Solid composition

Abstract

To provide a solid composition containing coffee bean extract with resistance to color tone change during storage.SOLUTION: A solid composition contains following components (A)-(C): (A) coffee bean extract, (B) a stearate of 1-9 mass%, and (C) a cellulose derivative, where the mass ratio between component (B) and component (C) [(C) / (B)] is 0.03-11.SELECTED DRAWING: None

Description

[Technical field]

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

[0002] In recent years, functional ingredients derived from plants have been attracting attention for the purpose of health promotion, etc. For example, chlorogenic acids, a type of polyphenol, have been reported to have physiological effects such as antioxidant and blood pressure lowering effects, and coffee beans are known as a material that contains a lot of chlorogenic acids. In order to enjoy the physiological functions of chlorogenic acids, it is effective to continuously ingest chlorogenic acids for a long period of time, and one of the forms that can be easily and reasonably ingested is a solid composition containing coffee bean extract. However, solid compositions containing plant extracts are generally prone to color changes due to moisture absorption during storage, and the color change becomes even more noticeable when the plant extract is contained in a high content.

[0003] Various studies have been conducted to suppress color changes in solid compositions containing plant extracts and the like. For example, it has been reported that discoloration over time can be suppressed by adding a stearate salt to an oral composition containing an extract of Onji at a certain ratio to the extract of Onji (Patent Document 1). It has also been reported that discoloration of the extract of Onji due to moisture absorption can be suppressed by adding magnesium stearate and silicon dioxide and / or silicate salt to a tablet containing an extract of Onji (Patent Document 2). It has also been reported that discoloration of the solid preparation containing red yeast rice and / or its processed products can be suppressed by adding calcium stearate to the solid preparation (Patent Document 3). [Prior art documents] [Patent documents]

[0004] [Patent Document 1] JP 2017-75141 A [Patent Document 2] JP 2019-6749 A [Patent Document 3] JP 2022-93587 A Summary of the Invention [Problem to be solved by the invention]

[0005] Thus, prior to filing the present application, it was known that stearates are effective in suppressing color change in solid compositions containing plant extracts and the like, but the present inventors have unexpectedly discovered through their research that the coexistence of coffee bean extract and stearate accelerates color change during storage, which is an action contrary to the above-mentioned prior art. Furthermore, the present inventors have confirmed through their research that the color change is enhanced as the amount of stearate increases. An object of the present invention is to provide a solid composition containing a coffee bean extract which is inhibited from changing in color tone during storage. [Means for solving the problem]

[0006] Means for Solving the Problems The present inventors conducted research in light of the above-mentioned problems and found that by adding a cellulose derivative to a solid composition containing a coffee bean extract and a stearate in a specific quantitative ratio relative to the stearate, it is possible to suppress change in color tone during storage.

[0007] That is, the present invention provides the following [1] to [5]. [1] The following components (A) to (C); (A) Coffee bean extract (B) 1 to 9% by mass of a stearate, and (C) Cellulose derivatives Including, The mass ratio of component (B) to component (C) [(C) / (B)] is 0.03 to 11. Solid composition. [2] The solid composition according to [1] above, wherein component (A) is one or more selected from extracts of green coffee beans and extracts of lightly roasted coffee beans. [3] The content of component (A) in the solid composition is 1) The solid composition according to [1] or [2] above, wherein the content of chlorogenic acids is 3 to 35 mass %. [4] The solid composition according to any one of the above [1] to [3], wherein the component (C) comprises one or more selected from hydroxyalkyl alkyl celluloses and alkyl celluloses. [5] The solid composition according to any one of the above [1] to [4], further comprising an excipient as component (D). Effect of the Invention

[0008] According to the present invention, it is possible to provide a solid composition containing a coffee bean extract, which is inhibited from changing in color tone during storage. DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS

[0009] <Solid composition> (Coffee Bean Extract) The solid composition of the present invention contains a coffee bean extract as component (A). The coffee bean extract may be an extract of green coffee beans or an extract of roasted coffee beans. From the viewpoint of chlorogenic acid content, the roasted coffee bean extract is preferably a lightly roasted coffee bean extract. Here, in the present specification, "lightly roasted coffee beans" refers to roasted coffee beans with an L value of 30 to 60, and "L value" refers to the brightness of the roasted coffee beans measured with a colorimeter, with black being L value 0 and white being L value 100. As the colorimeter, for example, a spectrophotometer SE2000 (manufactured by Nippon Denshoku Co., Ltd.) can be used. In addition, in the present specification, "chlorogenic acids" is a collective term for monocaffeoylquinic acids, which are 3-caffeoylquinic acid, 4-caffeoylquinic acid, and 5-caffeoylquinic acid, and monoferulic acid, which are 3-ferulic acid, 4-ferulic acid, and 5-ferulic acid. In the present invention, at least one of the above six types of chlorogenic acids may be contained. The chlorogenic acids may be in the form of a salt or a hydrate. There is no particular limitation on the salt as long as it is physiologically acceptable, and examples of the salt include alkali metal salts.

[0010] From the viewpoint of the chlorogenic acids content, the L value of the light roasted coffee beans is preferably 33 or more, more preferably 36 or more, and even more preferably 40 or more, and from the viewpoint of flavor, it is preferably 58 or less, and even more preferably 56 or less. The L value of the light roasted coffee beans is preferably 33 to 60, more preferably 36 to 58, and even more preferably 40 to 56. The component (A) may be used alone or in combination of two or more. The type and place of origin of the coffee beans are not particularly limited, and one or more coffee beans of different types and places of origin may be used.

[0011] Among these, as component (A), from the viewpoint of easily enjoying the effects of the present invention, one or more selected from an extract of green coffee beans and an extract of lightly roasted coffee beans are preferable, one or more selected from an extract of green coffee beans and an extract of roasted coffee beans having an L value of 33 to 60 are more preferable, and a green coffee bean extract is even more preferable.

[0012] The extraction method and extraction conditions for the coffee bean extract are not particularly limited, and known methods can be used. The coffee bean extract may be concentrated or dried, and may be purified to increase the purity of chlorogenic acids. Known methods may be used for each of the concentration, drying, and purification methods.

[0013] The content of component (A) can be indexed by the content of chlorogenic acids, which are physiologically functional substances. The content of component (A) is determined by the amount of chlorogenic acids in the solid composition of the present invention from the viewpoint of physiological effects. 1 It is preferable that the content of chlorogenic acids in the solid composition of the present invention is the following amount. 1 The content of chlorogenic acids is preferably 3% by mass or more, more preferably 5% by mass or more, even more preferably 7% by mass or more, and even more preferably 9% by mass or more, from the viewpoint of suppressing color tone change during storage and flavor, and is preferably 35% by mass or less, more preferably 30% by mass or less, and even more preferably 25% by mass or less, from the viewpoint of suppressing color tone change during storage and flavor. 1The content of chlorogenic acids in the solid composition of the present invention is preferably 3 to 35% by mass, more preferably 5 to 30% by mass, even more preferably 7 to 25% by mass, and even more preferably 9 to 25% by mass. 1 The content of chlorogenic acids is defined based on the total amount of the above six types. 1 ) When the chlorogenic acids are in the form of a salt or a hydrate, (A 1 The content of chlorogenic acids is the value converted into the free acid chlorogenic acids. 1 The content of chlorogenic acids can be measured by an analytical method suitable for the condition of the measurement sample among commonly known measurement methods, for example, liquid chromatography. Specifically, the method described in the Examples below can be mentioned. When measuring, the sample may be freeze-dried to fit the detection range of the device, or impurities in the sample may be removed to fit the separation ability of the device, or other appropriate treatment may be performed as necessary.

[0014] The solid composition of the present invention contains a stearate salt as component (B). Component (B) may be used alone or in combination of two or more. Component (B) is not particularly limited as long as it is physiologically acceptable, and examples thereof include metal salts of stearic acid. Examples of metal salts include salts of monovalent metals and salts of divalent metals. Specific examples include potassium stearate, sodium stearate, magnesium stearate, calcium stearate, and zinc stearate. Among these, as component (B), from the viewpoint of easily enjoying the effects of the present invention, one or more selected from magnesium stearate and calcium stearate are preferred, with calcium stearate being more preferred.

[0015] The content of component (B) in the solid composition of the present invention is 1 to 9% by mass, but from the viewpoint of suppressing color tone change during storage, the upper limit of the content of component (B) is preferably 8.5% by mass or less, more preferably 8% by mass or less, and even more preferably 7.3% by mass or less. The content of component (B) in the solid composition of the present invention is preferably 1 to 8.5% by mass, more preferably 1 to 8% by mass, and even more preferably 1 to 7.5% by mass. The lower limit of the content of component (B) may be 1.1% by mass or more, 1.3% by mass or more, or 1.5% by mass or more from the viewpoint of manufacturability.

[0016] The solid composition of the present invention contains a cellulose derivative as component (C). In this specification, the term "cellulose derivative" refers to cellulose having a substituent, and does not include cellulose itself that has no substituent. In the cellulose derivative, it is not necessary that all hydrogen atoms of hydroxyl groups in the monomer unit (glucose) are substituted with a substituent, and it is sufficient that some hydrogen atoms of hydroxyl groups are substituted with a substituent. The number of substituents in the monomer unit is usually 1 to 5, preferably 1 to 3, and more preferably 1 or 2.

[0017] Examples of component (C) include hydroxyalkyl alkyl cellulose, hydroxyalkyl cellulose, carboxyalkyl cellulose, carboxy cellulose, alkyl cellulose, and salts thereof. Component (C) may be used alone or in combination of two or more.

[0018] Examples of the salt include metal salts, acid addition salts, and salts with bases. Examples of the metal salt include salts with monovalent metals (e.g., sodium, potassium) and salts with divalent metals (e.g., calcium, magnesium). Examples of the acid addition salt include salts with inorganic acids (e.g., hydrogen chloride, hydrogen bromide, sulfuric acid, phosphoric acid) and salts with organic acids (e.g., acetic acid, lactic acid, citric acid, tartaric acid, maleic acid, fumaric acid, monomethylsulfuric acid). Examples of the salt with a base include salts with inorganic bases (e.g., ammonia) and salts with organic bases (e.g., ethylenediamine, propylenediamine, ethanolamine, monoalkylethanolamine, dialkylethanolamine, diethanolamine, triethanolamine). As the salt, metal salts are preferred.

[0019] The alkyl in the hydroxyalkyl alkyl cellulose, hydroxyalkyl cellulose, carboxyalkyl cellulose and alkyl cellulose may be linear or branched, and preferably has 1 to 12 carbon atoms, more preferably 1 to 6, and even more preferably 1 to 4. When the alkyl has two or more alkyl groups, they may be the same or different.

[0020] Hydroxyalkyl alkyl cellulose is a cellulose having both a hydroxyalkyl and an alkyl, and examples thereof include hydroxymethyl methyl cellulose, hydroxyethyl methyl cellulose, hydroxypropyl methyl cellulose (HPMC), and hydroxybutyl methyl cellulose.

[0021] Examples of hydroxyalkyl cellulose include hydroxymethyl cellulose, hydroxyethyl cellulose (HEC), hydroxypropyl cellulose (HPC), low-substituted hydroxypropyl cellulose (L-HPC), hydroxybutyl cellulose, hydroxypentyl cellulose, and hydroxyhexyl cellulose.

[0022] Examples of the carboxyalkyl cellulose include carboxymethyl cellulose (CMC), carboxyethyl cellulose, carboxypropyl cellulose, carboxybutyl cellulose, carboxypentyl cellulose, and carboxyhexyl cellulose.

[0023] Examples of alkyl cellulose include methyl cellulose (MC), ethyl cellulose (EC), propyl cellulose, butyl cellulose, pentyl cellulose, and hexyl cellulose.

[0024] Among them, from the viewpoint of suppressing color tone change during storage, component (C) is preferably one or more selected from hydroxyalkyl alkyl cellulose and alkyl cellulose, more preferably hydroxyalkyl alkyl cellulose. As the hydroxyalkyl alkyl cellulose, one or more selected from hydroxymethyl methyl cellulose, hydroxyethyl methyl cellulose, hydroxypropyl methyl cellulose and hydroxybutyl methyl cellulose are preferred. As the alkyl cellulose, one or more selected from methyl cellulose, ethyl cellulose and propyl cellulose are preferred.

[0025] The mass ratio of component (B) to component (C) [(C) / (B)] is 0.03 to 11, and from the viewpoint of suppressing color tone change during storage, it is preferably 0.04 or more, more preferably 0.05 or more, and preferably 10.5 or less, more preferably 9.5 or less, even more preferably 9.0 or less, and even more preferably 8.5 or less. Such a mass ratio [(C) / (B)] is preferably 0.04 to 10.5, more preferably 0.05 to 9.5, even more preferably 0.05 to 9.0, and even more preferably 0.05 to 8.5.

[0026] In addition, the total content of the components (B) and (C) [(C)+(B)] is preferably 20% by mass or less, more preferably 18% by mass or less, even more preferably 17% by mass or less, and even more preferably 16.5% by mass or less in the solid composition of the present invention from the viewpoint of suppressing color tone change during storage. The lower limit of the total content [(C)+(B)] is preferably 1.1% by mass or more, more preferably 1.3% by mass or more, and even more preferably 1.5% by mass or more in terms of manufacturability. In addition, the total content [(C)+(B)] is preferably 1.1 to 20% by mass, more preferably 1.3 to 18% by mass, even more preferably 1.5 to 17% by mass, and even more preferably 1.5 to 16.5% by mass in the solid composition of the present invention.

[0027] The content of component (C) is not particularly limited as long as it satisfies the above-mentioned mass ratio [(C) / (B)], but from the viewpoint of suppressing color tone change during storage, it is preferably 0.1 mass% or more in the solid composition of the present invention, more preferably 0.2 mass% or more, and even more preferably 0.3 mass% or more, and from the viewpoint of manufacturability, it is preferably 12.5 mass% or less, more preferably 11 mass% or less, even more preferably 9.5 mass% or less, and even more preferably 9 mass% or less. The content of component (C) in the solid composition of the present invention is preferably 0.1 to 12.5 mass%, more preferably 0.3 to 11 mass%, even more preferably 0.5 to 9.5 mass%, and even more preferably 0.5 to 9 mass%.

[0028] The solid composition of the present invention may contain an excipient as component (D) in order to make it solid. Component (D) may be used alone or in combination of two or more. Examples of the component (D) include organic excipients and inorganic excipients. Examples of organic excipients include lactose, starch, and sugar alcohols. Examples of inorganic excipients include sodium chloride, aluminum silicate, calcium silicate, silicon dioxide, light anhydrous silicic acid, calcium sulfate, and calcium hydrogen phosphate. Among these, as component (D), from the viewpoint of easily enjoying the effects of the present invention, an organic excipient is preferred, and it is preferable that the excipient contains one or more selected from sugar alcohols and starches, and it is preferable that the excipient contains a sugar alcohol.

[0029] Examples of sugar alcohols include monosaccharide alcohols, disaccharide alcohols, and trisaccharide or higher alcohols. The sugar alcohols may be used alone or in combination of two or more. Examples of monosaccharide alcohols include pentitols such as erythritol and xylitol, and hexitols such as sorbitol and mannitol. Examples of disaccharide alcohols include reduced maltose (maltitol), lactitol (reduced lactose), reduced palatinose (isomalt), trehalose, and palatinose. Examples of trisaccharide or higher alcohols include maltotriitol, isomaltotriitol, and panitol. Among these, as the sugar alcohol, one or more selected from monosaccharide alcohols and disaccharide alcohols are preferred, disaccharide alcohols are more preferred, and reduced maltose (maltitol) is even more preferred, in terms of making it easier to enjoy the effects of the present invention.

[0030] The starch is not particularly limited as long as it is starch extracted from a plant or processed starch (hereinafter also referred to as "processed starch") and is edible. The starch may be used alone or in combination of two or more. Examples of starches extracted from plants include corn starch, wheat starch, rice starch, potato starch, sweet potato starch, and tapioca starch. The starches extracted from plants may be purified by known methods, if necessary.

[0031] Examples of processed starches include those obtained by subjecting raw starch to a crosslinking treatment such as hydrolysis, esterification or etherification, as well as oxidation, gelatinization, heating, moist heat treatment, bleaching, sterilization, acid treatment, alkali treatment, enzyme treatment, etc. A specific example of processed starch is dextrin. In this specification, "dextrin" refers to raw starch decomposed with an enzyme or acid. Dextrose equivalent (DE value) is generally used as an index for grasping the degree of decomposition of raw starch, and the DE value of the dextrin used in the present invention is preferably 2 to 30, more preferably 2 to 13, and even more preferably 2 to 5, from the viewpoint of easily enjoying the effects of the present invention. The DE value can be analyzed by a commonly known method for measuring dextrose, and an example of this can be the Wilstetter-Schudel method. Dextrin has a molecular structure in which sugars are polymerized through glycosidic bonds, and the glycosidic bonds may be linear, cyclic, or a mixture of these. The sugar bonds may be α-1,4, α-1,6, β-1,2, β-1,3, β-1,4, or β-1,6, and may be a single bond or two or more bond types.

[0032] Among these, dextrin is preferred as the starch, since it is easy to obtain the effects of the present invention.

[0033] The content of component (D) is usually the remainder obtained by subtracting the total content of components (A), (B) and (C) and other components from the total amount of the solid composition of the present invention. For example, the content of component (D) in the solid composition of the present invention is preferably 20% by mass or more, more preferably 25% by mass or more, even more preferably 30% by mass or more, and preferably 85% by mass or less, more preferably 80% by mass or less, and even more preferably 75% by mass or less, in terms of the ease of enjoying the effects of the present invention. The content of component (D) in the solid composition of the present invention is 20 to 85% by mass, more preferably 25 to 80% by mass, and even more preferably 30 to 75% by mass.

[0034] The solid composition of the present invention may contain other ingredients to enhance palatability. The other ingredients are not particularly limited as long as they are ingredients that are acceptable in final products such as food and beverage products and pharmaceuticals and can be orally ingested, and examples thereof include flavoring agents such as sweeteners and acidulants, vitamins, minerals, antioxidants, lubricants, and flavoring agents. In addition, in order to improve the fluidity of the powder mixture, a fluidizing agent such as talc, silicon dioxide, or magnesium aluminometasilicate may be contained. The other ingredients may be used alone or in combination of two or more. The content of the other ingredients may be appropriately set within a range that does not impair the object of the present invention.

[0035] The solid composition of the present invention is solid at room temperature (20°C ± 15°C), and its form is not particularly limited, and it may be in any suitable form such as powder, granules, tablets, rods, plates, blocks, etc. Here, in this specification, "granules" refers to a solid having a median diameter of 0.5 to 2.0 mm, and "powder" refers to a solid having a smaller median diameter than granules. In addition, "median diameter" refers to the particle diameter (D) corresponding to a frequency of 50% in a cumulative distribution based on volume. 50 The particle size distribution can be measured using a laser diffraction / scattering type particle size distribution measuring device.

[0036] The moisture content of the solid composition of the present invention is preferably 6% by mass or less, more preferably 4% by mass or less, and even more preferably 3% by mass or less, from the viewpoint of suppressing color tone change during storage. The lower limit of the moisture content of the solid composition is not particularly limited, and may be 0% by mass. Here, in this specification, the "moisture content" refers to the value calculated from the mass loss when 5 g of a sample is dried at 105°C for 15 minutes using an infrared moisture meter. As the infrared moisture meter, for example, the FD-660 manufactured by Kett Electric Laboratory Co., Ltd. can be used.

[0037] The solid composition of the present invention may be provided as a food or drink, or as a pharmaceutical for oral administration, but is preferably a food or drink.Product forms include, for example, supplements, powders, tablets, and granules.Among them, powders, tablets, and granules are preferred, and tablets are more preferred, in that they are easy to enjoy the effects of the present invention.

[0038] The solid composition of the present invention may be contained in a container or bag, for example, a container or bag made of paper, plastic, glass, or metal. It may also be packaged in small portions for each oral intake. Among these, a form in which the composition is packaged in small portions for each oral intake (stick packaging, individual sachet packaging, etc.) is preferred. The packaging material is not limited as long as it is normally used for food or medicine, and may be, for example, a combination of aluminum foil, synthetic resin (polyethylene terephthalate, etc.), laminated paper, etc. The container and packaging material may be filled with nitrogen gas from the viewpoint of maintaining quality.

[0039] The solid composition of the present invention is suppressed from changing in color tone during storage. Specifically, for example, when the solid composition of the present invention is placed in a low-density polyethylene bag and stored for 9 hours under an atmosphere of 40° C. and 75% relative humidity, the L of the solid composition after storage is * Value, a * value and b * value and the L value of the solid composition before storage (e.g., immediately after production) * Value, a * value and b * From the value, the value (ΔE * ab ) can be preferably less than 7, more preferably 6 or less, and even more preferably 5 or less.

[0040] ΔE * ab = [(ΔL * ) 2 +(Δa * ) 2 +(Δb * ) 2 ] 1 / 2 (I) [In the formula, ΔL* , Δa * and Δb * is a value calculated by the following formula. ΔL * = (L of solid composition after storage * value)-(L value of solid composition before storage * value) Δa * = (a of the solid composition after storage * a value)-(a value of the solid composition before storage * value) ΔL * = (b of solid composition after storage * value)-(b value of solid composition before storage * value)〕

[0041] <Method of producing solid composition> The solid composition of the present invention can be produced by an appropriate method depending on the form of the composition. A method for producing tablets, which is a preferred embodiment, will be described below. The tablets may be produced, for example, by tableting a mixture containing the granulated material and a stearate salt. The granulated product can be produced by a known method, but a wet granulation method is preferred. As the wet granulation method, a fluidized bed granulation method is preferred from the viewpoints of suppressing color change during storage and improving tableting properties. The fluidized bed granulation method is a granulation method in which hot air is blown into a fluidized bed granulation device, the powder raw material is stirred up in the air, and a binder liquid is sprayed onto the powder raw material, which is then grown into granules by agglomeration or coating. Therefore, in fluidized bed granulation, hot air is blown from below the granulation layer in the fluidized bed granulation device, the powder raw material is stirred up in the air, and the powder raw material is fluidized, and a binder liquid is sprayed onto the powder raw material from a spray nozzle.

[0042] The fluidized bed granulation apparatus is not particularly limited as long as it is one that is normally used for fluidized bed granulation, but examples thereof include an apparatus equipped with a granulation tank for accommodating, granulating, and drying the material to be treated, a hot air supplying device for supplying hot air for fluidizing the material to be treated, and a spray nozzle for spraying a liquid onto the material to be treated. Examples of such fluidized bed granulation apparatus include Flowcoater (manufactured by Freund Corporation), GPCG-CT series, WST / WSG series, BF series, pulse fluidized bed granulation dryer, and MP series (all manufactured by Powrex Corporation).

[0043] The powdered raw materials include at least a coffee bean extract and an excipient. The powdered raw materials may be charged into the fluidized bed granulator individually or mixed together. The mixing method is not particularly limited as long as the raw materials can be mixed uniformly, and may be hand mixing or using a mixer. Examples of the mixer include a container mixer, a V-type mixer, a ribbon type mixer, and a high-speed stirring mixer (high-speed mixer). The mixing temperature is not particularly limited, but is usually 10 to 35°C, and preferably 15 to 25°C. The mixing time is also not particularly limited, but is usually 0.5 to 10 minutes, and preferably 1 to 5 minutes.

[0044] The binding liquid usually contains an aqueous medium. Examples of the aqueous medium include water, ethanol, and a mixture of water and ethanol (aqueous ethanol solution). When an aqueous ethanol solution is used, the mixing ratio of water and ethanol is not particularly limited and can be selected appropriately. The aqueous ethanol solution may be a commercially available ethanol preparation or alcohol. The alcohol is not particularly limited as long as it is edible. For example, there are those produced by the alcohol fermentation action of yeast from natural raw materials containing starch and sugars, or those containing these components, and liquids containing ethanol can be used, such as sake, shochu, wine, whiskey, brandy, and other alcoholic beverages, and fermented seasonings such as mirin.

[0045] The binding liquid may contain all or a part of the cellulose derivative. In particular, from the viewpoint of further suppressing color change during storage, it is preferable that the binding liquid contains the entire amount of the cellulose derivative. When the binding liquid contains a part of the cellulose derivative, the content can be appropriately selected, and the remainder can be contained in the powder raw material.

[0046] The concentration of the cellulose derivative in the binding liquid can be appropriately selected, but is usually 1 to 25% by mass, preferably 1.5 to 20% by mass, and more preferably 2 to 15% by mass.

[0047] The hot air to be blown in to fluidize the powder raw material can be air, but it may also be an inert gas such as nitrogen or carbon dioxide, or a mixed gas containing an inert gas. Using an inert gas or a mixed gas as the hot air can prevent deterioration due to oxidation.

[0048] The hot air temperature can be appropriately selected, but from the viewpoints of suppressing color change during storage and improving tableting properties, it is usually 60 to 95°C, preferably 65 to 90°C, and more preferably 70 to 95°C.

[0049] The spray rate can be appropriately selected, but from the viewpoints of suppressing color change during storage and improving tableting properties, it is usually 2 to 8 mL / min, preferably 3 to 7 mL / min, and more preferably 4 to 5 mL / min. The spray pressure can be appropriately selected, but from the viewpoints of suppressing color change during storage and improving tableting properties, it is usually 0.1 to 0.3 MPa, and preferably 0.13 to 0.2 MPa.

[0050] After the fluidized bed granulation, the granulated product may be dried and, if necessary, sized. Drying may be performed simultaneously with granulation. The granulated product may be dried by a conventional drying method. Examples of the dryer include a thermostatic dryer, a forced air dryer, a fluidized bed dryer, a reduced pressure dryer, and a vacuum dryer. The drying conditions can be appropriately set. In addition, sizing may be performed by screening the granulated product using a sieve to control the particle size to a desired size.

[0051] Next, the mixture containing the granulated material and the stearate is compressed into tablets. Tableting can be carried out by any known method, including, for example, an internal lubrication method and an external lubrication method. Among these, the internal lubrication method is preferred in that it is easier to obtain the effects of the present invention. For tableting, a known tablet press can be used, for example, a single punch tablet press, a rotary tablet press, or a high-speed rotary tablet press.

[0052] The mass of each tablet is usually 0.05 to 3 g from the viewpoint of the effectiveness of component (A).

[0053] Tablets can be produced in this manner, and the following method is a suitable method for producing tablets. The following steps (a) and (b); (a) a granulation step in which hot air is blown into a fluidized bed granulator, and a binder is sprayed onto the fluidized powder raw material to obtain a granulated product; and (b) A tableting step for tableting a mixture containing the granulated material and a stearate salt. Equipped with A method for producing tablets, wherein the powdered raw materials include a coffee bean extract and an excipient, and the binder includes a cellulose derivative and an aqueous medium. EXAMPLES

[0054] The present invention will be described in more detail below with reference to examples and comparative examples, but the present invention is not limited to these examples.

[0055] 1. Analysis of chlorogenic acids The sample solution was filtered through a filter (0.45 μm), and a high-performance liquid chromatograph (model LC-20 Prominence, Shimadzu Corporation) was used with a column [Cadenza CD-C18 (3 μm, 4.6 mmφ × 150 mm, Imtakt)] attached, and the gradient method was performed at a column temperature of 35°C. The mobile phase A solution was a 5% acetonitrile solution containing 0.05 mol / L acetic acid, 0.01 mol / L sodium acetate, and 0.1 mmol / L HEDPO, and the B solution was an acetonitrile solution. The flow rate was 1 mL / min, the sample injection amount was 10 μL, and the UV detector wavelength was 325 nm. The gradient conditions were as follows.

[0056] Concentration gradient conditions Time (min) A solution concentration (volume %) B solution concentration (volume %) 0 100% 0% 10 100% 0% 15 95% 5% 20 95% 5% 22 92% 8% 50 92% 8% 52 10% 90% 60 10% 90% 60.1 100% 0% 70 100% 0%

[0057] 3-Caffeoylquinic acid: 5.3min 5-Caffeoylquinic acid: 8.8min 4-Caffeoylquinic acid: 11.6 min 3-Ferulacinic acid: 13.0 min 5-Ferulacinic acid: 19.9 min 4-Ferulacinic acid: 21.0 min From the area % calculated here, the content (mass %) of chlorogenic acids was calculated using 5-caffeoylquinic acid (Tokyo Chemical Industry Co., Ltd.) as a standard substance.

[0058] 2. Analysis of stearates Analysis of stearates is performed according to the following method described in the Japanese Pharmacopoeia, 18th Edition. Prepare the analytical sample solution according to the following procedure. Place 1.0 g of sample in a small conical flask equipped with a reflux condenser. Add 5.0 mL of boron trifluoride-methanol TS, shake and heat and stir for approximately 10 minutes until completely dissolved. Next, add 4 mL of heptane from the top of the reflux condenser, heat and stir for 10 minutes, then cool. After cooling, add 20 mL of saturated sodium chloride solution, shake and leave to separate the liquid into two layers. Of the two separated layers, take the heptane layer (upper layer) and transfer it to another flask through approximately 0.1 g of anhydrous sodium sulfate that has been washed with heptane beforehand. Place 1.0 mL of this liquid in a 10 mL measuring flask, add heptane to make 10 mL, and use this as the sample solution for analysis. Perform the test by gas chromatography under the following conditions.

[0059] The analytical equipment configuration is as follows: Detector: Flame ionization detector Column: A fused silica tube with an inner diameter of 0.32 mm and a length of 30 m, the inner surface of which is coated with polyethylene glycol 15000-diepoxide for gas chromatography to a thickness of 0.5 μm.

[0060] The analysis conditions are as follows. Column temperature: After injection, keep at 70°C for 2 minutes, then increase the temperature to 240°C at 5°C per minute, and hold at 240°C for 5 minutes. Inlet temperature: constant temperature around 220℃ Detector temperature: constant temperature around 260℃ Carrier gas: Helium Flow rate: 2.4mL per minute ·Injection volume: 1μL Splitless

[0061] 3. Analysis of cellulose derivatives The cellulose derivatives were analyzed by HPLC (high performance liquid chromatography) according to the following method. The analytical equipment configuration is as follows: Detector: Shodex RI Column: Shodex OHpac SB-806M HQ (8.0 mm ID x 300 mm) x 2 (Resonac Corporation)

[0062] The analysis conditions are as follows. Column temperature: 40℃ ·Mobile phase: 0.1M NaClaq. ·Flow rate: 1mL / min Sample injection volume: 20μL

[0063] 4. Analysis of sugar alcohols The sugar alcohols were analyzed by HPLC (high performance liquid chromatography) according to the following method. The analytical equipment configuration is as follows: Detector: Differential refractometer RID-10A (Shimadzu Corporation) Column: Shodex Asahipak NH2P-50 4E, φ4.6mm×250mm (Resonac Corporation)

[0064] The analysis conditions are as follows. Column temperature: Room temperature Mobile phase: A mixture of acetonitrile and water (81:19 volume ratio) ·Flow rate: 1mL / min Sample injection volume: 20μL

[0065] The analytical sample solution was prepared according to the following procedure. 3 g of sample was weighed out, dissolved and neutralized with 10 mL of water, and ultrasonic extraction was performed for 30 minutes using an ultrasonic cleaner. Water was added to the solution to make a constant volume of 20 mL. The solution was filtered through a membrane filter to prepare a sample solution for analysis. The sample solution for analysis was subjected to high performance liquid chromatography analysis.

[0066] 5. Evaluation of the effect of suppressing color change The tablets were placed in a low-density polyethylene bag (Unipack A-4, manufactured by Nippon Seisakusho Co., Ltd.) and stored for 9 hours under an atmosphere of 40°C and 75% relative humidity. The tablets immediately after production and after 9 hours of storage were measured for L using a spectrophotometer (CM-5, manufactured by Konica Minolta, Inc.) using the SCE method. * Value, a * value and b * The color difference (ΔE * ab ) was sought.

[0067] ΔE * ab = [(ΔL * ) 2 +(Δa * ) 2 +(Δb * ) 2 ] 1 / 2 (II) [In the formula, ΔL * , Δa * and Δb * is a value calculated by the following formula. ΔL * = (L of tablets after storage) * value)-(L of tablets before storage * value) Δa * = (a of tablets after storage) * value)-(a of tablets before storage * value) Δb * = (b of tablets after storage) * value)-(b of tablets before storage * value)〕

[0068] 6.Raw materials The raw materials used in this example are shown below. (1) Calcium stearate Calcium stearate (vegetable-based) (manufactured by Taihei Chemical Industry Co., Ltd.) (2) Cellulose derivatives Hydroxypropyl methylcellulose (HPMC): Metolose SE-03 (Shin-Etsu Chemical Co., Ltd.) Methylcellulose (MC): Metolose MCE-4 (Shin-Etsu Chemical Co., Ltd.) (3) Maltitol Resis fine powder (manufactured by Mitsubishi Corporation Life Sciences Ltd.) (4) Silicon dioxide Carplex FPS-500 (manufactured by Evonik Japan Co., Ltd.)

[0069] Manufacturing Example 1 Green Coffee Bean Extract 45g of unground Robusta coffee beans with an L value of 50 were placed in a container with a volume of 208cm 3 The column was then filled with 100 ml of ethanol. The solution was then passed through the column at a rate of 2 [hr -1 Next, after closing the supply valve at the bottom of the column, hot water at 80°C was fed from the shower nozzle at the top at a flow rate of 2 [hr ―1 ] and a flow rate of 12 (w / w), and at the same time, the discharge valve below the column was opened to obtain an extract. The extract was concentrated under reduced pressure using an evaporator (Tokyo Rikakikai Co., Ltd., N-1100V) to obtain a concentrate. The concentrate was then diluted with ion-exchanged water to obtain a diluted solution with a solid content of 1.7% by mass. The diluted solution was then passed through a column packed with 10.4 g of activated carbon (Kuraray Chemical Co., Ltd., Kuraray Coal GW) at a flow rate of 7 [hr -1 The activated carbon-treated liquid was then passed through a spray dryer (manufactured by Yamato Scientific Co., Ltd., DL-41) at an intake temperature of 180°C and a flow rate of 0.9 m 3 The mixture was dried at a spray pressure of 0.1 MPa and a liquid flow rate of 23 g / min to obtain a powdered green coffee bean extract. The green coffee bean extract had a chlorogenic acid content of 43.6% by mass in the solid matter.

[0070] Preparation Example 1 (1) Preparation of binding solution (i) Hydroxypropyl methylcellulose in the amount shown in Table 1 was dissolved in water to prepare a binding solution (i) having a hydroxypropyl methylcellulose concentration shown in Table 1. (2) Preparation of granules (i) The amounts of green coffee bean extract and maltitol shown in Table 1 were charged into a fluidized bed granulator (FLOW COATER FL-LABO, manufactured by Freund Corporation). Next, the intake air temperature was set at 80°C and the intake air volume was set at 0.3 m 3 Air was blown into the device at a pulse pressure of 0.36 MPa to fluidize the green coffee bean extract and maltitol, and the binding liquid (i) in the amount shown in Table 1 was sprayed at a spray speed of 4.5 mL / min, a spray pressure of 0.18 MPa, and a spray flow rate of 30 NL / min to granulate the mixture. 3 The mixture was dried for 10 minutes while air was being blown into the apparatus at a rate of 0.36 MPa / min and a pulse pressure of 0.36 MPa, and then sieved through a 30 mesh sieve to obtain granulated material (i).

[0071] Preparation Examples 2 to 4 (1) Preparation of binding solutions (ii) to (iv) Binding solutions (ii) to (iv) having the hydroxypropyl methylcellulose concentrations shown in Table 1 were prepared in the same manner as in Preparation Example 1, except that the amounts of hydroxypropyl methylcellulose shown in Table 1 were used. (2) Preparation of granules (ii) to (iv) Granulated materials (ii) to (iv) were obtained by the same procedure as in Preparation Example 1, except that the amounts of green coffee bean extract and maltitol shown in Table 1 were used and the amounts of binding liquid (ii) to (iv) shown in Table 1 were sprayed.

[0072] Preparation Example 5 (1) Preparation of binding solution (v) A binding solution (v) having a methylcellulose concentration shown in Table 1 was prepared in the same manner as in Preparation Example 1, except that the amount of methylcellulose shown in Table 1 was used instead of hydroxypropylmethylcellulose. (2) Granule (v) preparation Granulated material (v) was obtained by the same procedure as in Preparation Example 1, except that the amounts of green coffee bean extract and maltitol shown in Table 1 were used and the amount of binding liquid (v) shown in Table 1 was sprayed.

[0073] Comparative Preparation Example 1 (1) Preparation of binding solution (vi) Water was used as the binding liquid (vi). (2) Preparation of granules Granulated material (vi) was obtained by the same procedure as in Example 1, except that the amounts of green coffee bean extract and maltitol shown in Table 1 were used and the amount of binding liquid (vi) shown in Table 1 was sprayed.

[0074] [Table 1]

[0075] Example 1 89.3 parts by mass of the granulated material (i) was placed in a polyethylene bag (Unipack I-4, manufactured by Seizo Nippon Co., Ltd.), 0.9 parts by mass of silicon dioxide was added thereto, and 9.8 parts by mass of calcium stearate and maltitol were added in total so as to obtain the final composition shown in Table 2, and then the mixture was mixed by hand to prepare a mixture. The obtained mixture was then compressed under the following conditions to produce tablets having the composition shown in Table 2. The obtained tablets were analyzed and evaluated. The results are shown in Table 2.

[0076] Tableting conditions Tablet press: Mini Press Kit CDM-5M (manufactured by Riken Machinery Co., Ltd.) Tablet weight: 400mg ·Pinch diameter, shape: φ10, R13 ·Tableting pressure: 10MPa

[0077] Examples 2 to 3 and Comparative Example 1 A mixture was prepared in the same manner as in Example 1, except that the type of granulated material and the amount of cellulose derivative were changed according to Table 2. Then, a tablet having the composition shown in Table 2 was manufactured in the same manner as in Example 1, except that this mixture was used. The obtained tablets were analyzed and evaluated. The results are shown in Table 2. [Table 2]

[0078] Examples 4 to 9 and Comparative Examples 2 to 4 A mixture was prepared in the same manner as in Example 1, except that the type of granulated material and the blending amounts of the stearate salt and the cellulose derivative were changed according to Table 3. Then, a tablet having the composition shown in Table 3 was manufactured in the same manner as in Example 1, except that this mixture was used. The obtained tablets were analyzed and evaluated. The results are shown in Table 3.

[0079] [Table 3]

[0080] Examples 10 to 12 and Comparative Example 5 A mixture was prepared in the same manner as in Example 1, except that the types of granules and cellulose derivative, and the blending amounts of stearate and cellulose derivative were changed according to Table 4. Then, a tablet having the composition shown in Table 4 was manufactured in the same manner as in Example 1, except that this mixture was used. The obtained tablets were analyzed and evaluated. The results are shown in Table 4.

[0081] [Table 4]

[0082] Examples 13 to 16 A mixture was prepared in the same manner as in Example 1, except that the type of granules, and the amounts of green coffee extract, stearate, and cellulose derivative were changed according to Table 5. Then, tablets having the composition shown in Table 5 were manufactured in the same manner as in Example 1, except that this mixture was used. The obtained tablets were analyzed and evaluated. The results are shown in Table 5.

[0083] [Table 5]

[0084] Examples 17 to 19 A mixture was prepared in the same manner as in Example 1, except that the type of granulated material and the blending amounts of the stearate salt and the cellulose derivative were changed according to Table 6. Then, a tablet having the composition shown in Table 6 was manufactured in the same manner as in Example 1, except that this mixture was used. The obtained tablets were analyzed and evaluated. The results are shown in Table 6.

[0085] [Table 6]

[0086] It can be seen from Tables 1 to 6 that by adding a specific ratio of a cellulose derivative to a stearate to a solid composition containing a coffee bean extract and a stearate, the change in color tone during storage can be suppressed.

Claims

1. The following components (A) to (C): (A) Coffee bean extract (B) Stearate 1 to 9% by mass, and (C) Cellulose derivative Includes, The mass ratio of component (B) to component (C) [(C) / (B)] is between 0.03 and 11. Solid composition.

2. The solid composition according to claim 1, wherein component (A) is one or more selected from green coffee bean extract and light roast coffee bean extract.

3. The content of component (A) is the amount of (A) in the solid composition. １ The solid composition according to claim 1 or 2, wherein the chlorogenic acid content is 3 to 35% by mass.

4. The solid composition according to claim 1 or 2, wherein component (C) comprises one or more selected from hydroxyalkylalkylcellulose and alkylcellulose.

5. The solid composition according to claim 1 or 2, further comprising an excipient as component (D).