Solid shape composition

Abstract

Provided is a solid composition that contains chlorogenic acids and γ-aminobutyric acid and that has improved solubility in water and suppressed moisture absorbency.　This solid composition contains chlorogenic acids (A) and 0.5 mass% or more of γ-aminobutyric acid (B). The content ratio by mass of the component (A) and the component (B) is 100:0.7 to 100:140.

Description

[Technical Field]

[0001] The present invention relates to a solid composition. [Background technology]

[0002] Chlorogenic acids are polyphenols found in green coffee beans. Physiological effects of chlorogenic acids have been reported, including improving autonomic nervous function and alleviating vague symptoms (Patent Document 1).

[0003] On the other hand, gamma-aminobutyric acid (GABA) is the major inhibitory neurotransmitter in the central nervous system of mammals. GABA is also found in a wide range of organisms, including not only mammals but also other animals and plants. γ-Aminobutyric acid is known to have a strong tranquilizing effect, and has been reported to be effective against, for example, menopausal or presenile insomnia, depression, and irritability (Non-Patent Document 1).

[0004] In order to enjoy the physiological effects of chlorogenic acids and γ-aminobutyric acid, solid compositions such as tablets and powders are suitable forms. Patent Document 2 describes tablets and granules for oral administration that contain a γ-aminobutyric acid-containing coffee bean extract prepared from a hot water extract of coffee beans of the Rubiaceae family.

[0005] (Patent Document 1) Japanese Patent Application Laid-Open No. 2002-145765 (Patent Document 2) JP 2010-187554 A

[0006] (Non-patent document 1) Food and Development, 2001, 36(6):4-6 Summary of the Invention

[0007] The present invention provides a solid composition containing chlorogenic acids (A) and 0.5% by mass or more of γ-aminobutyric acid (B), in which the mass ratio of component (A) to component (B) is 100:0.7 to 140.

[0008] However, chlorogenic acids in solid form, such as powders, have low solubility in water, raising concerns about their in vivo bioavailability. In other words, because oral preparations only exert their pharmacological effects once the active ingredient is released in the gastrointestinal tract and absorbed through the gastrointestinal membrane, it is important that the active ingredient dissolves quickly after ingestion. Furthermore, when dissolving powders in liquid, low solubility in water can lead to residual chlorogenic acid, reducing the amount of chlorogenic acid that can be ingested. On the other hand, solid γ-aminobutyric acid is highly hygroscopic and deliquesces in the presence of moisture in the air, so solid compositions containing even small amounts of γ-aminobutyric acid are prone to quality deterioration, such as discoloration, during storage. Therefore, the present invention relates to providing a solid composition containing chlorogenic acids and γ-aminobutyric acid, which has improved solubility in water and reduced hygroscopicity.

[0009] As a result of extensive research, the inventors have found that when a solid composition contains chlorogenic acids and γ-aminobutyric acid in a specific mass ratio, the solubility in water is improved and the hygroscopicity is reduced, thereby preventing changes in appearance.

[0010] According to the present invention, it is possible to provide a solid composition containing chlorogenic acids and γ-aminobutyric acid, which has improved solubility in water, reduced hygroscopicity, and little change in appearance.

[0011] The solid composition of the present invention contains chlorogenic acids (A). In this specification, "chlorogenic acids" is a collective term for monocaffeoylquinic acids, i.e., 3-caffeoylquinic acid, 4-caffeoylquinic acid, and 5-caffeoylquinic acid, and monoferuloylquinic acids, i.e., 3-feruloylquinic acid, 4-feruloylquinic acid, and 5-feruloylquinic acid. In the present invention, at least one of the six types listed above may be contained. Stereoisomers and analogs of the chlorogenic acids exist, and include pure stereoisomers, analogs, and mixtures thereof. Hereinafter, in this specification, "chlorogenic acids (A)" may be referred to as "component (A)".

[0012] Component (A) may be in the form of a salt or a hydrate. The salt is preferably a pharmaceutically acceptable salt. Examples of such salts include salts with alkali metals such as lithium, sodium, and potassium; salts with alkaline earth metals such as magnesium and calcium; salts with inorganic bases such as ammonium salts; salts with basic amino acids such as arginine, lysine, histidine, and ornithine; and salts with organic bases such as monoethanolamine, diethanolamine, and triethanolamine. Of these, salts with alkali metals or alkaline earth metals are preferred.

[0013] As component (A), commercially available reagents may be used, but plant extracts containing chlorogenic acids may also be used. The plant is not particularly limited as long as it contains chlorogenic acids, and examples thereof include one or more selected from sunflower seeds, unripe apples, coffee beans, Simon leaves, cones of pine plants, seed husks of pine plants, sugarcane, nandina leaves, burdock, eggplant skin, plum fruit, coltsfoot, and plants of the Vitaceae family. Of these, coffee beans are preferred in terms of the content of chlorogenic acids. The species and origin of the coffee beans are not particularly limited.

[0014] The coffee beans may be green coffee beans or roasted coffee beans, or a combination of these can be used. From the viewpoint of the content of chlorogenic acids, the roasted coffee beans are preferably lightly roasted. The L value range of lightly roasted coffee beans is preferably 27 or more, more preferably 29 or more, and even more preferably 35 or more, from the viewpoint of the content of chlorogenic acids. From the viewpoint of flavor, it is preferably less than 62, more preferably 60 or less, and even more preferably 55 or less. The L value range 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 even more preferably 35 or more and 55 or less. Herein, the "L value" refers to the lightness of the roasted coffee beans after grinding, measured with a colorimeter (e.g., a spectrophotometer SE2000, manufactured by Nippon Denshoku Co., Ltd.), with black being an L value of 0 and white being an L value of 100. The coffee beans to be extracted may be unground or ground.

[0015] The extraction method and conditions can be appropriately selected, and can be performed by known methods such as batch extraction, drip extraction, column extraction, etc. using water, hot water, or a water-soluble organic solvent. Examples of water-soluble organic solvents include lower alcohols such as ethanol. Examples of extraction methods that can be used include those described in JP-A-58-138347, JP-A-59-51763, JP-A-62-111671, and JP-A-5-236918. The purification method is not particularly limited, and known methods can be used, but for example, various types of chromatography, such as ion chromatography, molecular sieve chromatography, and reversed-phase chromatography, can be used alone or in combination. After extraction, the resulting extract may be concentrated by known means such as atmospheric concentration, reduced pressure concentration, or membrane concentration, or the extract or concentrate may be dried by known means such as spray drying or freeze drying. The reagent of component (A) and the plant extract containing component (A) are in the form of a solid (powder, granules, etc.) at room temperature (25°C).

[0016] In terms of physiological effects, the content of component (A) in the coffee bean extract is preferably 10% by mass or more, more preferably 15% by mass or more, of the total amount, and is preferably 70% by mass or less, more preferably 60% by mass or less.

[0017] The coffee bean extract is preferably decaffeinated. The mass ratio of caffeine to chlorogenic acids in the coffee bean extract is preferably 0.015 or less, more preferably 0.014 or less, even more preferably 0.010 or less, even more preferably 0.0066 or less, even more preferably 0.0050 or less, even more preferably 0.0020 or less, and even more preferably 0.0005 or less. In other words, the mass ratio of chlorogenic acids to caffeine in the coffee bean extract is preferably 65 or more, more preferably 70 or more, even more preferably 100 or more, even more preferably 150 or more, even more preferably 200 or more, even more preferably 500 or more, and even more preferably 2000 or more. In terms of physiological effects, the caffeine content in the coffee bean extract is preferably 0.5% by mass or less, more preferably 0.4% by mass or less, even more preferably 0.3% by mass or less, even more preferably 0.2% by mass or less, even more preferably 0.15% by mass or less, even more preferably 0.1% by mass or less, and even more preferably 0.05% by mass or less, of the total amount. It is even more preferable that the coffee bean extract is substantially free of caffeine (for example, below the detection limit of HPLC). In this specification, chlorogenic acids and caffeine will be analyzed according to the methods described in the Examples below. Note that in this specification, the contents of chlorogenic acids and caffeine in a coffee bean extract refer to their mass proportions in the dry coffee bean extract.

[0018] Examples of methods for selectively reducing caffeine in coffee bean extracts include a method of subjecting decaffeinated coffee beans to an extraction process and a method of subjecting a coffee bean extract or a concentrate thereof to a decaffeination process. Of these, a method of subjecting a coffee bean extract or a concentrate thereof to a decaffeination process is preferred. The decaffeination process for a coffee bean extract or a concentrate thereof is preferably performed by dissolving the coffee bean extract or concentrate thereof in a mixed solution of water and an organic solvent and contacting it with activated carbon and / or activated clay or acid clay. For example, the method described in JP 2011-4766 A can be employed. The coffee bean extract or concentrate thereof to be subjected to the decaffeination process may be a commercially available product. Decaffeinated coffee beans are coffee beans that have been subjected to a decaffeination process. Known methods can be used for the decaffeination process for coffee beans, including, for example, the water method, supercritical carbon dioxide extraction, and organic solvent extraction.

[0019] The content of component (A) in the solid composition of the present invention is preferably 1% by mass or more, more preferably 2% by mass or more, more preferably 3% by mass or more, and even more preferably 5% by mass or more from the viewpoint of physiological activity and reducing the hygroscopicity of the solid composition, and is preferably 99.5% by mass or less, more preferably 98% by mass or less, more preferably 97% by mass or less, and even more preferably 95% by mass or less from the viewpoint of processing. The content of 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, and even more preferably 5 to 95% by mass. In this specification, the content of component (A) is defined based on the total amount of the above six components unless otherwise specified. When component (A) is a salt or a hydrate, the content of component (A) is the value converted into chlorogenic acids, which are free acids.

[0020] The solid composition of the present invention contains γ-aminobutyric acid (B). Hereinafter, in this specification, "γ-aminobutyric acid (B)" may be referred to as "component (B)". Component (B) can be produced by various methods, or commercially available products (e.g., GABA-S; Kyowa Hakko Bio Co., Ltd.) can be used. Examples of methods for producing γ-aminobutyric acid include producing γ-aminobutyric acid from L-glutamic acid by fermentation using γ-aminobutyric acid-producing bacteria such as Lactobacillus plantum and Lactobacillus brevis TY414 (FERMP-16910; JP 2000-210075 A); extracting γ-aminobutyric acid from plants containing γ-aminobutyric acid, such as rice germ, wheat germ, and gabaron tea; and further purifying the fermentation product of the above-mentioned γ-aminobutyric acid-producing bacteria or extracts from plants containing γ-aminobutyric acid by ion exchange chromatography. Component (B) may be a commercially available product or a purified product, but may also be in the form of a fermentation product of the above-mentioned γ-aminobutyric acid-producing bacteria, a plant containing γ-aminobutyric acid, or an extract thereof, as long as it contains an effective amount of γ-aminobutyric acid.

[0021] The content of component (B) in the solid composition of the present invention is 0.5% by mass or more, but from the viewpoints of making it easier to enjoy the effects of the present invention, reducing the total amount of solid food to be orally ingested, and improving the solubility of the solid composition in water, it is more preferably 3% by mass or more, and from the same viewpoints, it is preferably 58% by mass or less, more preferably 50% by mass or less, and even more preferably 40% by mass or less. The content of 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, more preferably 3 to 50% by mass, and even more preferably 3 to 40% by mass. In this specification, the analysis of γ-aminobutyric acid will be carried out in accordance with the method described in the Examples below.

[0022] In the solid composition of the present invention, the content ratio of component (A) to component (B) is, in mass ratio, 100:0.7 to 140. By setting the mass ratio in this range, the solubility of chlorogenic acids in water can be improved and the hygroscopicity of γ-aminobutyric acid can be reduced in the solid composition. From the viewpoint of improving the solubility in water and reducing the hygroscopicity of the solid composition, the mass ratio of component (A) to component (B) is preferably 100:1 to 120, more preferably 100:5 to 100, even more preferably 100:7 to 90, even more preferably 100:8 to 80, even more preferably 100:10 to 70, and even more preferably 100:30 to 60.

[0023] In addition to the above components, the solid composition of the present invention may contain additives such as minerals (e.g., calcium, magnesium, iron, zinc, chromium, selenium, manganese, molybdenum, copper, iodine, phosphorus, potassium, sodium), vitamins (e.g., vitamin A, vitamin B1, vitamin B2, vitamin B6, vitamin B12, vitamin C, vitamin D, vitamin E, folic acid and salts thereof or esters thereof), sweeteners (e.g., monosaccharides, oligosaccharides, sugar alcohols, synthetic sweeteners), acidulants, flavorings, coloring agents, preservatives, etc., within a range that does not impair the effects of the present invention. The content of the additives can be appropriately set within a range that does not impair the object of the present invention.

[0024] 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, oral solid preparations such as capsules, granules, powders, tablets (including chewable tablets), pills, lozenges, etc. Among these, tablets and powders are preferred because they can be taken in small amounts per dose and are easy to ingest as a food.

[0025] When preparing such a solid composition, an acceptable carrier can be used in appropriate combination as needed. Examples of the carrier include excipients (e.g., lactose, starches, crystalline cellulose, sucrose, mannitol, light anhydrous silicic acid, calcium hydrogen phosphate), binders (e.g., hydroxypropylmethylcellulose, hydroxypropylcellulose, gelatin, pregelatinized starch, polyvinylpyrrolidone, polyvinyl alcohol, pullulan, methylcellulose, hydrogenated oil), disintegrants (e.g., carmellose, carmellose calcium, croscarmellose sodium, crospovidone, corn starch, low-substituted hydroxypropylcellulose), lubricants (e.g., calcium stearate, magnesium stearate, sucrose fatty acid esters, sodium stearyl fumarate, talc), flow improvers (e.g., silicon dioxide), flavoring agents (e.g., stevia, aspartame), flavorings, fillers, surfactants, dispersants, buffers, coating agents, diluents, etc. The content of the carrier can be appropriately set within a range that does not impair the object of the present invention.

[0026] The solid composition of the present invention preferably has a dissolution time (seconds) of 200 seconds or less, more preferably 180 seconds or less, and even more preferably 100 seconds or less, as determined by the water solubility evaluation described in the Examples below. If this value is small, the composition dissolves quickly in water and can prevent a decrease in intake due to residual residue, which is expected to improve the absorbability of chlorogenic acids after oral ingestion and to exhibit high functionality. Furthermore, the solid composition of the present invention preferably has a moisture absorption increase (mass%) of 20% or less, more preferably 18% or less, and even more preferably 10% or less, as measured by the same moisture absorption evaluation. When this value is small, the appearance of the solid composition changes little, handling is not affected, and quality stability can be maintained. Although the reason why a solid composition containing components (A) and (B) at a specific mass ratio not only improves solubility in water but also suppresses hygroscopicity is unclear, it is thought to be as follows: Deliquescence occurs when a small volume of saturated aqueous solution on a solid surface is lower than the water vapor pressure in the atmosphere, and water vapor is absorbed, diluting the saturated aqueous solution. In contrast, in a solid composition containing components (A) and (B) at a specific mass ratio, a mixture of water, components (A), and (B) is formed on the surface of component (B), and this inhibits the movement of water on the surface of component (B), thereby reducing hygroscopicity and suppressing changes in appearance.

[0027] The solid composition of the present invention can be produced by conventional methods, and any suitable method can be employed. For example, it can be produced by mixing component (A) and component (B), and optionally a carrier and / or additives, so that the mass ratio of component (A) to component (B) falls within the above-mentioned range. The order of mixing the components is not particularly limited, and they may be added in any order or simultaneously. Suitable mixing methods, such as stirring and shaking, can be employed, and a mixing device can also be used. The mixing method of the mixing device may be either a rotating container type or a fixed container type. Examples of rotating container types that can be used include horizontal cylindrical, V-type, double-cone, and cubic types. Examples of fixed container types that can be used include ribbon, screw, conical screw, paddle, fluidized bed, and Phillips blenders. Alternatively, the granules may be prepared by a known granulation method, such as spray granulation, fluidized bed granulation, compression granulation, tumbling granulation, stirring granulation, extrusion granulation, powder coating granulation, etc. Granulation conditions can be appropriately selected depending on the granulation method.

[0028] When making tablets, a mixture of component (A) and component (B), and if necessary a carrier and / or additives, may be directly compressed as a raw powder to form tablets, or the mixture may be granulated by the above-mentioned granulation method and then compressed and molded in a tableting machine. When tablets are produced by compressing the granules directly or by molding, a commonly used tableting machine such as a rotary tableting machine or a single punch tableting machine can be used. The compression molding pressure during tableting is preferably about 10 to 30 MPa in order to maintain the hardness of the molded product. Furthermore, the tablet hardness is preferably a hardness that can withstand transportation, storage, etc., and is preferably about 10N to 200N. The shape of the tablet may be various irregular shapes such as circular, oval, elliptical, rectangular, etc., but circular is preferred from the viewpoint of ease of administration. In the case of circular tablets, the diameter is preferably 3 to 30 mm, more preferably 3 to 20 mm, from the viewpoint of ease of administration. Furthermore, it is preferred that the weight of each tablet be 0.1 to 6 g from the viewpoint of convenience and effectiveness.

[0029] In terms of improving solubility in water and reducing hygroscopicity, the solid composition of the present invention preferably contains chlorogenic acids (A) and 0.5 mass% or more of γ-aminobutyric acid (B), and the mass ratio of the components (A) to (B) is preferably 100:7 to 90.

[0030] In terms of improving solubility in water and reducing hygroscopicity, the solid composition of the present invention preferably contains chlorogenic acids (A) and 0.5 mass% or more of γ-aminobutyric acid (B), and the mass ratio of the components (A) to (B) is 100:8-80.

[0031] In terms of improving solubility in water and reducing hygroscopicity, the solid composition of the present invention preferably contains chlorogenic acids (A) and 0.5 mass% or more of γ-aminobutyric acid (B), and the mass ratio of the components (A) to (B) is 100:10-70.

[0032] In terms of improving solubility in water and reducing hygroscopicity, the solid composition of the present invention preferably contains chlorogenic acids (A) and 0.5 mass% or more of γ-aminobutyric acid (B), and the mass ratio of the components (A) to (B) is preferably 100:30-60.

[0033] From the viewpoints of improving solubility in water and reducing hygroscopicity, the solid composition of the present invention is preferably a solid composition that contains a coffee bean extract containing chlorogenic acids (A) and 0.5 mass% or more of γ-aminobutyric acid (B), and the mass ratio of component (A) to component (B) is 100:7 to 90.

[0034] From the viewpoints of improving solubility in water and reducing hygroscopicity, the solid composition of the present invention is preferably a solid composition that contains a coffee bean extract containing chlorogenic acids (A) and 0.5 mass% or more of γ-aminobutyric acid (B), and the mass ratio of component (A) to component (B) is 100:8-80.

[0035] From the viewpoints of improving solubility in water and reducing hygroscopicity, the solid composition of the present invention is preferably a solid composition that contains a coffee bean extract containing chlorogenic acids (A) and 0.5 mass% or more of γ-aminobutyric acid (B), and the content ratio of component (A) to component (B) is preferably 100:10-70 by mass.

[0036] From the viewpoints of improving solubility in water and reducing hygroscopicity, the solid composition of the present invention is preferably a solid composition that contains a coffee bean extract containing chlorogenic acids (A) and 0.5 mass% or more of γ-aminobutyric acid (B), with the content ratio of component (A) to component (B) being 100:30-60 by mass.

[0037] In relation to the above-mentioned embodiment, the present invention further discloses the following solid composition.

[0038] <1> A solid composition containing chlorogenic acids (A) and 0.5 mass % or more of γ-aminobutyric acid (B), wherein the content ratio of component (A) to component (B) is 100:0.7-140 by mass.

[0039] <2> A solid composition comprising a coffee bean extract containing chlorogenic acids (A) and 0.5% by mass or more of γ-aminobutyric acid (B), wherein the content ratio of component (A) to component (B) is 100:0.7 to 140 by mass. <3> The L value of the coffee beans is preferably 27 or more, more preferably 29 or more, even more preferably 35 or more, and is preferably less than 62, more preferably 60 or less, even more preferably 55 or less, and is preferably 27 or more but less than 62, more preferably 29 or more but less than 60, even more preferably 35 or more but less than 55. <2> The solid composition according to claim 1. <4> The mass ratio of caffeine to chlorogenic acids in the coffee bean extract is preferably 0.015 or less, more preferably 0.014 or less, even more preferably 0.010 or less, even more preferably 0.0066 or less, even more preferably 0.0050 or less, even more preferably 0.0020 or less, and even more preferably 0.0005 or less. <2> or <3> The solid composition according to claim 1. <5> The content of 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, and even more preferably 5% by mass or more, and is preferably 99.5% by mass or less, more preferably 98% by mass or less, more preferably 97% by mass or less, and even more preferably 95% by mass or less, and is preferably 1 to 99.5% by mass, more preferably 2 to 98% by mass, more preferably 3 to 97% by mass, and even more preferably 5 to 95% by mass. <1> ~ <4> 1. The solid composition according to claim 1 , <6> The content of γ-aminobutyric acid (B) in the solid composition is 0.5% by mass or more, preferably 3% by mass or more, and is preferably 58% by mass or less, more preferably 50% by mass or less, and even more preferably 40% by mass or less, and is preferably 0.5 to 58% by mass, more preferably 3 to 58% by mass, more preferably 3 to 50% by mass, and even more preferably 3 to 40% by mass. <1> ~ <5> 1. The solid composition according to claim 1 , <7> The mass ratio of component (A) to component (B) is preferably 100:1 to 120, more preferably 100:5 to 100, even more preferably 100:7 to 90, even more preferably 100:8 to 80, even more preferably 100:10 to 70, and even more preferably 100:30 to 60. <1> ~ <6> 1. The solid composition according to claim 1 , <8> The solid composition is preferably in the form of an oral solid preparation, more preferably in the form of a capsule, granule, powder, tablet, pill or lozenge, and even more preferably in the form of a tablet or powder. <1> ~ <7> 1. The solid composition according to claim 1 , [Example]

[0040] [Analysis of chlorogenic acids] Chlorogenic acids were measured using HPLC. [Analytical equipment] Equipment: High-performance liquid chromatograph system Prominence (Shimadzu Corporation) Absorbance detector: SPD-20A (Shimadzu Corporation) Separation column: Cadenza CD-C18, inner diameter 4.6 mm x length 150 mm, particle size 3 μm (Intact Co., Ltd.) [Analysis conditions] Sample injection volume: 10 μL Flow rate: 1.0mL / min Detection wavelength: 325 nm Column oven temperature setting: 35℃ Eluent A: 5% (v / v) acetonitrile containing 0.05 mol / L acetic acid, 0.01 mol / L sodium acetate, and 0.1 mmol / L HEDP (1-hydroxyethane-1,1-diphosphonic acid). Eluent B: Acetonitrile [Concentration gradient conditions] Time (min) Solution A (%(v / v)) Solution 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] The retention times of chlorogenic acids were confirmed using standard samples, and were as follows: 3-Caffeoylquinic acid (3-CQA) 6.1 min 5-Caffeoylquinic acid (5-CQA) 10.5 min 4-Caffeoylquinic acid (4-CQA) 14.0 min 3-feruloylquinic acid (3-FQA) 15.5 min 5-feruloylquinic acid (5-FQA) 22.4 min 4-feruloylquinic acid (4-FQA) 23.7 min Chlorogenic acids were quantified from the area value of the peak that coincided with the above retention time.

[0041] [Caffeine Analysis] As in the above [Analysis of chlorogenic acids], caffeine was measured by absorbance at a wavelength of 270 nm using reagent caffeine as a standard substance. Caffeine was quantified from the area ratio calculated from the peak area at 21.1 minutes.

[0042] [γ-aminobutyric acid analysis] After weighing out 1 g of sample, it was dissolved in 25 mL of 10% sulfosalicylic acid solution and shaken for 20 minutes. The solution was adjusted to pH 2.2 with 3 mol / L sodium hydroxide, and the volume was adjusted to 100 mL with sodium citrate buffer (pH 2.2), followed by filtration. 2.5 mL of the filtrate was taken and adjusted to 25 mL with sodium citrate buffer (pH 2.2), and then 2.5 mL was taken and adjusted to 25 mL with sodium citrate buffer (pH 2.2). The resulting test solution was analyzed using an automated amino acid analysis method. [Automatic amino acid analyzer operating conditions] Model: JLC-500 / V2 (JEOL Ltd.) Column: LCR-6, inner diameter 4 mm x 120 mm (JEOL Ltd.) Mobile phase: Sodium citrate buffer solution (H-01 to H-04) (JEOL Ltd.) Reaction solution: Ninhydrin coloring solution kit II for JEOL (Fujifilm Wako Pure Chemical Industries, Ltd.) Flow rate: Mobile phase 0.42 mL / min, reaction solution 0.22 mL / min Measurement wavelength: 570nm

[0043] Examples 1 to 10 and Comparative Examples 1 to 7 The raw material components were mixed uniformly in a mortar according to the composition shown in Table 1 to obtain a mixed powder. The resulting mixed powder was evaluated for solubility in water and moisture absorption as follows, and the results are shown in Table 1.

[0044] [Evaluation of solubility in water] (1) Dissolution time 100 mg of the mixed powder was taken and placed in a Falcon tube containing 10 mL of ion-exchanged water (25°C), and rotated in a Mix ROTOR (60 r / min, AS ONE Corporation). The time until the powder in the Falcon tube could no longer be visually confirmed was measured and taken as the dissolution time (seconds). (2) Determine remaining melted residue 30 mL of ion-exchanged water (25°C) was weighed into a 50 mL beaker, and 100 mg of the mixed powder was added while stirring at a constant speed with a magnetic stirrer. The mixture was stirred for 10 seconds and then filtered (using a black milk sediment disk). The residue remaining on the filter paper was photographed and binarized using image analysis software (ImageJ). The results were evaluated according to the following criteria. A: 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

[0045] [Evaluation of moisture absorption] (1) Increase in moisture absorption 100 mg of the mixed powder was taken and stored at rest for 4.5 hours in an environment of 40°C and 75% RH. After storage, the mass of the powder was measured and the increase in moisture content was calculated using the following formula. Moisture absorption increase (mass%) = [(total mass after 4.5 hours - container mass) / (initial total mass - container mass)] x 100 (2) Changes in appearance 100 mg of the mixed powder was taken and left to stand for 4.5 hours in an environment of 40°C and 75% RH, after which the change in the appearance of the powder was visually observed and judged according to the following criteria. A: Remains white or has only slight discoloration B: Slight brown discoloration, but within acceptable quality limits C: Discoloration to grayish brown, but within acceptable quality limits D: Black discoloration or deliquescence is observed, resulting in failure.

[0046] [Table 1]

[0047] Example 11 and Comparative Examples 8 to 11 The raw material components were mixed uniformly in a mortar according to the composition shown in Table 2 to obtain a mixed powder. The resulting mixed powder was evaluated for moisture absorption ((1) moisture absorption increase) in the same manner as in Example 1. The results are shown in Table 2.

[0048] [Table 2]

[0049] As is clear from Table 1, Examples 1 to 10, which contain components (A) and (B) at a specific mass ratio, showed shorter dissolution times in water and less residual material than Comparative Example 1. Furthermore, as is clear from Tables 1 and 2, the amount of moisture absorption increases as the amount of component (B) increases, but it was confirmed that Examples 1 to 11, which contain components (A) and (B) at a specific mass ratio, showed a smaller amount of moisture absorption and also showed less change in appearance.

[0050] Prescription example 1 (1) Preparation of coffee bean extract Ground green coffee beans were extracted with hot water and then spray-dried to prepare a powder, which was then dissolved in an aqueous ethanol solution. The filtrate was filtered and processed through a column containing activated carbon and ion exchange resin to prepare a green coffee bean extract. This was then dried into a powder and used in the following procedure. The resulting coffee bean extract powder contained 33% by mass of chlorogenic acids (total of 3-CQA, 4-CQA, 5-CQA, 3-FQA, 4-FQA, and 5-FQA) and 0.006% by mass of caffeine. The mass ratio of caffeine to chlorogenic acids (CQA + FQA) was 0.0002.

[0051] (2) Production of test food A solid test food (300 mg of chlorogenic acids (CQA + FQA) and 100 mg of γ-aminobutyric acid per 1.8 g) was prepared using the coffee bean extract powder produced in (1) above and commercially available GABA (GABA-S; Kyowa Hakko Bio Co., Ltd., GABA content 99% by mass or more) with the composition shown in Table 3.

[0052] [Table 3]

Claims

1. An oral solid preparation containing chlorogenic acids (A) and 0.7% by mass or more of γ-aminobutyric acid (B), in which the content ratio of said components (A) to (B) is 100:7 to 90 by mass (however, excluding oral solid preparations containing yeast β-glucan, poplar flower extract, bamboo shoot bark extract, phytase-producing Bacillus subtilis powder, propolis, and mannose oligosaccharides).

2. 2. The oral solid preparation according to claim 1, wherein the content of the chlorogenic acids (A) in the oral solid preparation is 1 to 91.5% by mass.

3. 3. The oral solid preparation according to claim 1, wherein the content of γ-aminobutyric acid (B) in the oral solid preparation is 0.7 to 47.4% by mass.

4. 3. The oral solid preparation according to claim 1, wherein the content of γ-aminobutyric acid (B) in the oral solid preparation is 3 to 47.4% by mass.

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