Particulate components

A granular composition with 18% or more of 212 μm particles by mass addresses high hygroscopicity and adhesion issues, enhancing storage stability and handling through controlled production methods and materials.

JP2026061752APending Publication Date: 2026-04-09ROHTO PHARM CO LTD
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Patent Information

Authority / Receiving Office
JP · JP
Patent Type
Applications
Current Assignee / Owner
Filing Date
2024-09-30
Publication Date
2026-04-09

AI Technical Summary

Technical Problem

Existing granular compositions containing ascorbic acid exhibit high hygroscopicity and adhesion to containers, particularly when the mass of powder particles with a diameter of 212 μm or less is less than 18% of the total mass.

Method used

A granular composition with a mass of powder particles with a diameter of 212 μm or less being 18% or more of the total mass, produced through methods like extrusion granulation, exhibits reduced moisture absorption and adhesion to containers, using specific production conditions and materials such as polyolefin and polyester containers.

Benefits of technology

The composition effectively suppresses moisture absorption and adhesion to containers, improving handling and storage stability.

✦ Generated by Eureka AI based on patent content.

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Abstract

The present invention aims to provide a granular composition containing ascorbic acid or a salt thereof that suppresses moisture absorption and prevents adhesion to containers or other objects it comes into contact with. [Solution] A granular composition containing ascorbic acid or a salt thereof, When a granular strength test is performed on the above granular composition, the mass of powder particles with a diameter of 212 μm or less is 18% or more of the total mass of the granular composition before the granular strength test. The granular strength test described above involves placing a sieve with an inner diameter of 75 mm and a mesh size of 710 μm below a sieve with an inner diameter of 75 mm and a mesh size of 212 μm, then placing four stainless steel balls with a diameter of 11.1 mm and 2 g of the granular composition on top of the sieve with a mesh size of 710 μm, and shaking at 290 rpm for 6 minutes.
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Description

Technical Field

[0001] The present invention relates to a granular composition.

Background Art

[0002] L-ascorbic acid is also called vitamin C and is generally known to have various physiological activities in the living body, such as the production of collagen, antioxidant activity, whitening activity, anti-inflammatory activity, and anti-cancer activity. On the other hand, although L-ascorbic acid has such important and excellent properties, humans cannot synthesize L-ascorbic acid in the body. Therefore, humans need to ingest L-ascorbic acid from outside the body through diet and supplements. However, in many cases, sufficient amounts of L-ascorbic acid cannot be ingested only through diet, and attention has been focused on the use of compositions containing L-ascorbic acid, such as L-ascorbic acid supplements. Against this background, various compositions containing ascorbic acid have been developed.

[0003] As a composition containing ascorbic acid, for example, Patent Document 1 discloses an oral composition containing vitamins B1, C, and D, in which discoloration during storage is suppressed. Patent Document 1 also discloses that the vitamin C may be ascorbic acid.

Prior Art Documents

Patent Documents

[0004]

Patent Document 1

Summary of the Invention

Problems to be Solved by the Invention

[0005] The inventors have found that a granular composition containing ascorbic acid in which the mass of powder particles with a diameter of 212 μm or less, generated when a specific granular strength test is performed, is less than 18% of the total mass of the granular composition before the granular strength test, has room for improvement in terms of hygroscopicity and adhesion to containers, etc.

[0006] Therefore, the present invention aims to provide a granular composition containing ascorbic acid or a salt thereof that suppresses moisture absorption and prevents adhesion to containers or other objects it comes into contact with. [Means for solving the problem]

[0007] As a result of diligent research, the present inventors have discovered that a granular composition containing ascorbic acid in which the mass of powder particles with a diameter of 212 μm or less, generated during a specific granular strength test, is 18% or more of the total mass of the granular composition before the granular strength test, exhibits lower levels of moisture absorption and adhesion to specific containers, etc., compared to a granular composition containing ascorbic acid in which the above value is less than 18%, leading to the completion of the present invention.

[0008] In other words, this disclosure relates, for example, to the following: [1] A granular composition containing ascorbic acid or a salt thereof, When a granular strength test is performed on the above granular composition, the mass of powder particles with a diameter of 212 μm or less is 18% or more of the total mass of the granular composition before the granular strength test. The granular strength test described above involves placing a sieve with an inner diameter of 75 mm and a mesh size of 710 μm below a sieve with an inner diameter of 75 mm and a mesh size of 212 μm, then placing four stainless steel balls with a diameter of 11.1 mm and 2 g of the granular composition on top of the sieve with a mesh size of 710 μm, and shaking at 290 rpm for 6 minutes. [2] A granular composition containing ascorbic acid or a salt thereof, When a granular strength test is performed on the above granular composition, the mass of powder particles with a diameter of 212 μm or less is 18% or more of the total mass of the granular composition before the granular strength test. The above granular strength test is performed by placing a sieve with an inner diameter of 75 mm and a mesh opening of 212 μm below a sieve with an inner diameter of 75 mm and a mesh opening of 710 μm, then placing four stainless steel balls with a diameter of 11.1 mm and 2 g of the above granular composition on top of the sieve with a mesh opening of 710 μm, and shaking at 290 rpm for 6 minutes. The granular composition is the same composition as the above granular composition, and the granular composition exhibits reduced adhesion compared to a granular composition in which the mass of powder with a particle size of 212 μm or less, generated when the above granular strength test is performed on the said granular composition, is less than 18% of the total mass of the granular composition before the above granular strength test. [3] A granular composition containing ascorbic acid or a salt thereof, When a granular strength test is performed on the above granular composition, the mass of powder particles with a diameter of 212 μm or less is 18% or more of the total mass of the granular composition before the granular strength test. The above granular strength test is performed by placing a sieve with an inner diameter of 75 mm and a mesh opening of 212 μm below a sieve with an inner diameter of 75 mm and a mesh opening of 710 μm, then placing four stainless steel balls with a diameter of 11.1 mm and 2 g of the above granular composition on top of the sieve with a mesh opening of 710 μm, and shaking at 290 rpm for 6 minutes. The granular composition is the same composition as the above granular composition, and the granular composition exhibits reduced moisture absorption compared to a granular composition in which the mass of powder with a particle size of 212 μm or less, generated when the above granular strength test is performed on the said granular composition, is less than 18% of the total mass of the granular composition before the above granular strength test. [4] A granular composition according to any one of [1] to [3], which is a granulated product. [5] The granular composition according to [4], wherein the granules are extruded granules. [6] A granular composition according to any one of [1] to [5], containing 10% by mass or more of the above-mentioned ascorbic acid or a salt thereof. [7] A granular composition according to any one of [1] to [6], further containing a sugar alcohol. [8] A granular composition according to any one of [1] to [7], further containing starch. [9] A granular composition according to any one of [1] to [8], containing 10 to 80% by mass of ascorbic acid or a salt thereof, 5 to 70% by mass of sugar alcohol, and 10 to 50% by mass of starch.

[10] The granular composition according to any one of [1] to [9], wherein the granular composition is housed in a container in which part or all of the part in contact with the granular composition is made of polyolefin and / or polyester. [Effects of the Invention]

[0009] According to the present invention, it is possible to provide a granular composition containing ascorbic acid or a salt thereof in which moisture absorption is suppressed and adhesion to containers or other objects in contact is suppressed. [Modes for carrying out the invention]

[0010] The embodiments for carrying out the present invention will be described in detail below. However, the present invention is not limited to the following embodiments. Note that the numerical range indicated by the symbol "~" includes the lower limit and the upper limit. That is, the numerical range indicated by "x~y" means x or greater and y or less.

[0011] In the granular composition containing ascorbic acid or a salt thereof according to this embodiment, the mass of powder with a particle diameter of 212 μm or less, generated when a specific granular strength test is performed on the granular composition, is 18% or more of the total mass of the granular composition before the granular strength test.

[0012] As described above, the granular composition according to this embodiment exhibits suppressed moisture absorption and adhesion to containers, etc., compared to a granular composition in which the mass of powder with a particle diameter of 212 μm or less, generated when a specific granular strength test is performed, is less than 18% of the total mass of the granular composition before the granular strength test. Specifically, for example, if the former granular composition absorbs less moisture and adheres to containers, etc., compared to the latter granular composition, by less than 1, 0.9 or less, 0.8 or less, 0.7 or less, 0.6 or less, 0.5 or less, 0.4 or less, 0.3 or less, 0.2 or less, or 0.1 or less, it can be determined that moisture absorption and adhesion to containers, etc., are suppressed. Suppression of moisture absorption and adhesion to containers, etc., can be determined, for example, by the method described in the examples below.

[0013] Ascorbic acid is a compound also known as (R)-3,4-dihydroxy-5-((S)-1,2-dihydroxyethyl)furan-2(5H)-one. Ascorbic acid may be, for example, the L-isomer, D-isomer, or DL-isomer. The L-isomer (L-ascorbic acid) is also known as vitamin C.

[0014] The salts of ascorbic acid are not particularly limited as long as they are pharmacologically or physiologically acceptable. Specific examples of such salts include, for example, salts with inorganic acids such as hydrochloric acid, hydrobromic acid, sulfuric acid, nitric acid, and phosphoric acid; salts with organic acids such as acetic acid, succinic acid, fumaric acid, maleic acid, tartaric acid, citric acid, malic acid, lactic acid, stearic acid, benzoic acid, methanesulfonic acid, ethanesulfonic acid, p-toluenesulfonic acid, α-ketoglutaric acid, gluconic acid, and caprylic acid; salts with alkali metals such as sodium and potassium; salts with aluminum; salts with zinc; salts with alkaline earth metals such as calcium and magnesium; salts with ammonium such as ammonium and tetramethylammonium; salts with organic amines such as morpholine and piperidine; and salts with amino acids such as glycine, L-phenylalanine, L-lysine, L-aspartic acid, and L-glutamic acid.

[0015] In the granular composition according to the present embodiment, the content of ascorbic acid or its salt is not limited, but may be, for example, 5% by mass or more, 10% by mass or more, 15% by mass or more, 20% by mass or more, etc., and may also be 90% by mass or less, 80% by mass or less, 60% by mass or less, 40% by mass or less, 30% by mass or less, etc., and may be 5 to 90% by mass, 10 to 80% by mass, 5 to 60% by mass, 10 to 50% by mass, etc.

[0016] The granule strength test is, for example, a test in which after placing a sieve with a mesh size of 212 μm and an inner diameter of 75 mm under a sieve with a mesh size of 710 μm and an inner diameter of 75 mm, 4 stainless steel balls with a diameter of 11.1 mm and 2 g of the above granular composition are placed on the sieve with a mesh size of 710 μm, and the test is carried out by shaking at 290 rpm for 6 minutes using a rotary tap type sieve shaker.

[0017] The granular composition according to the present embodiment only needs to be such that the mass of the powder with a particle size of 212 μm or less generated when the granule strength test is performed is 18% or more of the total mass of the granular composition before the granule strength test. This value may be, for example, 18.5% or more, 19% or more, 19.5% or more, 20% or more, 20.5% or more, 21% or more, 21.5% or more, 22% or more, 22.5% or more, 23% or more, 23.4% or more, 23.5% or more, 24% or more, 24.5% or more, 25% or more, 25.5% or more, or 25.9% or more, etc., and may also be 50% or less, 40% or less, 30% or less, 28% or less, or 26% or less, etc. Here, in this specification, "powder with a particle size of 212 μm or less" means powder with a size that passes through a sieve with a mesh size of 212 μm. Note that "powder" refers to an aggregate of a large number of minute solid particles.

[0018] The granular composition according to the present embodiment may be a granulated product. The granular composition according to the present embodiment can be produced, for example, by known granulation methods such as extrusion granulation, fluidized bed granulation, stirring granulation, rolling granulation, pneumatic granulation, compression molding granulation, crushing granulation, spray granulation, injection granulation, etc., and it is preferably produced by extrusion granulation.

[0019] When performing the granule strength test, the mass of the powder having a particle diameter of 212 μm or less with respect to the total mass of the granular composition before the granule strength test can be adjusted by appropriately changing the production method or production conditions of the granular composition. For example, by appropriately adjusting the type and concentration of the binder, the amount of water added, the mixing conditions of the composition before forming into granules, and the compression conditions, etc. in the composition before forming into granules, the mass of the powder having a particle diameter of 212 μm or less with respect to the total mass of the granular composition before the granule strength test can be adjusted. When the granular composition according to the present embodiment is produced by extrusion granulation, for example, the speed of extruding the composition before forming into granules, the amount of the composition before forming into granules (for example, powder, etc.) with respect to the extrusion surface, and the amount of the composition before forming into granules (for example, powder, etc.) fed per mesh used during extrusion granulation, etc., the above value can be appropriately adjusted.

[0020] The granular composition according to the present embodiment may further contain a sugar alcohol. A sugar alcohol is a polyhydric alcohol obtained by reducing the carbonyl group of a sugar molecule. Although not limited, examples of sugar alcohols include, for example, xylitol, sorbitol, erythritol, maltitol, lactitol, mannitol, α - glucopyranosyl - 1,1 - mannitol, α - glucopyranosyl - 1,6 - sorbitol, reduced maltose syrup, etc. From the viewpoint of significantly exhibiting the effects of the present invention, it is preferably at least one selected from the group consisting of xylitol, erythritol, and mannitol. The sugar alcohol contained in the granular composition according to the present embodiment may be one kind or two or more kinds.

[0021] The sugar alcohol content in the granular composition according to this embodiment is not limited to the total amount of the composition, but may be, for example, 3% by mass or more, 5% by mass or more, 10% by mass or more, 20% by mass or more, 30% by mass or more, 40% by mass or more, 50% by mass or more, 60% by mass or more, 70% by mass or more, etc. It may also be 80% by mass or less, 70% by mass or less, 60% by mass or less, 50% by mass or less, 40% by mass or less, etc. It may also be 3 to 80% by mass, 5 to 70% by mass, 10 to 60% by mass, 20 to 60% by mass, 30 to 60% by mass, 20 to 40% by mass, 10 to 30% by mass, etc.

[0022] The granular composition according to this embodiment may further contain starch. Starch is composed of two components: amylose, in which glucose molecules are linked in a linear chain, and amylopectin, which has side chains branched from the linear chain. Examples of starch include corn starch, wheat starch, rice starch, potato starch, tapioca starch, sweet potato starch, sago palm starch, pea starch, mung bean starch, kudzu starch, etc., and may also be modified starch made from these raw materials. The processing method for modified starch is not particularly limited, but examples of modified starch include acetylated adipic acid crosslinked starch, acetylated phosphate crosslinked starch, acetylated oxidized starch, sodium octenyl succinate starch, starch acetate, oxidized starch, hydroxypropyl starch, hydroxypropylated phosphate crosslinked starch, phosphate monoesterified phosphate crosslinked starch, phosphorylated starch, phosphate crosslinked starch, sodium starch glycolate, and sodium starch phosphate ester. The granular composition according to this embodiment may contain one type of starch or two or more types.

[0023] The starch content in the granular composition according to this embodiment is not limited to the total amount of the composition, but may be, for example, 3% by mass or more, 5% by mass or more, 10% by mass or more, 20% by mass or more, 30% by mass or more, 40% by mass or more, 50% by mass or more, 60% by mass or more, 70% by mass or more, etc., and may be 80% by mass or less, 70% by mass or less, 60% by mass or less, 50% by mass or less, 40% by mass or less, 30% by mass or less, 20% by mass or less, etc., and may also be 5 to 60% by mass, 10 to 50% by mass, 20 to 40% by mass, 30 to 50% by mass, etc.

[0024] The granular composition according to this embodiment may optionally contain a carrier, excipient, disintegrant, binder, lubricant, chelating agent, pH adjuster, thickener, stabilizer, preservative, isotonic agent, fragrance, flavoring agent, etc.

[0025] Examples of suitable carriers include aqueous solvents such as water and aqueous ethanol.

[0026] Examples of excipients include sugar alcohols such as D-sorbitol, mannitol, and xylitol; sugars such as glucose, sucrose, lactose, and fructose; crystalline cellulose; carmellose sodium; croscarmellose sodium; calcium hydrogen phosphate; dextrin; β-cyclodextrin; light anhydrous silicic acid; titanium dioxide; magnesium aluminometasilicate; calcium silicate; talc; and kaolin.

[0027] Examples of disintegrants include low-substituted hydroxypropyl cellulose, carboxymethylcellulose calcium, and croscarmellose sodium.

[0028] Examples of binders include hydroxypropyl methylcellulose, carboxymethylcellulose, hydroxypropylcellulose, gelatin, gum arabic, tragacanth, polyvinylpyrrolidone, methylcellulose, polyvinyl alcohol, sodium alginate, pullulan, and glycerin.

[0029] Examples of lubricants include stearic acid, magnesium stearate, calcium stearate, silicon dioxide, polyoxyl stearate, cetanol, talc, and dimethylpolysiloxane.

[0030] Examples of chelating agents include ethylenediaminediacetic acid (EDDA), ethylenediaminetriacetic acid, ethylenediaminetetraacetic acid (EDTA), N-(2-hydroxyethyl)ethylenediaminetriacetic acid (HEDTA), and diethylenetriaminepentaacetic acid (DTPA).

[0031] Examples of pH adjusting agents include hydrochloric acid, acetic acid, sodium hydroxide, potassium hydroxide, calcium hydroxide, magnesium hydroxide, triethanolamine, monoethanolamine, and diisopropanolamine.

[0032] Examples of thickening agents include cellulosic polymers such as methylcellulose, ethylcellulose, hydroxypropylmethylcellulose, hydroxyethylcellulose, and sodium carboxymethylcellulose; polyvinyl polymers such as polyvinylpyrrolidone and polyvinyl alcohol; carboxyvinyl polymers; guar gum; hydroxypropyl guar gum; gum arabic; karaya gum; xanthan gum; agar; alginic acid and its salts (sodium salts, etc.); mucopolysaccharides such as heparinoids, heparin, heparin sulfate, heparan sulfate, heparinoids, hyaluronic acid and its salts (sodium salts, etc.); starch; chitin and its derivatives; chitosan and its derivatives; carrageenan; and monosaccharides such as glucose.

[0033] Examples of stabilizers include EDTA, EDTA salts (disodium EDTA, calcium disodium EDTA, trisodium EDTA, tetrasodium EDTA), sodium formaldehyde sulfoxylate (Longalit), aluminum monostearate, glyceryl monostearate, cyclodextrin, monoethanolamine, dibutylhydroxytoluene, sodium bisulfite, sodium pyrosulfite, etc.

[0034] Examples of preservatives include alkyl polyaminoethylglycine quaternary ammonium salts (e.g., benzalkonium chloride, benzethonium chloride, etc.), chlorhexidine gluconate, polydronium chloride, zinc chloride, sodium benzoate, ethanol, chlorobutanol, sorbic acid, potassium sorbate, sodium dehydroacetate, methyl parahydroxybenzoate, ethyl parahydroxybenzoate, propyl parahydroxybenzoate, butyl parahydroxybenzoate, oxyquinoline sulfate, phenethyl alcohol, benzyl alcohol, biguanide compounds (specifically, polyhexanide hydrochloride (polyhexamethylene biguanide), alexidine, etc.), and Glokill (a trade name of Rhodia Corporation).

[0035] Examples of isotonic agents include potassium chloride, calcium chloride, sodium chloride, magnesium chloride, potassium acetate, sodium acetate, sodium bicarbonate, sodium carbonate, sodium thiosulfate, magnesium sulfate, glycerin, propylene glycol, sodium bisulfite, and sodium sulfite.

[0036] Examples of fragrances include lemon oil, orange oil, menthol, peppermint oil, borneol, and vanilla flavor.

[0037] Examples of flavoring agents include aspartame, ascorbic acid, stevia, menthol, licorice extract, and simple syrup.

[0038] The granular composition according to this embodiment is preferably administered orally or ingested, for example, 1 to 3 times a day.

[0039] The dosage or intake of the granular composition according to this embodiment is not particularly limited, but for example, for a subject weighing 60 kg, the daily dosage or intake of ascorbic acid or its salt may be 100-3000 mg, 200-2500 mg, or 500-2000 mg.

[0040] The granular composition according to this embodiment can be applied to humans and other mammals, but humans are preferred. Examples of other mammals include mice, rats, guinea pigs, hamsters, rabbits, cats, dogs, sheep, pigs, cows, horses, goats, and monkeys.

[0041] The granular composition according to this embodiment may be contained in a container. Examples of the container's shape include pouches, bottles, sachets, and jars. Examples of materials used to form the container include metal (aluminum, etc.), polyolefins (polypropylene, polyethylene (HDPE, LDPE, and LLDPE, etc.), ABS resin, ethylene vinyl alcohol resin, polystyrene, polyester (polyethylene terephthalate, etc.), and glass. Although not limited, it is preferable that the container containing the granular composition according to this embodiment is a container (hereinafter referred to as a pouch) in which part or all of the portion in contact with the granular composition is made of polyolefin or polyester.

[0042] The granular composition according to this embodiment can be contained in a container containing a polyolefin-containing resin. The container preferably has a polyolefin-containing layer on the surface in contact with the composition. Here, the polyolefin is preferably polyethylene (PE) (including high-density polyethylene (HDPE), low-density polyethylene (LDPE), ultra-low-density polyethylene, linear low-density polyethylene (LLDPE), ultra-high molecular weight polyethylene, etc.), polypropylene (PP) (including homopolymers, random copolymers, block copolymers, etc.), and ethylene-propylene copolymer, cyclic olefin copolymer, polymethylpentene, and polybutene-1,1,2-polybutadiene, with polyethylene resin or polypropylene resin being more preferred. Of these, it is particularly preferable that the resin contains at least polyethylene. The polyolefin-containing layer may consist solely of polyolefin, but it is sufficient that it contains polyolefin, and the proportion is not limited. It may also contain aluminum. For example, packaging materials having a layer with an aluminum content of 3% or more by mass, or 5% or more by mass, can be used. The aluminum layer is preferably 1 μm or more, 3 μm or more, or 5 μm or more, and preferably 20 μm or less, 15 μm or less, or 10 μm or less. Here, the packaging material may be multilayered or single-layered, and the form is not limited as long as it contains polyolefin. It may also contain polyester. Of the layers, the layer containing polyolefin or the layer made of polyolefin that is in contact with the composition is preferably 5 μm or more, 10 μm or more, 20 μm or more, 30 μm or more, or 40 μm or more, and preferably 100 μm or less, 80 μm or less, 60 μm or less, 50 μm or less, or 40 μm or less.

[0043] The granular composition according to this embodiment can be contained in a container containing a polyester-containing resin. The container preferably has a polyester-containing layer on the surface in contact with the composition. Here, the polyester is preferably polyethylene terephthalate (PET), polybutylene terephthalate (PBT), polyethylene naphthalate (PEN), polybutylene naphthalate (PBN), polyethylene isophthalate (PEIT), or polycaprolactone (PCL), and more preferably a resin containing at least polyethylene terephthalate. It may also contain aluminum. For example, packaging materials having layers with an aluminum content of 3% by mass or 5% by mass or more can be used. The aluminum layer is preferably 1 μm or more, 3 μm or more, or 5 μm or more, and preferably 20 μm or less, 15 μm or less, or 10 μm or less. Here, the packaging material may be multilayer or single-layer, and the form is not limited as long as polyester is contained. It may also contain polyolefin.

[0044] One embodiment of the granular composition is a granular composition containing ascorbic acid or a salt thereof, wherein the mass of powder with a particle size of 212 μm or less generated when a granular strength test is performed on the granular composition is 18% or more of the total mass of the granular composition before the granular strength test, and the granular strength test is performed by placing a sieve with an inner diameter of 75 mm and a mesh opening of 212 μm below a sieve with an inner diameter of 75 mm and a mesh opening of 710 μm, then placing four stainless steel balls with a diameter of 11.1 mm and 2 g of the granular composition on the sieve with a mesh opening of 710 μm, and shaking at 290 rpm for 6 minutes, and the granular composition exhibits reduced adhesion compared to a granular composition in which the mass of powder with a particle size of 212 μm or less generated when the same test is performed on the granular strength test is less than 18% of the total mass of the granular composition before the granular strength test. The above-mentioned adhesion may be adhesion to the container described above, and the container may be formed of polyolefin or polyester in part or all of the portion that comes into contact with the granular composition.

[0045] Furthermore, a granular composition according to one embodiment is a granular composition containing ascorbic acid or a salt thereof, wherein the mass of powder with a particle diameter of 212 μm or less generated when a granular strength test is performed on the granular composition is 18% or more of the total mass of the granular composition before the granular strength test, and the granular strength test is performed by placing a sieve with an inner diameter of 75 mm and a mesh opening of 212 μm below a sieve with an inner diameter of 75 mm and a mesh opening of 710 μm, then placing four stainless steel balls with a diameter of 11.1 mm and 2 g of the granular composition on the sieve with a mesh opening of 710 μm, and shaking at 290 rpm for 6 minutes, and the granular composition exhibits reduced moisture absorption compared to a granular composition in which the mass of powder with a particle diameter of 212 μm or less generated when the same test is performed as described above is less than 18% of the total mass of the granular composition before the granular strength test.

[0046] One embodiment of the present invention provides a method for producing a granular composition containing ascorbic acid or a salt thereof, wherein the mass of powder with a particle size of 212 μm or less, generated when a granular strength test is performed on the granular composition, is adjusted to be 18% or more of the total mass of the granular composition before the granular strength test, and the granular strength test is a test in which a sieve with an inner diameter of 75 mm and a mesh opening of 710 μm is placed below a sieve with an inner diameter of 75 mm and a mesh opening of 212 μm, then four stainless steel balls with a diameter of 11.1 mm and 2 g of the granular composition are placed on the sieve with a mesh opening of 710 μm, and the mixture is shaken at 290 rpm for 6 minutes.

[0047] The method for producing the granular composition according to this embodiment may further include placing the granular composition in a container in which part or all of the portion in contact with the granular composition is made of polyolefin or polyester.

[0048] The components used in the method for producing the above-mentioned granular composition, their content, the method for adjusting the mass of powder with a particle size of 212 μm or less relative to the total mass of the granular composition before the granular strength test, and other conditions are as described above.

[0049] One embodiment of the present invention provides a method for suppressing moisture absorption and adhesion to a container in a granular composition containing ascorbic acid or a salt thereof, comprising adjusting the mass of powder with a particle size of 212 μm or less generated when a granular strength test is performed on the granular composition to 18% or more of the total mass of the granular composition before the granular strength test, wherein the granular strength test is performed by placing a sieve with an inner diameter of 75 mm and a mesh opening of 710 μm below a sieve with an inner diameter of 75 mm and a mesh opening of 212 μm, then placing four stainless steel balls with a diameter of 11.1 mm and 2 g of the granular composition on the sieve with a mesh opening of 710 μm, and shaking at 290 rpm for 6 minutes. The container may be as described above, and part or all of the part in contact with the granular composition may be made of polyolefin or polyester.

[0050] The method according to this embodiment may further include housing the granular composition in a container in which part or all of the portion in contact with the granular composition is made of polyolefin or polyester.

[0051] The components used in the above method, their content, the method for adjusting the mass of powders with a particle diameter of 212 μm or less relative to the total mass of the granular composition before the granular strength test, and other conditions are as described above. [Examples]

[0052] The present invention will be described more specifically below based on examples. However, the present invention is not limited to the following examples.

[0053] (Preparation example: Preparation of a granular composition containing ascorbic acid) Granular compositions for Preparation Examples 1 to 31 were prepared by extrusion granulation using the compositions shown in Tables 1 to 4 below, with varying granulation conditions (amount of powder relative to the extrusion surface and the extrusion speed). Subsequently, these granular compositions were subjected to granular strength tests as described below, and the mass of powder with a particle diameter of 212 μm or less was 18% or more of the total mass of the granular composition before the granular strength test. Hereafter, the ratio of the mass of powder with a particle diameter of 212 μm or less after the granular strength test to the total mass of the granular composition before the granular strength test will also be referred to as "212 μm under". For example, in a granular composition where the mass of powder with a particle diameter of 212 μm or less generated during the granular strength test is 18% of the total mass of the granular composition before the granular strength test, "212 μm under" is 18%.

[0054] The above granule strength test was performed by placing a sieve with an inner diameter of 75 mm and a mesh size of 710 μm below a sieve with an inner diameter of 75 mm and a mesh size of 212 μm. Then, four stainless steel balls with a diameter of 11.1 mm and 2 g of the granular composition were placed on top of the sieve with a mesh size of 710 μm, and the mixture was shaken for 6 minutes at 290 rpm using a rotary tap type sieve shaker (Iida Seisakusho, ES-65 model).

[0055] [Table 1]

[0056] [Table 2]

[0057] [Table 3]

[0058] [Table 4]

[0059] (Test Example 1: Evaluation of hygroscopic properties of granular composition) <Preparation of granular composition> Four types of granular compositions (extruded granules) were prepared by extrusion granulation using the compositions shown in Table 5 below, with varying granulation conditions (amount of powder relative to the extrusion surface and the extrusion speed). Subsequently, these granular compositions were subjected to granular strength tests similar to those used in the preparation examples. The mass of powder with a particle size of 212 μm or less was 25.9%, 23.4%, 15.6%, and 13.4% of the total mass of the granular composition before the granular strength test, respectively.

[0060] [Table 5]

[0061] <Moisture absorption test> Each of the prepared granular compositions was placed in a Petri dish, and its mass was measured immediately after the start of the experiment and one hour after the start of the experiment under conditions of 25°C and 75% RH. These measurement results were applied to the following formula (1) to calculate the moisture absorption rate (%) of each granular composition. The calculated results are shown in Table 6 below. Equation (1): Moisture absorption rate (%) = {(BA) / A} × 100 However, A to B are as follows: A: Mass (g) of the granular composition immediately after the start of the experiment. B: Mass (g) of the granular composition after 1 hour

[0062] [Table 6]

[0063] As shown in Table 6, granular compositions with a 212 μm under of 18% or more had lower moisture absorption rates and suppressed moisture absorption compared to granular compositions with a 212 μm under of less than 18%. Furthermore, the greater the 212 μm under value was compared to a predetermined value (13.4%), i.e., the weaker the granular strength was compared to a predetermined value (13.4%), the lower the moisture absorption rate of the granular composition and the more suppressed moisture absorption of the granular composition.

[0064] (Test Example 2: Evaluation of the adhesion of granular composition to aluminum pouches) <Adhesion Test> On a board covered with an aluminum pouch:AL-G (PET12 / Special Polyethylene (SPE)15 / Aluminum (AL)7 / SPE15 / PE40 from the inside out: manufactured by Nippon Seisan Co., Ltd.), 1 g of the granular composition (sample) prepared in Test Example 1 was placed, and a beaker containing 300 mL of water was placed on top as a weight for 1 second. The numbers in parentheses above represent the thickness (μm) of each layer. The board was tilted to a 30-degree angle, and the sample was slid down to a distance of 10 cm. After that, the amount of sample remaining due to adhesion was measured, and the retention rate (%) (the percentage of sample remaining attached to the board) of each granular composition was calculated by applying it to the following formula (2). The calculated results are shown in Table 7 below. Equation (2): Survival rate = Mass of sample remaining after tilting (g) ÷ Mass of sample initially placed on the plate (g)

[0065] [Table 7]

[0066] As shown in Table 7, granular compositions with 212 μm under content of 18% or more had lower retention rates and less adhesion of the granular composition to the aluminum pouch compared to granular compositions with less than 18% of 212 μm under content. Furthermore, the greater the 212 μm under content value was above the predetermined value (13.4% or 15.6%), i.e., the weaker the granular strength was compared to the predetermined value (13.4% or 15.6%), the higher the retention rate of the granular composition and the less adhesion of the granular composition to the aluminum pouch.

[0067] (Test Example 3: Evaluation of user experience when taking granular composition from an aluminum pouch container) Four types of granular compositions (extruded granules) were prepared by extrusion granulation using the compositions shown in Table 8 below, with varying granulation conditions (amount of powder relative to the extrusion surface and the extrusion speed). Subsequently, these granular compositions were subjected to granular strength tests similar to those used in the preparation examples. The mass of powder with a particle size of 212 μm or less was 21.2%, 18.3%, 16.8%, or 12.1% of the total mass of the granular composition before the granular strength test, respectively.

[0068] [Table 8]

[0069] Samples of these four granular compositions were each filled into 2cm x 10cm aluminum pouch containers used in Test Example 2. Five trained monitors were given a questionnaire regarding the "ease of administration" from each aluminum pouch container. The evaluation item for "ease of administration" was "the number of times the aluminum pouch was tapped to take all of the contents," and this was evaluated using a three-point scoring system as described below.

[0070] (Method for evaluating the number of times the aluminum pouch was tapped to take all the contents) With the opening of each aluminum pouch container fully opened, and tilted at an angle of approximately 30 degrees from the horizontal towards the mouth of the monitor, the number of taps required to dispense approximately the entire contents (to the point where no granules remaining on the inner surface of the pouch were visible), excluding any granules stuck in the folds of the container, was measured (rounded to the nearest whole number). The tapping force was light, simulating typical use, so as not to move the container too much or deform the aluminum pouch. 3 points: Number of taps: 1 2 points: Number of taps: 2 1 point: Number of taps: 3

[0071] As a result, the samples with 21.2% and 18.3% of the particles under 212 μm received the highest evaluation scores of 2.5 and 2.3 points, respectively. The sample with 16.8% of the same value received a score of 1.8 points, and the sample with 12.1% received a score of 1.2 points. As shown in the above test examples, it is presumed that the effect of the present invention is not based on a specific combination of components, but rather on the technical significance of having a value of 18% or more of the particles under 212 μm, which is a value relating to the mass of powder particles with a diameter of 212 μm or less, when a granular composition containing ascorbic acid or a salt thereof is subjected to a specific granular strength test.

Claims

1. A granular composition containing ascorbic acid or a salt thereof, When a granular strength test is performed on the granular composition, the mass of powder particles with a diameter of 212 μm or less is 18% or more of the total mass of the granular composition before the granular strength test. The granular strength test is performed by placing a sieve with an inner diameter of 75 mm and a mesh size of 710 μm below a sieve with an inner diameter of 75 mm and a mesh size of 212 μm, then placing four stainless steel balls with a diameter of 11.1 mm and 2 g of the granular composition on top of the sieve with a mesh size of 710 μm, and shaking at 290 rpm for 6 minutes.

2. The granular composition according to claim 1, which is a granulated product.

3. The granular composition according to claim 2, wherein the granules are extruded granules.

4. A granular composition according to any one of claims 1 to 3, containing 10% by mass or more of the ascorbic acid or a salt thereof.

5. A granular composition according to any one of claims 1 to 3, further containing a sugar alcohol.

6. A granular composition according to any one of claims 1 to 3, further containing starch.

7. The granular composition according to claim 6, comprising 10 to 80% by mass of ascorbic acid or a salt thereof, 5 to 70% by mass of a sugar alcohol, and 10 to 50% by mass of starch.

Citation Information

Patent Citations

  • Composition for internal use

    JP2023095834A