-10-08 2020-10-08 固形状組成物

Publications (1)

Publication Number Publication Date
WO2022074798A1 true WO2022074798A1 (ja) 2022-04-14

Family

ID=81126376

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/JP2020/038183 Ceased WO2022074798A1 (ja) 2020-10-08 2020-10-08 固形状組成物

Country Status (2)

Country Link
JP (1) JP7727653B2 (https=)
WO (1) WO2022074798A1 (https=)

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS57115147A (en) * 1981-01-07 1982-07-17 San Ei Chem Ind Ltd Method for preventing browning of saccharide
JP2008150350A (ja) * 2006-12-20 2008-07-03 Unitika Ltd γ−アミノ酪酸含有組成物
JP2010150212A (ja) * 2008-12-26 2010-07-08 Lion Corp チュアブル錠
JP2010187554A (ja) * 2009-02-16 2010-09-02 Oriza Yuka Kk γ−アミノ酪酸含有コーヒー豆抽出物
CN103315191A (zh) * 2013-07-18 2013-09-25 广南(湛江)家丰饲料有限公司 一种猪用免疫增强剂及其制备方法
CN111346061A (zh) * 2018-12-21 2020-06-30 北京科莱博医药开发有限责任公司 绿原酸组合物及其制备方法
JP2020169123A (ja) * 2019-04-01 2020-10-15 花王株式会社 ホットフラッシュ改善剤

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2000187554A (ja) * 1998-12-24 2000-07-04 Casio Comput Co Ltd 入力装置

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS57115147A (en) * 1981-01-07 1982-07-17 San Ei Chem Ind Ltd Method for preventing browning of saccharide
JP2008150350A (ja) * 2006-12-20 2008-07-03 Unitika Ltd γ−アミノ酪酸含有組成物
JP2010150212A (ja) * 2008-12-26 2010-07-08 Lion Corp チュアブル錠
JP2010187554A (ja) * 2009-02-16 2010-09-02 Oriza Yuka Kk γ−アミノ酪酸含有コーヒー豆抽出物
CN103315191A (zh) * 2013-07-18 2013-09-25 广南(湛江)家丰饲料有限公司 一种猪用免疫增强剂及其制备方法
CN111346061A (zh) * 2018-12-21 2020-06-30 北京科莱博医药开发有限责任公司 绿原酸组合物及其制备方法
JP2020169123A (ja) * 2019-04-01 2020-10-15 花王株式会社 ホットフラッシュ改善剤

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
NISHIMURA MIE, SUZUKI MIHO, TAKAHASHI RYUTO, YAMAGUCHI SHOHEI, TSUBAKI KAZUFUMI, FUJITA TOMOYUKI, NISHIHIRA JUN, NAKAMURA KOZO: "Daily Ingestion of Eggplant Powder Improves Blood Pressure and Psychological State in Stressed Individuals: A Randomized Placebo-Controlled Study", NUTRIENTS, vol. 11, no. 11, 1 January 2019 (2019-01-01), XP055934177, DOI: 10.3390/nu11112797 *

Also Published As

Publication number Publication date
JPWO2022074798A1 (https=) 2022-04-14
JP7727653B2 (ja) 2025-08-21

Similar Documents

Publication Publication Date Title
EP4129270B1 (en) Modified release orally administered amino acid formulations
JP2018191634A (ja) 食品組成物
US11813303B2 (en) Hot flash ameliorant
JP7727653B2 (ja) 固形状組成物
JP5476782B2 (ja) アルギニン含有錠剤の製造方法
JP6815175B2 (ja) 固形組成物
MX2010010383A (es) Formulaciones orodispersables de inhibidores de fosfodiesterasa-5 (pde-5).
US20210046010A1 (en) Tablets containing arginine at high concentration
CN108024968A (zh) 门冬氨酸鸟氨酸的泡腾制剂
JP6823446B2 (ja) 固形状組成物
JP7167286B2 (ja) 圧縮成型製剤
JP2020169123A (ja) ホットフラッシュ改善剤
JP7321743B2 (ja) 固形状組成物
JPWO2006106805A1 (ja) 物質の保存安定性向上方法
CN112826802A (zh) 一种枸橼酸西地那非咀嚼片及其制备方法
JP2016108265A (ja) 持続性抗酸化剤
JP7758478B2 (ja) 固形組成物
AU2019314671A1 (en) Mixtures of branched chain keto acids (BCKA) and method for the production of such mixtures
JP2019085361A (ja) 経口毛穴目立ち改善剤
JPH059120A (ja) 悪酔改善剤
TW202425814A (zh) 口服用組合物
CN121099990A (zh) 器官或组织的功能保护剂
JP2023066490A (ja) 経口用顆粒組成物
JP2013216642A (ja) キノコの超臨界二酸化炭素抽出物を含むリパーゼ活性阻害用組成物
JP2020169124A (ja) ホットフラッシュ改善剤

Legal Events

Date Code Title Description
121 Ep: the epo has been informed by wipo that ep was designated in this application

Ref document number: 20956745

Country of ref document: EP

Kind code of ref document: A1

ENP Entry into the national phase

Ref document number: 2022555207

Country of ref document: JP

Kind code of ref document: A

NENP Non-entry into the national phase

Ref country code: DE

122 Ep: pct application non-entry in european phase

Ref document number: 20956745

Country of ref document: EP

Kind code of ref document: A1