JP2020000074A - Oral composition - Google Patents
Oral composition Download PDFInfo
- Publication number
- JP2020000074A JP2020000074A JP2018122201A JP2018122201A JP2020000074A JP 2020000074 A JP2020000074 A JP 2020000074A JP 2018122201 A JP2018122201 A JP 2018122201A JP 2018122201 A JP2018122201 A JP 2018122201A JP 2020000074 A JP2020000074 A JP 2020000074A
- Authority
- JP
- Japan
- Prior art keywords
- mass
- component
- oral composition
- unpleasant taste
- solution
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000000203 mixture Substances 0.000 title claims abstract description 44
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Abstract
Description
本発明は、経口組成物に関する。 The present invention relates to oral compositions.
デキストリンは、でんぷん分解物の一種であり、通常でんぷんを原料として酸処理や加熱処理を行い、部分的に加水分解することにより製造される。デキストリンの特性は加水分解の程度により大きく異なり、食品分野においては、例えば、食物繊維源、賦形剤、結合剤、滑沢剤、マスキング剤等として利用され（特許文献１）、顆粒剤や錠剤では吸湿性や分散性、賦形性等製造物性の面で優れているが、デキストリンはざらつく口内感の悪さ、粉臭、不快な苦味や甘味があり、その呈味を改善することが望まれている（特許文献２、３）。 Dextrin is a type of starch degradation product, and is usually produced by subjecting starch to a raw material and subjecting it to an acid treatment or a heat treatment and partially hydrolyzing it. The properties of dextrin vary greatly depending on the degree of hydrolysis. In the food field, for example, it is used as a dietary fiber source, an excipient, a binder, a lubricant, a masking agent, etc. (Patent Document 1), and granules and tablets Is excellent in terms of product properties such as hygroscopicity, dispersibility and shapeability, but dextrin has a rough mouthfeel, powdery odor, unpleasant bitterness and sweetness, and it is desired to improve its taste. (Patent Documents 2 and 3).
一方、カフェインは、脂質エネルギー代謝や運動機能の向上等の生理活性物質であり（特許文献３、４）、コーヒー、緑茶、紅茶、烏龍茶、コーラ、チョコレート等に含まれる苦味物質として知られている。そしてカフェインをより摂取しやすくするため、マスキング剤としてデキストリンが使用されている（特許文献５）。
また、アストラガリンは、柿の葉や桑の葉に含まれるケンフェロールモノグリコシドの一種であり、抗アレルギー作用を有することが報告されている。このようなアストラガリンの生理作用に着目し、飲食品への応用が検討されており、例えば、アストラガリンに、果糖、ガラクトース、乳糖及びブドウ糖からなる群から選ばれる糖の１種又は２種以上を配合することで、アストラガリンの吸収性が向上するとの報告がある（特許文献６）。
On the other hand, caffeine is a physiologically active substance for improving lipid energy metabolism and motor function (Patent Documents 3 and 4), and is known as a bitter substance contained in coffee, green tea, black tea, oolong tea, cola, chocolate and the like. I have. Dextrin is used as a masking agent to make caffeine more ingestible (Patent Document 5).
Astragalin is a kind of kaempferol monoglycoside contained in persimmon leaves and mulberry leaves, and has been reported to have an antiallergic effect. Focusing on the physiological action of such astragalin, application to foods and drinks is being studied. For example, astragalin, one or more sugars selected from the group consisting of fructose, galactose, lactose and glucose There is a report that the absorption of astragalin is improved by blending (Patent Document 6).
デキストリンは、粉臭、不快な苦味や甘味といった独特の不快味を有するため、飲食品の味を損なう原因となっている。本発明者らは、デキストリンにカフェインを一定の比率添加したところ、デキストリンが少量であるとカフェインのマスキング剤として機能する一方、デキストリンが多量であるとデキストリンの不快味とカフェインの苦味とが相俟って、それら有する甘味や苦味とは異なる独特の甘味や苦味が醸成され、それが不快味として強調されることが判明した。
本発明の課題は、デキストリン及びカフェインを一定比率含有しながらも、不快味の抑制された経口組成物を提供することにある。
Dextrin has a peculiar unpleasant taste such as powdery smell, unpleasant bitterness and sweetness, and is a cause of impairing the taste of food and drink. The present inventors have added caffeine to dextrin at a certain ratio.When dextrin is in a small amount, it functions as a caffeine masking agent, whereas when dextrin is in a large amount, dextrin has an unpleasant taste and caffeine bitterness. In combination, unique sweetness and bitterness different from those sweetness and bitterness are brewed, and it is found that they are emphasized as unpleasant taste.
An object of the present invention is to provide an oral composition which contains dextrin and caffeine at a certain ratio and has a suppressed unpleasant taste.
本発明者らは、上記課題に鑑み、鋭意研究を重ねた結果、特定量のデキストリンとカフェインとを特定の量比で含有させたうえで、更に特定量のケンフェロールモノグルコシドを含有させることで、意外なことに、デキストリン及びカフェインを含有しながらも、不快味の抑制された経口組成物が得られることを見出した。 The present inventors, in view of the above problems, as a result of intensive studies, after containing a specific amount of dextrin and caffeine in a specific amount ratio, further containing a specific amount of kaempferol monoglucoside. Surprisingly, they have found that an oral composition containing dextrin and caffeine and having a suppressed unpleasant taste can be obtained.
すなわち、本発明は、次の成分（Ａ）、（Ｂ）及び（Ｃ）；
（Ａ）デキストリン
（Ｂ）カフェイン、及び
（Ｃ）ケンフェロールモノグルコシド
を含有し、
固形分中の成分（Ａ）の含有量が１０質量％以上であり、
固形分中の成分（Ｃ）の含有量が０．０１〜１．０質量％であり、かつ、
成分（Ａ）と成分（Ｂ）との質量比[（Ｂ）／（Ａ）]が０．００１〜０．２である、
経口組成物を提供するものである。
That is, the present invention provides the following components (A), (B) and (C);
(A) containing dextrin (B) caffeine, and (C) kaempferol monoglucoside,
The content of the component (A) in the solid content is 10% by mass or more;
The content of the component (C) in the solid content is 0.01 to 1.0% by mass, and
The mass ratio [(B) / (A)] between the component (A) and the component (B) is from 0.001 to 0.2.
An oral composition is provided.
本発明によれば、デキストリン及びカフェインを含有しながらも、不快味の抑制された経口組成物を提供することができる。 According to the present invention, it is possible to provide an oral composition containing dextrin and caffeine while suppressing unpleasant taste.
本明細書において「経口組成物」とは、経口摂取に供される製品をいう。経口組成物の製品形態としては、常温（２０℃±１５℃）において固形でも、液状でもよく、特に限定されない。液状の場合、濃縮液状、ゲル状、ゼリー状、スラリー状のいずれの形態であっても構わない。濃縮液状である場合、その固形分濃度はＲＴＤ（レディ・トゥ・ドリンク）よりも高濃度であれば適宜選択可能であり、特に限定されない。固形としては、例えば、粉末状、顆粒状、錠状、棒状、板状、ブロック状等を挙げることができる。経口組成物が固形である場合、経口組成物中の固形分量は通常８０質量％以上、好ましくは９０質量％以上、より好ましくは９３質量％以上、更に好ましくは９５質量％以上、殊更に好ましくは９７質量％以上である。なお、かかる固形分量の上限は特に限定されず、１００質量％であってもよい。ここで、本明細書において「固形分量」とは、試料を１０５℃の電気恒温乾燥機で３時間乾燥して揮発物質を除いた残分の質量をいう。中でも、経口組成物の製品形態としては、固形、濃縮液状、ゼリー状が好ましく、固形、濃縮液状がより好ましく、固形が更に好ましい。固形の中では、錠状、顆粒状が好ましく、顆粒状が更に好ましい。 As used herein, the term "oral composition" refers to a product that is to be taken orally. The product form of the oral composition may be solid or liquid at room temperature (20 ° C. ± 15 ° C.), and is not particularly limited. In the case of a liquid, any of a concentrated liquid, a gel, a jelly, and a slurry may be used. In the case of a concentrated liquid, the solid content concentration can be appropriately selected as long as it is higher than RTD (ready to drink), and is not particularly limited. Examples of the solid include powder, granules, tablets, rods, plates, blocks, and the like. When the oral composition is solid, the solid content in the oral composition is usually 80% by mass or more, preferably 90% by mass or more, more preferably 93% by mass or more, still more preferably 95% by mass or more, particularly preferably. 97% by mass or more. The upper limit of the solid content is not particularly limited, and may be 100% by mass. Here, in the present specification, the “solid content” refers to a mass of a residue obtained by drying a sample with an electric constant temperature drier at 105 ° C. for 3 hours to remove volatile substances. Among them, the product form of the oral composition is preferably solid, concentrated liquid, or jelly, more preferably solid or concentrated liquid, and further preferably solid. Among solids, tablets and granules are preferred, and granules are more preferred.
本発明の経口組成物は、成分（Ａ）としてデキストリンを含有する。ここで、本明細書において「デキストリン」とは、でんぷん分解物の一種であり、でんぷんを酸処理又は加熱処理して部分的に加水分解し低分子化した化合物である。デキストリンは、糖がグリコシド結合によって重合した分子構造を有しており、グリコシド結合は、鎖状に結合していても、環状に結合していても、これらの混合物であっても構わない。糖の結合方式としては、α−１，４結合、α−１，６結合、β−１，２結合、β−１，３結合、β−１，４結合、β−１，６結合等が挙げられ、単一の結合方式のみでも、２種以上の結合方式でも構わない。 The oral composition of the present invention contains dextrin as component (A). Here, in the present specification, “dextrin” is a kind of starch degradation product, and is a compound obtained by partially hydrolyzing starch by acid treatment or heat treatment to reduce the molecular weight. Dextrin has a molecular structure in which a sugar is polymerized by glycosidic bonds, and the glycosidic bonds may be linked in a chain form, may be linked in a cyclic manner, or may be a mixture thereof. Examples of the sugar binding method include α-1,4 bond, α-1,6 bond, β-1,2 bond, β-1,3 bond, β-1,4 bond, β-1,6 bond and the like. For example, only a single coupling method or two or more coupling methods may be used.
また、成分（Ａ）は、本発明の効果を享受しやすい点から、デキストロース当量（ＤＥ値）が、１以上が好ましく、２以上がより好ましく、３以上が更に好ましく、そして５０以下が好ましく、４０以下がより好ましく、３０以下が更に好ましく、２５以下が更に好ましく、２０以下がより更に好ましく、１６以下が殊更に好ましい。かかるＤＥ値の範囲としては、好ましくは１〜４０であり、より好ましくは２〜４０であり、更に好ましくは３〜３０であり、更に好ましくは３〜２５であり、より更に好ましくは３〜２０であり、殊更に好ましくは３〜１６ある。なお、デキストロース当量（ＤＥ値）は、通常知られているデキストロースの測定法のうち測定試料の状況に適した分析法により測定することができる。具体的には、後掲の実施例に記載の方法により測定することができる。 In addition, the component (A) has a dextrose equivalent (DE value) of preferably 1 or more, more preferably 2 or more, still more preferably 3 or more, and preferably 50 or less, from the viewpoint that the effects of the present invention are easily enjoyed. It is more preferably 40 or less, more preferably 30 or less, still more preferably 25 or less, even more preferably 20 or less, and particularly preferably 16 or less. The range of the DE value is preferably from 1 to 40, more preferably from 2 to 40, further preferably from 3 to 30, further preferably from 3 to 25, and still more preferably from 3 to 20. And particularly preferably 3 to 16. The dextrose equivalent (DE value) can be measured by an analytical method suitable for the condition of the sample to be measured among the generally known methods for measuring dextrose. Specifically, it can be measured by the method described in Examples described later.
本発明の経口組成物は、固形分中の成分（Ａ）の含有量が１０質量％以上であるが、製造物性の観点から、１５質量％以上が好ましく、２０質量％以上がより好ましく、２５質量％以上が更に好ましく、３０質量％以上が殊更に好ましく、またデキストリン由来の不快味低減の観点から、９０質量％以下が好ましく、８５質量％以下がより好ましく、８０質量％以下が更に好ましく、７５質量％以下がより更に好ましく、７０質量％以下が殊更に好ましい。成分（Ａ）の含有量の範囲としては、経口組成物の固形分中に、好ましくは１０〜９０質量％、より好ましくは１５〜８５質量％、更に好ましくは２０〜８０質量％、より更に好ましくは２５〜７５質量％、殊更に好ましくは３０〜７０質量％である。なお、成分（Ａ）の含有量は、通常知られている測定法のうち測定試料の状況に適した分析法により測定することが可能であり、例えば、液体クロマトグラフで分析することが可能である。具体的には、後掲の実施例に記載の方法が挙げられる。なお、測定の際には装置の検出域に適合させるため、試料を凍結乾燥したり、装置の分離能に適合させるため試料中の夾雑物を除去したりする等、必要に応じて適宜処理を施してもよい。 In the oral composition of the present invention, the content of the component (A) in the solid content is 10% by mass or more, but from the viewpoint of production properties, it is preferably 15% by mass or more, more preferably 20% by mass or more, and 25% by mass or more. And more preferably at least 90% by mass, more preferably at most 90% by mass, even more preferably at most 80% by mass, from the viewpoint of reducing unpleasant taste derived from dextrin. It is more preferably at most 75% by mass, particularly preferably at most 70% by mass. The range of the content of the component (A) is preferably 10 to 90% by mass, more preferably 15 to 85% by mass, still more preferably 20 to 80% by mass, and still more preferably, in the solid content of the oral composition. Is 25 to 75% by mass, particularly preferably 30 to 70% by mass. In addition, the content of the component (A) can be measured by an analytical method suitable for the situation of a measurement sample among commonly known measuring methods, and for example, it can be analyzed by a liquid chromatograph. is there. Specifically, the method described in Examples described later can be used. In addition, at the time of measurement, the sample may be freeze-dried in order to conform to the detection range of the device, or contaminants in the sample may be removed in order to adapt to the resolution of the device. May be applied.
本発明の経口組成物は、成分（Ｂ）としてカフェインを含有する。成分（Ｂ）は、原料に由来するものでも、新たに加えられたものでもよい。また、成分（Ｂ）は、飲食品の分野において通常使用されているものであれば由来は特に限定されず、例えば、化学合成品でも、天然由来品でもよい。 The oral composition of the present invention contains caffeine as the component (B). Component (B) may be derived from a raw material or newly added. The origin of the component (B) is not particularly limited as long as it is commonly used in the field of foods and drinks, and may be, for example, a chemically synthesized product or a naturally derived product.
本発明の経口組成物は、固形分中の成分（Ｂ）の含有量は、生理効果の観点から、０．１質量％以上が好ましく、０．３質量％以上がより好ましく、０．５質量％以上が更に好ましく、０．８質量％以上が殊更に好ましく、またカフェイン由来の苦味抑制の観点から、５質量％以下が好ましく、４質量％以下がより好ましく、３質量％以下が更に好ましく、２．５質量％以下が殊更に好ましい。成分（Ｂ）の含有量の範囲としては、経口組成物の固形分中に、好ましくは０．１〜５質量％、より好ましくは０．３〜４質量％、更に好ましくは０．５〜３質量％、殊更に好ましくは０．８〜２．５質量％である。なお、成分（Ｂ）の含有量は、通常知られている測定法のうち測定試料の状況に適した分析法により測定することが可能であり、例えば、液体クロマトグラフィで分析することが可能である。具体的には、後掲の実施例に記載の方法が挙げられる。なお、測定の際には装置の検出域に適合させるため、試料を凍結乾燥したり、装置の分離能に適合させるため試料中の夾雑物を除去したりする等、必要に応じて適宜処理を施してもよい。 In the oral composition of the present invention, the content of the component (B) in the solid content is preferably 0.1% by mass or more, more preferably 0.3% by mass or more, and 0.5% by mass from the viewpoint of physiological effects. % Or more, more preferably 0.8% by mass or more, and particularly preferably 5% by mass or less, more preferably 4% by mass or less, still more preferably 3% by mass or less, from the viewpoint of suppressing bitterness derived from caffeine. , 2.5% by mass or less is particularly preferred. The range of the content of the component (B) is preferably 0.1 to 5% by mass, more preferably 0.3 to 4% by mass, and still more preferably 0.5 to 3% by mass in the solid content of the oral composition. %, Particularly preferably 0.8 to 2.5% by weight. In addition, the content of the component (B) can be measured by an analysis method suitable for the situation of a measurement sample among commonly known measurement methods, and can be analyzed by, for example, liquid chromatography. . Specifically, the method described in Examples described later can be used. In addition, at the time of measurement, the sample may be freeze-dried in order to conform to the detection range of the device, or contaminants in the sample may be removed in order to adapt to the resolution of the device. May be applied.
本発明の経口組成物は、成分（Ｃ）としてケンフェロールモノグルコシドを含有する。ここで、本明細書において「ケンフェロールモノグルコシド」とは、ケンフェロールの水酸基にグルコースが１つ結合した化合物をいい、グルコースの結合位置は特に限定されない。成分（Ｃ）としては、例えば、アストラガリン、ポプルニン等を挙げることができる。中でも、本発明の効果を享受しやすい点から、アストラガリンが好ましい。成分（Ｃ）は、原料に由来するものでも、新たに加えられたものでもよい。 The oral composition of the present invention contains kaempferol monoglucoside as component (C). Here, in the present specification, “kaempferol monoglucoside” refers to a compound in which one glucose is bound to a hydroxyl group of kaempferol, and the binding position of glucose is not particularly limited. As the component (C), for example, astragalin, poprunin and the like can be mentioned. Above all, astragalin is preferable because the effect of the present invention is easily enjoyed. Component (C) may be derived from a raw material or newly added.
本発明の経口組成物は、固形分中の成分（Ｃ）の含有量が０．０１〜１質量％であるが、不快味抑制の観点から、０．０２質量％以上が好ましく、０．０３質量％以上がより好ましく、０．０４質量％以上が更に好ましく、０．０６質量％以上がより更に好ましく、０．０８質量％以上が殊更に好ましく、またアストラガリン由来の渋味抑制の観点から、０．７質量％以下が好ましく、０．５質量％以下がより好ましく、０．３質量％以下が更に好ましく、０．２質量％以下が殊更に好ましい。成分（Ｃ）の含有量の範囲としては、経口組成物の固形分中に、好ましくは０．０２〜０．７質量％、より好ましくは０．０３〜０．５質量％、更に好ましくは０．０３〜０．３質量％、更に好ましくは０．０４〜０．３質量％、より更に好ましくは０．０６〜０．２質量％、殊更に好ましくは０．０８〜０．２質量％である。なお、成分（Ｃ）の含有量は、通常知られている測定法のうち測定試料の状況に適した分析法により測定することが可能であり、例えば、液体クロマトグラフで分析することが可能である。具体的には、後掲の実施例に記載の方法が挙げられる。なお、測定の際には装置の検出域に適合させるため、試料を凍結乾燥したり、装置の分離能に適合させるため試料中の夾雑物を除去したりする等、必要に応じて適宜処理を施してもよい。 In the oral composition of the present invention, the content of the component (C) in the solid content is 0.01 to 1% by mass, and from the viewpoint of suppressing unpleasant taste, 0.02% by mass or more is preferable, and 0.03% by mass or less. % By mass or more, more preferably 0.04% by mass or more, still more preferably 0.06% by mass or more, particularly preferably 0.08% by mass or more, and from the viewpoint of suppressing astringency derived from astragalin. , 0.7% by mass or less, more preferably 0.5% by mass or less, still more preferably 0.3% by mass or less, particularly preferably 0.2% by mass or less. The range of the content of the component (C) is preferably 0.02 to 0.7% by mass, more preferably 0.03 to 0.5% by mass, and still more preferably 0% by mass in the solid content of the oral composition. 0.03 to 0.3% by mass, more preferably 0.04 to 0.3% by mass, still more preferably 0.06 to 0.2% by mass, particularly preferably 0.08 to 0.2% by mass. is there. In addition, the content of the component (C) can be measured by an analytical method suitable for the situation of a measurement sample among commonly known measurement methods, and for example, it can be analyzed by a liquid chromatograph. is there. Specifically, the method described in Examples described later can be used. In addition, at the time of measurement, the sample may be freeze-dried in order to conform to the detection range of the device, or contaminants in the sample may be removed in order to adapt to the resolution of the device. May be applied.
本発明の経口組成物は、成分（Ａ）と成分（Ｂ）との質量比[（Ｂ）／（Ａ）]が０．００１〜０．２であるが、不快味抑制の観点から、０．００３以上が好ましく、０．００５以上がより好ましく、０．０１以上が更に好ましく、０．０１５以上が殊更に好ましく、またカフェイン由来の苦味抑制の観点から、０．１５以下が好ましく、０．１以下がより好ましく、０．０７以下が更に好ましく、０．０４以下が殊更に好ましい。かかる質量比[（Ｂ）／（Ａ）]の範囲としては、好ましくは０．００３〜０．１５、より好ましくは０．００５〜０．１、更に好ましくは０．０１〜０．０７、殊更に好ましくは０．０１５〜０．０４である。 The oral composition of the present invention has a mass ratio [(B) / (A)] of the component (A) to the component (B) of 0.001 to 0.2. 0.003 or more, more preferably 0.005 or more, still more preferably 0.01 or more, particularly preferably 0.015 or more, and from the viewpoint of suppressing bitterness derived from caffeine, 0.15 or less, preferably 0. .1 or less, more preferably 0.07 or less, even more preferably 0.04 or less. The range of the mass ratio [(B) / (A)] is preferably from 0.003 to 0.15, more preferably from 0.005 to 0.1, still more preferably from 0.01 to 0.07, and particularly preferably from 0.01 to 0.07. Is preferably 0.015 to 0.04.
また、本発明の経口組成物は、成分（Ｂ）と成分（Ｃ）との質量比[（Ｃ）／（Ｂ）]が、不快味抑制の観点から、０．００４以上が好ましく、０．００８以上がより好ましく、０．０１以上が更に好ましく、０．０２以上がより更に好ましく、０．０３以上がより更に好ましく、０．０５以上がより更に好ましく、０．０７以上が殊更に好ましく、またアストラガリン由来の苦味抑制の観点から、０．５以下が好ましく、０．４以下がより好ましく、０．３以下が更に好ましく、０．２以下がより更に好ましく、０．１５以下が殊更に好ましい。かかる質量比[（Ｃ）／（Ｂ）]の範囲としては、好ましくは０．００４〜０．５、より好ましくは０．００８〜０．４、更に好ましくは０．０１〜０．３、より更に好ましくは０．０２〜０．３、より更に好ましくは０．０３〜０．２、より更に好ましくは０．０５〜０．２、殊更に好ましくは０．０７〜０．１５である。 In the oral composition of the present invention, the mass ratio of the component (B) to the component (C) [(C) / (B)] is preferably 0.004 or more from the viewpoint of suppressing unpleasant taste. 008 or more, more preferably 0.01 or more, still more preferably 0.02 or more, still more preferably 0.03 or more, still more preferably 0.05 or more, and still more preferably 0.07 or more. In addition, from the viewpoint of suppressing bitterness derived from astragalin, it is preferably 0.5 or less, more preferably 0.4 or less, still more preferably 0.3 or less, still more preferably 0.2 or less, and particularly preferably 0.15 or less. preferable. The range of the mass ratio [(C) / (B)] is preferably 0.004 to 0.5, more preferably 0.008 to 0.4, and still more preferably 0.01 to 0.3. It is still more preferably 0.02 to 0.3, still more preferably 0.03 to 0.2, still more preferably 0.05 to 0.2, and still more preferably 0.07 to 0.15.
本発明の経口組成物は、所望により、酸味料、甘味料、アミノ酸、たんぱく質、ビタミン、ミネラル、香料、果汁、植物エキス、エステル、色素、乳化剤、乳成分、ココアパウダー、調味料、植物油脂、酸化防止剤、保存料、ｐＨ調整剤、品質安定剤、花蜜エキス等の添加剤を１種又は２種以上を含有することができる。添加剤の含有量は、本発明の目的を損なわない範囲内で適宜設定することができる。 The oral composition of the present invention may optionally contain an acidulant, a sweetener, an amino acid, a protein, a vitamin, a mineral, a flavor, a fruit juice, a plant extract, an ester, a pigment, an emulsifier, a milk component, a cocoa powder, a seasoning, a vegetable oil, One or more additives such as an antioxidant, a preservative, a pH adjuster, a quality stabilizer, a nectar extract and the like can be contained. The content of the additive can be appropriately set within a range that does not impair the purpose of the present invention.
また、本発明の経口組成物は、必要に応じて許容される担体を含有することができる。例えば、賦形剤（例えば、グルコース、ガラクトース、フルクトース等の単糖類、スクロース、ラクトース、マルトース、パラチノース等の二糖類、マルチトール、キシリトール、ソルビトール、還元パラチノース等の糖アルコール）；結合剤（例えば、ヒドロキシプロピルメチルセルロース、ヒドロキシプロピルセルロース、ゼラチン、アルファー化デンプン、ポリビニルピロリドン、ポリビニルアルコール、プルラン、メチルセルロース、硬化油等）；崩壊剤（例えば、カルメロース、カルメロースカルシウム、クロスカルメロースナトリウム、クロスポピドン、トウモロコシデンプン、低置換度ヒドロキシプロピルセルロース等）；滑沢剤（例えば、ステアリン酸カルシウム、ステアリン酸マグネシウム、ショ糖脂肪酸エステル、フマル酸ステアリルナトリウム、タルク、二酸化ケイ素等）；嬌味剤（例えば、ステビア等）；オリゴ糖、寒天、結晶セルロース、軽質無水ケイ酸、リン酸水素カルシウム、増量剤、増粘剤、界面活性剤、分散剤、緩衝剤、希釈剤等の担体が挙げられる。なお、担体の含有量は、本発明の目的を損なわない範囲内で適宜設定することが可能である。 In addition, the oral composition of the present invention can contain an acceptable carrier as necessary. For example, excipients (eg, monosaccharides such as glucose, galactose, fructose, disaccharides such as sucrose, lactose, maltose, palatinose, sugar alcohols such as maltitol, xylitol, sorbitol, reduced palatinose); binders (eg, Hydroxypropylmethylcellulose, hydroxypropylcellulose, gelatin, pregelatinized starch, polyvinylpyrrolidone, polyvinylalcohol, pullulan, methylcellulose, hardened oil, etc .; disintegrants (eg, carmellose, carmellose calcium, croscarmellose sodium, crospopidone, corn starch) Lubricants (eg, calcium stearate, magnesium stearate, sucrose fatty acid ester, fuma) Flavoring agents (eg, stevia); oligosaccharides, agar, crystalline cellulose, light anhydrous silicic acid, calcium hydrogen phosphate, extenders, thickeners, surfactants, Carriers such as dispersants, buffers, and diluents are included. The content of the carrier can be appropriately set within a range that does not impair the object of the present invention.
本発明の経口組成物の具体例としては、例えば、インスタント飲料；濃縮飲料；乳飲料、ヨーグルト、チーズ等の乳製品；ゼリー、スナック、ビスケット、米菓等の菓子の飲食品が挙げられ、健康食品（栄養機能食品、特定保健用食品、栄養補助食品、健康補助食品、サプリメント等）、医薬品、医薬部外品とすることもできる。なお、インスタント飲料又は濃縮飲料とは、液体に希釈溶解して飲料として飲用に供されるものをいい、液体は飲料に還元できれば特に限定されない。例えば、水、炭酸水、牛乳、豆乳等が挙げられ、液体の温度は問わない。また、健康食品、医薬品、又は医薬部外品である場合の剤型としては、例えば、顆粒剤、錠剤、カプセル剤、散剤、丸剤、チュアブル剤、トローチ剤等が挙げられる。中でも、経口組成物としては、インスタント飲料、濃縮飲料、ゼリー食品、顆粒剤、錠剤が好ましく、インスタント飲料、濃縮飲料、顆粒剤が更に好ましい。 Specific examples of the oral composition of the present invention include, for example, instant beverages; concentrated beverages; dairy products such as milk drinks, yogurt, and cheese; and confectionery foods and drinks such as jelly, snacks, biscuits, and rice crackers. Foods (functional nutritional foods, foods for specified health use, nutritional supplements, health supplements, supplements, etc.), pharmaceuticals, and quasi-drugs can also be used. In addition, the instant beverage or the concentrated beverage refers to a beverage that is diluted and dissolved in a liquid and provided for drinking as a beverage, and is not particularly limited as long as the liquid can be reduced to the beverage. For example, water, carbonated water, milk, soymilk and the like can be mentioned, and the temperature of the liquid is not limited. Examples of the dosage form in the case of a health food, a pharmaceutical, or a quasi-drug include, for example, granules, tablets, capsules, powders, pills, chewables, and troches. Among them, the oral composition is preferably an instant beverage, a concentrated beverage, a jelly food, a granule, or a tablet, and more preferably an instant beverage, a concentrated beverage, or a granule.
また、経口組成物がインスタント飲料である場合、例えば、瓶等に容器詰し飲用する際にカップ１杯分をスプーン等で計量するもの、１杯分を収容したカップタイプ、カップ１杯分毎に小分け包装したスティックタイプ等とすることができる。また、経口組成物が濃縮飲料である場合、例えば、カップ１杯分毎に小分け包装したポーションタイプの希釈飲料等が挙げられる。なお、カップの容量は３０〜３２０ｍＬであることが好ましく、また小分け包装の内容量はカップ容量に適合するように適宜設定することが可能である。中でも、本発明の効果を享受しやすい点から、カップ１杯分毎に小分け包装したものが好ましく、例えば、スティック包装したもの、ピロー包装したものを挙げることができる。小分け包装は、アルミ蒸着フィルム等を材質とする包装材料で包装することができる。なお、容器内及び包材内は窒素ガスを充填してもよく、また包材は酸素透過性の低いものが品質維持の点で好ましい。 When the oral composition is an instant beverage, for example, when a bottle is packed in a bottle or the like and one cup is weighed with a spoon or the like when drinking, a cup type containing one cup, every cup It can be a stick type or the like which is subdivided and packaged. When the oral composition is a concentrated beverage, for example, a portion-type diluted beverage that is packaged in small portions for each cup is exemplified. In addition, the capacity of the cup is preferably 30 to 320 mL, and the inner capacity of the subdivided package can be appropriately set so as to match the capacity of the cup. Among them, from the viewpoint that the effects of the present invention can be easily enjoyed, those packaged in small portions for each cup are preferable, and examples thereof include those packaged in sticks and those packaged in pillows. The subdivided packaging can be packaged with a packaging material made of an aluminum evaporated film or the like. The inside of the container and the inside of the packaging material may be filled with nitrogen gas, and the packaging material is preferably low in oxygen permeability from the viewpoint of maintaining quality.
本発明の経口組成物は、常法にしたがって製造することが可能であり、適宜の方法を採り得る。例えば、特定量の成分（Ａ）、成分（Ｂ）及び成分（Ｃ）、必要に応じて担体及び／又は添加剤を、成分（Ａ）及び成分（Ｃ）の各含有量、並びに成分（Ａ）と成分（Ｂ）との質量比[（Ｂ）／（Ａ）]が上記範囲内となるように混合して製造することができる。成分（Ａ）、成分（Ｂ）及び成分（Ｃ）の混合順序は特に限定されず、任意の順序で添加しても、３者を同時に添加してもよい。混合方法としては、撹拌、震盪等の適宜の方法を採用することが可能であり、混合装置を使用しても構わない。混合装置の混合方式は、容器回転型でも、容器固定型でもよい。容器回転型として、例えば、水平円筒型、Ｖ型、ダブルコーン型、立方体型等を採用することができる。また、容器固定型として、例えば、リボン型、スクリュー型、円錐形スクリュー型、パドル型、流動層型、フィリップスブレンダ−等を採用することができる。また、公知の造粒法により造粒物としてもよい。造粒方法としては、例えば、噴霧造粒、流動層造粒、圧縮造粒、転動造粒、撹拌造粒、押出造粒、粉末被覆造粒等が挙げられる。なお、造粒条件は、造粒方法により適宜選択することができる。また、錠剤とする場合には、湿式打錠及び乾式打錠のいずれでもよく、公知の圧縮成形機を使用することができる。更に、濃縮液状である場合、例えば、常圧にて溶媒の蒸発を行う常圧濃縮法、減圧にて溶媒の蒸発を行う減圧濃縮法、膜分離により溶媒を除去する膜濃縮法等の公知の濃縮方法を採用することができる。 The oral composition of the present invention can be produced according to a conventional method, and an appropriate method can be adopted. For example, specific amounts of component (A), component (B) and component (C), and if necessary, a carrier and / or an additive, the content of each of component (A) and component (C), and component (A) ) And component (B) so that the mass ratio [(B) / (A)] is within the above range. The mixing order of the component (A), the component (B) and the component (C) is not particularly limited, and they may be added in an arbitrary order or may be added simultaneously. As a mixing method, an appropriate method such as stirring or shaking can be adopted, and a mixing device may be used. The mixing method of the mixing device may be a rotating container type or a fixed container type. As the container rotating type, for example, a horizontal cylindrical type, a V type, a double cone type, a cubic type, or the like can be adopted. Further, as the container fixed type, for example, a ribbon type, a screw type, a conical screw type, a paddle type, a fluidized bed type, a Philips blender and the like can be adopted. Further, a granulated product may be obtained by a known granulation method. Examples of the granulation method include spray granulation, fluidized bed granulation, compression granulation, tumbling granulation, stirring granulation, extrusion granulation, and powder coating granulation. The granulation conditions can be appropriately selected depending on the granulation method. In the case of making a tablet, any of wet tableting and dry tableting may be used, and a known compression molding machine can be used. Furthermore, in the case of a concentrated liquid, for example, a known concentration method such as a normal pressure concentration method in which the solvent is evaporated at normal pressure, a reduced pressure concentration method in which the solvent is evaporated under reduced pressure, and a membrane concentration method in which the solvent is removed by membrane separation. Concentration methods can be employed.
１．デキストリンの分析
（１）定量法
試料、及び各濃度の標準溶液１．５ｍＬに、１Ｎ−ＮａＯＨ水溶液を２５０μＬと０．５ＭのＰＭＰ（３−メチル−１−フェニル−５−ピラゾロン）−メタノール溶液を５００μＬ加え、７０℃で３０分加熱する。得られた溶液に対し、１Ｎ−ＨＣｌ水溶液を２５０μＬにて中和し、５ｍＬのクロロホルムを加え分配し、水層を測定試料とする。上記操作により得られた測定試料について、高速液体クロマトグラフ質量分析を用い、下記条件にて測定する。
1. Analysis of dextrin (1) Quantitative method To a sample and 1.5 mL of a standard solution of each concentration, 250 μL of 1N-NaOH aqueous solution and 0.5 M of PMP (3-methyl-1-phenyl-5-pyrazolone) -methanol solution were added. Add 500 μL and heat at 70 ° C. for 30 minutes. The obtained solution is neutralized with a 1N-HCl aqueous solution with 250 μL, and 5 mL of chloroform is added and partitioned, and the aqueous layer is used as a measurement sample. The measurement sample obtained by the above operation is measured under the following conditions using high performance liquid chromatography / mass spectrometry.
分析条件
・ＨＰＬＣ装置：型式ＡＣＱＵＩＴＹ ＵＰＬＣ、Ｗａｔｅｒｓ製
・ＭＳ装置 ：型式ＳＹＮＡＰＴ Ｇ２−Ｓ ＨＤＭＳ型、Ｗａｔｅｒｓ製
・イオン化 ：ＥＳＩ
・質量範囲 ：ｍ／ｚ １００−２５００
・カラム ：型式Ｕｎｉｓｏｎ ＵＫ−Ｃ１８ ＵＰ(２．０×１００ｍｍ,３μｍ)，インタクト社製
・移動相 ：Ｅ液：ギ酸０．０５％水溶液、Ｆ液：アセトニトリル(％Ｆ＝１５→９０)
・流量 ：０．６ｍＬ／ｍｉｎ
・注入量 ：１μＬ
Analysis conditions / HPLC device: Model ACQUITY UPLC, manufactured by Waters / MS device: Model SYNAPT G2-S HDMS model, manufactured by Waters / Ionization: ESI
-Mass range: m / z 100-2500
・ Column: Model Unison UK-C18 UP (2.0 × 100 mm, 3 μm), manufactured by Intact Corporation ・ Mobile phase: E solution: 0.05% formic acid aqueous solution, F solution: acetonitrile (% F = 15 → 90)
・ Flow rate: 0.6 mL / min
・ Injection volume: 1 μL
（２）デキストロース当量
（Ｉ）分析は、デキストリンに含まれているぶどう糖、麦芽糖などの還元糖分をぶどう糖として定量する場合に適用し、次の手順にしたがって行う。
・水分の定量
・レイン・エイノン法による還元糖分の定量
・ぶどう糖として計算した還元糖の含有率（ＤＥ値、％）の計算
(2) The dextrose equivalent (I) analysis is applied to a case where reducing sugars such as glucose and maltose contained in dextrin are quantified as glucose, and is performed according to the following procedure.
・ Quantification of water content ・ Quantification of reducing sugar content by Rain-Aynon method ・ Calculation of reducing sugar content (DE value,%) calculated as glucose
（II）試料の調製及び力価の標定
（II-A）試料の調製
（II-1）標準転化糖溶液
スクロース（試薬）４．７５ｇを正確に量り取り、９０ｍＬの水を使用して５００ｍＬ容メスフラスコに移し入れる。これに塩酸（比重１．１８）５ｍＬを加え、２０〜３０℃で３日間放置した後、水を加えて定容し、冷暗所に保存する。その５０ｍＬを２００ｍＬ容メスフラスコにとり、フェノールフタレインを指示薬として１ｍｏｌ／Ｌ水酸化ナトリウム溶液で中和した後、水を加えて定容する。これを転化糖溶液としてフェーリング溶液の力価の標定に用いる。
（II-2）メチレンブルー溶液
１％メチレンブルー１ｇを水に溶かして１００ｍＬとする。
（II-3）フェーリング溶液
Ａ液：硫酸銅（CuSO4・5H2O）３４．６３９ｇを水に溶かして５００ｍＬとし、２日間放置後ろ過する。
Ｂ液：酒石酸カリウムナトリウム（KNaC4H4O6・4H2O）１７３ｇと水酸化ナトリウム５０ｇを水に溶かして５００ｍＬとし、これを２日間放置後ろ過する。
(II) Preparation of sample and standardization of titer (II-A) Preparation of sample (II-1) Standard invert sugar solution Weigh accurately 4.75 g of sucrose (reagent), and use a 90 mL water to make a 500 mL volume. Transfer to a volumetric flask. To this, 5 mL of hydrochloric acid (specific gravity: 1.18) was added, and the mixture was allowed to stand at 20 to 30 ° C. for 3 days. 50 mL thereof is placed in a 200 mL volumetric flask, neutralized with a 1 mol / L sodium hydroxide solution using phenolphthalein as an indicator, and then water is added thereto to make the volume constant. This is used as an invert sugar solution to determine the titer of the Fehling's solution.
(II-2) Methylene blue solution Dissolve 1 g of 1% methylene blue in water to make 100 mL.
(II-3) Fehling's solution A solution: 34.639 g of copper sulfate (CuSO 4 .5H 2 O) is dissolved in water to 500 mL, and left to stand for 2 days, followed by filtration.
Solution B: 173 g of potassium sodium tartrate (KNaC 4 H 4 O 6 .4H 2 O) and 50 g of sodium hydroxide are dissolved in water to make 500 mL, which is left for 2 days and filtered.
（II-B）フェーリング溶液の力価の標定
フェーリング溶液Ａ液５．０ｍＬ及びＢ液５ｍＬを２００ｍＬ容三角フラスコにとり、５０ｍＬ容ビュレットを用いて標準転化糖溶液１９．５ｍＬを加える。電熱器上で２分間沸騰させた後、メチレンブルー溶液４滴を加え、沸騰しながら標準転化糖溶液を滴下し、青色が消失したところを終点とする。滴定は沸騰し始めてから３分以内に終了する。この滴定を３回行い、平均値を求める。但し、３回の平均値を滴定値とするが、各滴定値の差は０．１ｍＬ以内とする。また、力価の小数点以下第４位を四捨五入し、１±０．０２の範囲内に収める。
(II-B) Determination of titer of Fehling solution 5.0 mL of Fehling solution A and 5 mL of B solution are placed in a 200 mL Erlenmeyer flask, and 19.5 mL of standard invert sugar solution is added using a 50 mL burette. After boiling on an electric heater for 2 minutes, 4 drops of methylene blue solution are added, and the standard invert sugar solution is added dropwise while boiling, and the point where the blue color disappears is regarded as the end point. The titration is completed within 3 minutes after starting to boil. This titration is performed three times, and the average value is determined. However, the average value of the three times is defined as the titration value, and the difference between the titration values is within 0.1 mL. The titer is rounded off to the fourth decimal place to fall within the range of 1 ± 0.02.
〔式中、Ａは、消費した標準転化糖溶液の量（ｍＬ）を示す。〕 [In the formula, A indicates the amount (mL) of the consumed standard invert sugar solution. ]
（III）試料の調製
分析試料は、試料の性状に応じて、次により調製する。
（III-1）液体試料
液体中に結晶又は塊状物が析出している場合には、密閉容器に入れ、６０〜７０℃の水浴に浸漬して溶解し、よく振り混合した後、室温に冷却する。
（III-2）固体試料
粉末又は結晶状とし、塊がある場合には砕き、よく混合する。
(III) Sample preparation The analysis sample is prepared as follows according to the properties of the sample.
(III-1) Liquid sample If crystals or lumps are precipitated in the liquid, put it in a closed container, immerse it in a water bath at 60 to 70 ° C, dissolve it, shake well, and cool it to room temperature. I do.
(III-2) Solid sample Powder or crystal form. If there are lumps, crush and mix well.
（IV）水分の定量
水分の定量は、試料の性状により、次の方法で行う。
（IV-1）液体試料
乾燥助剤として、予め秤量瓶に海砂を約１５ｇ取り、ガラス棒とともに１０５℃の乾燥機中で乾燥して恒量を求める。次に、前記（III）で調製した均一試料を固形分として約２ｇに相当する量を正確に量り取り、必要があれば少量の水を全体が浸るまで加え、時々ガラス棒でかき混ぜながら水浴上で加熱して大部分の水を揮散させる。更に、１０５℃の乾燥機内で時々かき混ぜ、ほとんど乾燥するまで乾かした後、真空乾燥機に移し、７０℃で４時間乾燥する。デシケータ中で室温まで放冷した後、重量を量る。１時間ずつ真空乾燥を繰り返して恒量を求める。減量が、２ｍｇ以下の変化になった時を恒量に達したとみなす。
（IV-2）固体試料
前記（III）で調製した均一試料約２ｇを予め恒量にした秤量瓶に正確に量り取り、真空乾燥機で７０℃、４時間乾燥する。次に、デシケータ中で室温まで放冷した後、重量を量る。更に、１時間ずつ真空乾燥を繰り返して、減量が２ｍｇ以下の変化になった時を恒量に達したとみなす。
（IV-3）水分の計算
試料中の水分は、次式により算出する。数値は小数点以下第２位を四捨五入する。
(IV) Quantification of water The water content is determined by the following method, depending on the properties of the sample.
(IV-1) Liquid sample As a drying aid, about 15 g of sea sand is previously taken in a weighing bottle and dried together with a glass rod in a dryer at 105 ° C. to obtain a constant weight. Next, the homogeneous sample prepared in the above (III) was weighed accurately in an amount corresponding to about 2 g as a solid content, and if necessary, a small amount of water was added until the whole was soaked, and occasionally stirred on a water bath while stirring with a glass rod. To evaporate most of the water. Further, the mixture is occasionally stirred in a dryer at 105 ° C., dried until almost dry, transferred to a vacuum dryer, and dried at 70 ° C. for 4 hours. After allowing to cool to room temperature in a desiccator, weigh. Vacuum drying is repeated for one hour to obtain a constant weight. When the weight loss changes by 2 mg or less, it is considered to have reached a constant weight.
(IV-2) Solid sample About 2 g of the uniform sample prepared in the above (III) is accurately weighed in a weighing bottle having a constant weight, and dried at 70 ° C. for 4 hours by a vacuum dryer. Next, after cooling to room temperature in a desiccator, the weight is measured. Further, vacuum drying is repeated for one hour, and when the weight loss changes by 2 mg or less, it is considered that the weight has reached a constant weight.
(IV-3) Calculation of moisture The moisture in the sample is calculated by the following formula. Numbers are rounded to the first decimal place.
〔式中、Ｗ0は試料の採取量（ｇ）を示し、Ｗ1は乾燥後の試料の重量（ｇ）を示す。〕 [In the formula, W 0 indicates the amount (g) of sample collected, and W 1 indicates the weight (g) of the sample after drying. ]
（Ｖ）ＤＥ値の定量
（V-1）検液の調製
前記（III）で調製した均一試料約１０ｇを正確に量り取り、水に溶かして５００ｍＬ容メスフラスコに移し入れ、水を加えて容定し検液とする。
（V-2）滴定操作
フェーリング溶液Ａ液５．０ｍＬ及びＢ液５ｍＬを２００ｍＬ容三角フラスコに採り、５０ｍＬ容ビュレットを用いて、（Ｖ-1）で調製した検液１５ｍLを加え、（II-B）の要領にしたがって滴定し、これを予備滴定とする。更に同様にして、予備滴定で得た滴定数より約１ｍＬ少ない量の検液を加え、（II-B）の要領にしたがって滴定する。ここで得た検液の消費量にフェーリング溶液の力価を乗じ、この数値から表１に示すレイン・エイノン糖量表（ぶどう糖）を用いて還元糖濃度（ＤＥ値，ｍｇ／１００ｍＬ）をぶどう糖として求める。
（V-3）ＤＥ値の計算
試料の乾燥状態におけるぶどう糖として計算したＤＥ値は、次式により算出する。数値は、小数点以下第２位を四捨五入する。
(V) Determination of DE value (V-1) Preparation of test solution Approximately 10 g of the homogeneous sample prepared in (III) above was accurately weighed, dissolved in water, transferred to a 500 mL volumetric flask, added with water, and added to the volume. Determine the test solution.
(V-2) Titration operation Transfer 5.0 mL of the Fehling solution A and 5 mL of the B solution into a 200 mL Erlenmeyer flask, add 15 mL of the test solution prepared in (V-1) using a 50 mL burette, and add (II- Titrate according to the procedure in B), and use this as the preliminary titration. Further, similarly, add a test solution in an amount of about 1 mL less than the titer obtained in the preliminary titration, and titrate according to the procedure of (II-B). The consumption of the test solution obtained here is multiplied by the titer of the Fehling's solution, and the reducing sugar concentration (DE value, mg / 100 mL) is determined from this value using the Rein-Aynone sugar amount table (glucose) shown in Table 1. Asking.
(V-3) Calculation of DE value The DE value calculated as glucose in a dry state of a sample is calculated by the following equation. Numbers are rounded to the first decimal place.
〔式中、
ＤSは、表１に示すレイン・エイノン糖量表（ぶどう糖）を用いて求めた検液１００ｍＬ中のぶどう糖量（ｍｇ）を示し、
Ｍは、（IV）で秤量した試料の水分（％）を示し、
Ｓは、（Ｖ-1）で秤量した試料の採取量（ｇ）を示す。〕
(In the formula,
D S indicates rain Einon sugar amount table shown in Table 1 (glucose) glucose amount in the test solution 100mL was determined using the (mg),
M represents the moisture (%) of the sample weighed in (IV),
S indicates the amount (g) of the sample weighed in (V-1). ]
２．カフェインの分析
試料溶液をフィルター（０．４５μｍ）で濾過し、高速液体クロマトグラフ（型式ＳＣＬ−１０ＡＶＰ）を用い、オクタデシル基導入液体クロマトグラフ用パックドカラム（Ｌ−カラムＴＭ ＯＤＳ、４．６ｍｍφ×２５０ｍｍ：財団法人 化学物質評価研究機構製）を装着し、カラム温度３５℃でグラジエント法により測定した。移動相Ａ液は酢酸を０．１ｍｏｌ／Ｌ含有する蒸留水溶液、Ｂ液は酢酸を０．１ｍｏｌ／Ｌ含有するアセトニトリル溶液とし、流速は１ｍＬ／分、試料注入量は１０μＬ、ＵＶ検出器波長は２８０ｎｍの条件で行った。グラジエント条件は以下の通りである。リテンションタイム条件は、カフェインの標準試薬を用いて設定した。
2. Analysis of Caffeine The sample solution was filtered through a filter (0.45 μm), and a packed column (L-column TM ODS, 4.6 mmφ ×) for octadecyl group-introduced liquid chromatography was applied using a high performance liquid chromatograph (model SCL-10AVP). 250 mm: manufactured by Chemicals Evaluation and Research Institute, Japan) and measured at a column temperature of 35 ° C. by a gradient method. The mobile phase A solution was a distilled aqueous solution containing 0.1 mol / L of acetic acid, and the B solution was an acetonitrile solution containing 0.1 mol / L of acetic acid. The flow rate was 1 mL / min, the sample injection amount was 10 μL, and the UV detector wavelength was The measurement was performed at 280 nm. The gradient conditions are as follows. The retention time condition was set using a caffeine standard reagent.
濃度勾配条件
時間（分） Ａ液濃度（体積％） Ｂ液濃度（体積％）
０分 ９７％ ３％
５分 ９７％ ３％
３７分 ８０％ ２０％
４３分 ８０％ ２０％
４３．５分 ０％ １００％
４８．５分 ０％ １００％
４９分 ９７％ ３％
６０分 ９７％ ３％
Concentration gradient conditions Time (min) Solution A concentration (% by volume) Solution B concentration (% by volume)
0 minutes 97% 3%
5 minutes 97% 3%
37 minutes 80% 20%
43 minutes 80% 20%
43.5 minutes 0% 100%
48.5 minutes 0% 100%
49 minutes 97% 3%
60 minutes 97% 3%
３．アストラガリンの分析
試料溶液をフィルター（０．４５μｍ）で濾過し、高速液体クロマトグラフ（型式ＬＣ−２０ Ｐｒｏｍｉｎｅｎｃｅ，島津製作所製）を用い、カラム〔Ｃａｄｅｎｚａ ＣＤ−Ｃ１８（３μｍ，４．６ｍｍφ×１５０ｍｍ，Ｉｍｔａｋｔ）〕を装着し、カラム温度４０℃にてグラジエント法により行った。移動相Ｃ液は酢酸を０．０５質量％含有するアセトニトリル溶液、Ｄ液はアセトニトリル溶液とし、流速は１ｍＬ／分、試料注入量は１０μＬ、ＵＶ検出器波長は３６０ｎｍの条件で行った。なお、グラジエントの条件は、以下のとおりである。
3. Analysis of Astragalin The sample solution was filtered with a filter (0.45 μm), and a column [Cadenza CD-C18 (3 μm, 4.6 mmφ × 150 mm, 3 μm, 4.6 mmφ × 150 mm, high performance liquid chromatograph (model: LC-20 Prominence, manufactured by Shimadzu Corporation)) was used. Imtakt)] and a gradient method at a column temperature of 40 ° C. The mobile phase C solution was an acetonitrile solution containing 0.05% by mass of acetic acid, the D 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 360 nm. The conditions for the gradient are as follows.
濃度勾配条件
時間（分） Ｃ液濃度（体積％） Ｄ液濃度（体積％）
０ ８５％ １５％
２０ ８０％ ２０％
３５ １０％ ９０％
５０ １０％ ９０％
５０．１ ８５％ １５％
６０ ８５％ １５％
Concentration gradient condition Time (min) Solution C concentration (% by volume) Solution D concentration (% by volume)
0 85% 15%
20 80% 20%
35 10% 90%
50 10% 90%
50.1 85% 15%
60 85% 15%
アストラガリンの標準品を用いて濃度既知の標準溶液を調製し、上記分析条件にて高速液体クロマトグラフ分析に供することによりリテンションタイムを測定するとともに、検量線を作成した。
・アストラガリン ：１８．２分
上記リテンションタイムで一致したピークをアストラガリンとして試料溶液中の各成分の定量を行った。
A standard solution having a known concentration was prepared using an astragalin standard product, and subjected to high performance liquid chromatography under the above-described analysis conditions to measure the retention time and to prepare a calibration curve.
Astragalin: 18.2 minutes Each component in the sample solution was quantified using as peak astragalin the above retention time as astragalin.
実施例１〜５、比較例１、２及び参考例１、２
表２に示す各成分を均一に混合し、インスタント粉末飲料を得た。得られたインスタント粉末飲料について分析及び官能評価を行った。その結果を表２に示す。なお、得られたインスタント粉末飲料は、いずれも固形分量が９７．０質量％であった。
Examples 1 to 5, Comparative Examples 1 and 2 and Reference Examples 1 and 2
The components shown in Table 2 were uniformly mixed to obtain an instant powdered beverage. The obtained instant powdered beverage was analyzed and sensory evaluated. Table 2 shows the results. In addition, all of the obtained instant powder drinks had a solid content of 97.0 mass%.
官能評価１
上記の各実施例、比較例及び参考例で得られたインスタント粉末飲料１ｇを、それぞれ８０℃の熱水１００ｍＬで溶解して還元飲料を調製し、各還元飲料を飲用したときの「不快味」について、専門パネル４名が官能試験を行った。官能試験は、各パネリストが「不快味」の評価基準を、下記の評価基準とすることに合意したうえで実施した。そして、専門パネルの評点の平均値を求めた。なお、評点の平均値は、小数第２位を四捨五入するものとする。
Sensory evaluation 1
"Unpleasant taste" when 1 g of the instant powdered beverage obtained in each of the above Examples, Comparative Examples and Reference Examples was dissolved in 100 mL of hot water at 80 ° C. to prepare reduced beverages, and each reduced beverage was consumed. , Four specialized panels performed a sensory test. The sensory test was carried out after each panelist agreed that the evaluation criteria for “unpleasant taste” were the following evaluation criteria. Then, the average value of the scores of the specialized panels was obtained. The average score is rounded to the first decimal place.
不快味の評価基準
不快味は、飲用したときに不快味が感じられるか否かを観点に、比較例１の還元飲料の不快味の評点を「１」とし、実施例３の還元飲料の不快味の評点を「５」として評価した。具体的な評価基準は以下のとおりである。
１：不快味を強く感じる
２：不快味を感じる
３：不快味を少し感じる
４：不快味をほとんど感じない
５：不快味を感じない
Evaluation criteria of unpleasant taste The unpleasant taste was evaluated as "1" for the unpleasant taste of the reduced beverage of Comparative Example 1 from the viewpoint of whether or not unpleasant taste was felt when drinking, and the unpleasant taste of the reduced beverage of Example 3 was evaluated. The taste was rated as "5". The specific evaluation criteria are as follows.
1: strong unpleasant taste 2: unpleasant taste 3: slightly unpleasant taste 4: little unpleasant taste 5: no unpleasant taste
実施例６〜８及び比較例３
表３に示す各成分を均一に混合し、インスタント粉末飲料を得た。得られたインスタント粉末飲料について分析及び官能評価を行った。なお、官能評価は、実施例１と同様の方法で調製された還元飲料について、官能評価１と同一基準にて実施した。その結果を、参考例１の結果とともに表３に示す。得られたインスタント粉末飲料は、いずれも固形分量が９７．０質量％であった。
Examples 6 to 8 and Comparative Example 3
The components shown in Table 3 were uniformly mixed to obtain an instant powdered beverage. The obtained instant powdered beverage was analyzed and sensory evaluated. The sensory evaluation was carried out on the reduced beverage prepared in the same manner as in Example 1 on the same basis as the sensory evaluation 1. The results are shown in Table 3 together with the results of Reference Example 1. All of the obtained instant powder beverages had a solid content of 97.0% by mass.
実施例９及び比較例４
表４に示す各成分を均一に混合し、インスタント粉末飲料を得た。得られたインスタント粉末飲料について分析及び官能評価を行った。なお、官能評価は、実施例１と同様の方法で調製された還元飲料について、官能評価１と同一基準にて実施した。その結果を、参考例１の結果とともに表４に示す。得られたインスタント粉末飲料は、いずれも固形分量が９７．０質量％であった。
Example 9 and Comparative Example 4
The components shown in Table 4 were uniformly mixed to obtain an instant powdered beverage. The obtained instant powdered beverage was analyzed and sensory evaluated. The sensory evaluation was carried out on the reduced beverage prepared in the same manner as in Example 1 on the same basis as the sensory evaluation 1. Table 4 shows the results together with the results of Reference Example 1. All of the obtained instant powder beverages had a solid content of 97.0% by mass.
実施例１０及び比較例５
表５に示す各成分を均一に混合し、インスタント粉末飲料を得た。得られたインスタント粉末飲料について分析及び官能評価を行った。なお、官能評価は、実施例１と同様の方法で調製された還元飲料について、官能評価１と同一基準にて実施した。その結果を、参考例１の結果とともに表５に示す。得られたインスタント粉末飲料は、いずれも固形分量が９７．０質量％であった。
Example 10 and Comparative Example 5
The components shown in Table 5 were uniformly mixed to obtain an instant powdered beverage. The obtained instant powdered beverage was analyzed and sensory evaluated. The sensory evaluation was carried out on the reduced beverage prepared in the same manner as in Example 1 on the same basis as the sensory evaluation 1. Table 5 shows the results together with the results of Reference Example 1. All of the obtained instant powder beverages had a solid content of 97.0% by mass.
実施例１１〜１３、比較例６〜８及び参考例３
表６に示す各成分を均一に混合し、インスタント粉末飲料を得た。得られたインスタント粉末飲料について分析及び官能評価を行った。なお、官能評価は、実施例１と同様の方法で調製された還元飲料について、参考例３で得られた還元飲料の不快味の評点を「２」とすることに合意したうえで実施した。また、評価基準は、官能評価１と同一の５段階で評価した。そして、専門パネルの評点の平均値を求めた。なお、評点の平均値は、小数第２位を四捨五入するものとする。その結果を表６に示す。得られたインスタント粉末飲料は、いずれも固形分量が９７．０質量％であった。
Examples 11 to 13, Comparative Examples 6 to 8 and Reference Example 3
The components shown in Table 6 were uniformly mixed to obtain an instant powdered beverage. The obtained instant powdered beverage was analyzed and sensory evaluated. In addition, the sensory evaluation was performed on the reduced beverage prepared in the same manner as in Example 1 after agreeing that the rating of the unpleasant taste of the reduced beverage obtained in Reference Example 3 was “2”. In addition, evaluation criteria were evaluated in the same five stages as sensory evaluation 1. Then, the average value of the scores of the specialized panels was obtained. The average score is rounded to the first decimal place. Table 6 shows the results. All of the obtained instant powder beverages had a solid content of 97.0% by mass.
実施例１４、１５、比較例９、１０及び参考例４、５
表７に示す各成分を均一に混合し、インスタント粉末飲料を得た。得られたインスタント粉末飲料について分析及び官能評価を行った。なお、官能評価は、実施例１と同様の方法で各還元飲料を調製した後、実施例１４、比較例９及び参考例４の還元飲料については比較例９で得られた還元飲料の不快味の評点を「１」とし、実施例１５、比較例１０及び参考例５の還元飲料については比較例１０で得られた還元飲料の不快味の評点を「１」とすることに合意したうえで実施した。また、評価基準は、官能評価１と同一の５段階で評価した。そして、専門パネルの評点の平均値を求めた。なお、評点の平均値は、小数第２位を四捨五入するものとする。その結果を、実施例３、比較例１及び参考例１の結果とともに表７に示す。得られたインスタント粉末飲料は、いずれも固形分量が９７．０質量％であった。
Examples 14 and 15, Comparative Examples 9 and 10, and Reference Examples 4 and 5
The components shown in Table 7 were uniformly mixed to obtain an instant powdered beverage. The obtained instant powdered beverage was analyzed and sensory evaluated. In the sensory evaluation, after preparing each reduced beverage in the same manner as in Example 1, for the reduced beverages of Example 14, Comparative Example 9 and Reference Example 4, the unpleasant taste of the reduced beverage obtained in Comparative Example 9 Of the reduced beverage of Example 15, Comparative Example 10 and Reference Example 5 after agreeing that the score of the unpleasant taste of the reduced beverage obtained in Comparative Example 10 was "1". Carried out. In addition, evaluation criteria were evaluated in the same five stages as sensory evaluation 1. Then, the average value of the scores of the specialized panels was obtained. The average score is rounded to the first decimal place. The results are shown in Table 7 together with the results of Example 3, Comparative Example 1, and Reference Example 1. All of the obtained instant powder beverages had a solid content of 97.0% by mass.
実施例１６、比較例１１及び参考例６
表８に示す各成分を均一に混合し、インスタント粉末緑茶飲料を得た。得られたインスタント粉末緑茶飲料について分析及び官能評価を行った。
Example 16, Comparative Example 11, and Reference Example 6
The components shown in Table 8 were uniformly mixed to obtain an instant powdered green tea beverage. The resulting instant powdered green tea beverage was analyzed and sensory evaluated.
官能評価２
上記の各実施例、比較例及び参考例で得られたインスタント粉末緑茶飲料１ｇを、それぞれ８０℃の熱水１００ｍＬで溶解させて還元飲料を調製した。還元飲料は途中インスタント粉末緑茶飲料がダマにならないよう熱水を３０秒かけてゆっくり注ぎ、茶筅でよく攪拌しながら均一に溶解するよう調製した。官能評価は、各還元飲料を飲用したときの「不快味」について、専門パネル４名が官能試験を行った。官能試験は、各パネリストが比較例１１で得られた還元飲料の不快味の評点を「１」とすることに合意したうえで実施した。また、評価基準は、官能評価１と同一の５段階で評価した。そして、専門パネルの評点の平均値を求めた。なお、評点の平均値は、小数第２位を四捨五入するものとする。その結果を表８に示す。得られたインスタント粉末緑茶飲料は、いずれも固形分量が９７．０質量％であった。
Sensory evaluation 2
1 g of the instant powdered green tea beverage obtained in each of the above Examples, Comparative Examples and Reference Examples was dissolved in 100 mL of hot water at 80 ° C. to prepare a reduced beverage. The reduced beverage was prepared by slowly pouring hot water over 30 seconds so that the instant powdered green tea beverage would not be littered on the way, and uniformly dissolving it with good stirring with a tea whisk. In the sensory evaluation, four specialized panels performed a sensory test on “unpleasant taste” when each reduced beverage was drunk. The sensory test was performed after each panelist agreed that the rating of the unpleasant taste of the reduced beverage obtained in Comparative Example 11 was “1”. In addition, evaluation criteria were evaluated in the same five stages as sensory evaluation 1. Then, the average value of the scores of the specialized panels was obtained. The average score is rounded to the first decimal place. Table 8 shows the results. Each of the obtained instant powdered green tea beverages had a solid content of 97.0% by mass.
実施例１７、比較例１２及び参考例７
８０℃に加温した温水９ｍＬにキサンタンガムを０．２ｇ添加し完全に溶解させポーション原液を調製した。次いで表９に示す成分のうちキサンタンガム以外の成分を均一に混合した粉末組成物をポーション原液に添加し完全に溶解させた。得られたポーション原液を容器（ポリスチレン、容量：１５ｍＬ、口径４３×高さ２６ｍｍ）に流し入れ、ヘッドスペースの空気を窒素ガスに置換した上でフタで密封し、容器入りポーションを製造した。得られた容器入りポーションについて分析及び官能評価を行った。なお、官能評価は、各実施例、比較例及び参考例で得られたポーション１０ｇを、８０℃の熱水９０ｍＬでそれぞれ希釈して調製し、各還元飲料を飲用したときの「不快味」について、専門パネル４名が官能試験を行った。官能試験は、各パネリストが比較例１２で得られた還元飲料の不快味の評点を「１」とすることに合意したうえで実施した。また、評価基準は、官能評価１と同一の５段階で評価した。そして、専門パネルの評点の平均値を求めた。なお、評点の平均値は、小数第２位を四捨五入するものとする。その結果を表９に示す。
Example 17, Comparative Example 12, and Reference Example 7
0.2 g of xanthan gum was added to 9 mL of warm water heated to 80 ° C. and completely dissolved to prepare a stock solution of potion. Next, a powder composition obtained by uniformly mixing components other than xanthan gum among the components shown in Table 9 was added to the stock portion liquid and completely dissolved. The obtained potion stock solution was poured into a container (polystyrene, volume: 15 mL, diameter 43 × height 26 mm), and the air in the head space was replaced with nitrogen gas and sealed with a lid to produce a potion in a container. Analysis and sensory evaluation were performed on the obtained potion in a container. In addition, the sensory evaluation was prepared by diluting 10 g of the potion obtained in each example, comparative example and reference example with 90 mL of hot water of 80 ° C., respectively, and regarding “unpleasant taste” when each reduced beverage was drunk. And four specialized panels performed a sensory test. The sensory test was performed after each panelist agreed that the rating of the unpleasant taste of the reduced beverage obtained in Comparative Example 12 was “1”. In addition, evaluation criteria were evaluated in the same five stages as sensory evaluation 1. Then, the average value of the scores of the specialized panels was obtained. The average score is rounded to the first decimal place. Table 9 shows the results.
実施例１８、１９、比較例１３、１４及び参考例８、９
表１０に示す各成分を均一に混合し、次いで単発式打錠機（ＲＩＫＥＮ社製）を用いて、穴径１４ｍｍのリング状杵で、質量１ｇ／１錠にて打錠し、円形の錠剤を得た。得られた錠剤について分析及び官能評価を行った。なお、得られた錠剤は、いずれも固形分量が９７．０質量％であった。
Examples 18 and 19, Comparative Examples 13 and 14, and Reference Examples 8 and 9
The components shown in Table 10 were uniformly mixed, and then, using a single-shot tableting machine (manufactured by RIKEN), the tablets were punched at a mass of 1 g / 1 tablet with a ring-shaped punch having a hole diameter of 14 mm to obtain circular tablets. Got. The obtained tablets were analyzed and sensory evaluated. In addition, all of the obtained tablets had a solid content of 97.0% by mass.
官能評価３
上記の各実施例、比較例及び参考例で得られた錠剤１錠を水なしで口に含み、腔内に含んだ後直ちに噛み砕き、唾液により錠剤が口内で完全に消滅したときの「不快味」について、専門パネル４名が官能試験を行った。官能試験では、各パネリストが「不快味」の評価基準を、下記の評価基準とすることに合意したうえで実施した。そして、専門パネルの評点の平均値を求めた。なお、評点の平均値は、小数第２位を四捨五入するものとする。
Sensory evaluation 3
One tablet obtained in each of the above Examples, Comparative Examples and Reference Examples was contained in the mouth without water, and immediately after being contained in the cavity, it was crushed, and the tablet was completely unpleasant in the mouth with saliva. , Four specialized panels performed a sensory test. The sensory test was performed after each panelist agreed that the evaluation criteria for “unpleasant taste” were the following evaluation criteria. Then, the average value of the scores of the specialized panels was obtained. The average score is rounded to the first decimal place.
不快味の評価基準
不快味は、服用したときに不快味が感じられるか否かを観点に、実施例１８、比較例１３及び参考例８の錠剤については比較例１３の錠剤の不快味の評点を「１」とし、実施例１９、比較例１４及び参考例９の錠剤については比較例１４で得られた錠剤の不快味の評点を「１」として評価した。具体的な評価基準は以下のとおりである。
１：不快味を強く感じる
２：不快味を感じる
３：不快味を少し感じる
４：不快味をほとんど感じない
５：不快味を感じない
Evaluation criteria of unpleasant taste The unpleasant taste was evaluated from the viewpoint of whether or not unpleasant taste was felt when taken, and the tablets of Example 18, Comparative Example 13 and Reference Example 8 were evaluated for the unpleasant taste of the tablet of Comparative Example 13. Was set to "1", and the tablets of Example 19, Comparative Example 14, and Reference Example 9 were evaluated with the score of the unpleasant taste of the tablet obtained in Comparative Example 14 set to "1". The specific evaluation criteria are as follows.
1: strong unpleasant taste 2: unpleasant taste 3: slightly unpleasant taste 4: little unpleasant taste 5: no unpleasant taste
実施例２０、比較例１５及び参考例１０
８０℃に加温した温水１００ｍＬに寒天を０．３ｇ添加し、１０分間温度を維持しながら攪拌子で攪拌して完全に溶解させた。次いで、表１１に示す残りの成分を全て加え、更に５分間攪拌して完全に溶解させてゼリー原液を調製した。次いで、得られたゼリー原液４０ｇを容器（スチロール樹脂製プラスチックカップ、容量：７０ｍＬ、取り出し口内径：５ｃｍ）に流し入れ、冷蔵庫で１０℃以下に冷却してゼリー食品を得た。得られたゼリー食品について分析及び官能評価を行った。
Example 20, Comparative Example 15, and Reference Example 10
0.3 g of agar was added to 100 mL of warm water heated to 80 ° C., and the mixture was stirred for 10 minutes with a stirrer to completely dissolve. Next, all of the remaining components shown in Table 11 were added, and further stirred for 5 minutes to completely dissolve, thereby preparing a jelly stock solution. Next, 40 g of the obtained jelly stock solution was poured into a container (plastic cup made of styrene resin, capacity: 70 mL, inner diameter of outlet: 5 cm), and cooled to 10 ° C. or lower in a refrigerator to obtain a jelly food. The obtained jelly food was analyzed and sensory evaluated.
官能評価４
上記の各実施例、比較例及び参考例で得られたゼリー食品を小さじのスプーンで３ｇすくい取った後、口腔内に含み、舌で唾液と混ぜて完全に消滅したときの「不快味」について、専門パネル４名が官能試験を行った。官能試験では、各パネリストが「不快味」の評価基準を、下記の評価基準とすることに合意したうえで実施した。そして、専門パネルの評点の平均値を求めた。なお、評点の平均値は、小数第２位を四捨五入するものとする。
Sensory evaluation 4
About "unpleasant taste" when the jelly food obtained in each of the above Examples, Comparative Examples and Reference Examples was scooped out with a spoon of 3 g with a teaspoon and then contained in the oral cavity and completely disappeared by mixing with saliva with the tongue. And four specialized panels performed a sensory test. The sensory test was performed after each panelist agreed that the evaluation criteria for “unpleasant taste” were the following evaluation criteria. Then, the average value of the scores of the specialized panels was obtained. The average score is rounded to the first decimal place.
不快味の評価基準
不快味は、摂取したときに不快味が感じられるか否かを観点に、比較例１５のゼリー食品の不快味の評点を「１」として評価した。具体的な評価基準は以下のとおりである。
１：不快味を強く感じる
２：不快味を感じる
３：不快味を少し感じる
４：不快味をほとんど感じない
５：不快味を感じない
Evaluation criteria of unpleasant taste The unpleasant taste was evaluated as “1” with the score of unpleasant taste of the jelly food of Comparative Example 15 from the viewpoint of whether or not unpleasant taste was felt when ingested. The specific evaluation criteria are as follows.
1: strong unpleasant taste 2: unpleasant taste 3: slightly unpleasant taste 4: little unpleasant taste 5: no unpleasant taste
表２〜１１から、特定量の（Ａ）デキストリンと（Ｂ）カフェインとを特定の量比で含有させたうえで、更に特定量の（Ｃ）ケンフェロールモノグルコシドを含有させることで、不快味の抑制された経口組成物が得られることがわかる。 From Tables 2 to 11, it is unpleasant that a specific amount of (A) dextrin and (B) caffeine are contained in a specific amount ratio, and further a specific amount of (C) kaempferol monoglucoside is further contained. It turns out that the oral composition with suppressed taste was obtained.
Claims (6)
（Ａ）デキストリン
（Ｂ）カフェイン、及び
（Ｃ）ケンフェロールモノグルコシド
を含有し、
固形分中の成分（Ａ）の含有量が１０質量％以上であり、
固形分中の成分（Ｃ）の含有量が０．０１〜１質量％であり、かつ、
成分（Ａ）と成分（Ｂ）との質量比[（Ｂ）／（Ａ）]が０．００１〜０．２である、
経口組成物。 The following components (A), (B) and (C);
(A) containing dextrin (B) caffeine, and (C) kaempferol monoglucoside,
The content of the component (A) in the solid content is 10% by mass or more;
The content of the component (C) in the solid content is 0.01 to 1% by mass, and
The mass ratio [(B) / (A)] between the component (A) and the component (B) is from 0.001 to 0.2.
Oral composition.
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