JP2020097536A - Oral product - Google Patents

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JP2020097536A
JP2020097536A JP2018236153A JP2018236153A JP2020097536A JP 2020097536 A JP2020097536 A JP 2020097536A JP 2018236153 A JP2018236153 A JP 2018236153A JP 2018236153 A JP2018236153 A JP 2018236153A JP 2020097536 A JP2020097536 A JP 2020097536A
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oral
powder composition
oral product
powder
component
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JP7127524B2 (en
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麻依子 松木
Maiko Matsuki
麻依子 松木
利一 牧
Toshikazu Maki
利一 牧
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Lion Corp
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Abstract

To provide an oral product that makes it possible to visually grasp a buffer ability of saliva, and resists color fading during its storage to show good temporal stability, and is suitable for inspection of a saliva buffer ability.SOLUTION: An oral product has a powder composition containing (A) anthocyanin dye powder and (B) an inorganic base that is solid at 5-40°C, the powder composition being charged into a moisture-proof container. The powder composition further has either one or both of (C) a humectant that is solid at 5-40°C and (D) a bactericidal antibacterial that is solid at 5-40°C.SELECTED DRAWING: None

Description

本発明は、唾液の緩衝能が視覚的に把握され、唾液緩衝能の検査用として好適な口腔用製品に関する。 TECHNICAL FIELD The present invention relates to a product for oral cavity, which is suitable for inspection of saliva buffering capacity, since the buffering capacity of saliva is visually grasped.

健康寿命の延伸が求められている昨今、口腔分野に関しても、虫歯、歯周病、口臭等の口腔内不具合が顕在化する前に、未然に防ぐ技術や製品は求められている。生活者に対して、自発的に口腔内の不具合に対する予防行為を促す一つの手段として、視覚等によるチェックによって自分の口腔内の健康状態を把握してもらうことが必要であると考えられるが、市場には日々の口腔内の健康状態を簡便かつ安価にチェックできる手段はほとんどなかった。
ところで、唾液には、アルカリや酸を口に含んだ際に口腔内を中性(pH7付近)に保つ緩衝作用があり、この緩衝作用が口腔内の健康状態に影響し、上記口腔内不具合の予防にも関与していると考えられ、生活者が自身の唾液力として唾液緩衝能を正しく把握することは、口腔内の健康状態を簡単に判断し、上記口腔内不具合を予防できる可能性が高いこともあり、的確かつ簡単な把握手段の開発が望まれた。
Nowadays, there is a demand for extension of healthy life expectancy, and also in the oral field, there is a demand for a technique and a product for preventing the occurrence of oral defects such as tooth decay, periodontal disease and bad breath before they become apparent. As a means to encourage consumers to voluntarily take preventive actions against problems in the oral cavity, it is thought that it is necessary to have them grasp the health condition of their oral cavity by visual check, etc. There were few means on the market to check daily oral health condition easily and inexpensively.
By the way, saliva has a buffering action for keeping the oral cavity neutral (around pH 7) when it contains an alkali or an acid, and this buffering action affects the oral health condition, and It is considered that it is also involved in prevention, and that the consumer correctly understands the saliva buffering ability as his saliva force, it is possible to easily judge the health condition in the oral cavity and prevent the above oral malfunctions. Since it is expensive, it was desired to develop an accurate and simple grasping method.

特許文献1(特表2015−500348号公報)は、固定化難溶性酸または塩基(例えば、難溶性酸または塩基を含有する固体粒子またはマトリックス)を含む第1成分および非活性液体、要すれば異なる非活性液体を含む第2成分、1以上の更なる成分を含有するオーラル・ケア、スキン・ケアまたはホーム・ケア組成物であって、貯蔵の間、非活性液体が固定化難溶性酸または塩基と接触しないが、使用時には非活性液体が固定化難溶性酸または塩基と接触して、溶液のpHが変化する組成物を提案し、非活性液体としてアントシアニンを記載している。特許文献2(特開2001−299298号公報)は、飲料に供する時点で果実等を添加してpHを低下させ、飲料に含まれるアントシアニン系色素の色調変化により飲料の色調を変化させた飲料を提案し、特許文献3(特開2012−219049号公報)は、アントシアニン系色素とシリカ系研磨剤等を含有し、使用時の色変化を実現した歯磨剤組成物を提案している。 Patent Document 1 (Japanese Patent Publication No. 2015-500348) discloses a first component containing an immobilized sparingly soluble acid or base (for example, solid particles or a matrix containing a sparingly soluble acid or base) and an inert liquid, if necessary. An oral care, skin care or home care composition containing a second component comprising a different inert liquid, one or more further components, wherein the inert liquid immobilizes a poorly soluble acid during storage. It proposes a composition that does not come into contact with a base, but when used, the inactive liquid comes into contact with the immobilized sparingly soluble acid or base to change the pH of the solution, and anthocyanin is described as the inactive liquid. Patent Document 2 (Japanese Patent Laid-Open No. 2001-299298) discloses a beverage in which a fruit or the like is added to a beverage to lower the pH and the color tone of the anthocyanin pigment contained in the beverage is changed to change the color tone of the beverage. Proposed, Patent Document 3 (JP 2012-219049A) proposes a dentifrice composition containing an anthocyanin dye and a silica-based abrasive, and realizing a color change during use.

特表2015−500348号公報Japanese Patent Publication No. 2015-500348 特開2001−299298号公報JP, 2001-299298, A 特開2012−219049号公報JP 2012-219049 A

本発明は、上記事情に鑑みなされたもので、唾液の緩衝能を視覚的に明確かつ簡単に把握でき、唾液緩衝能の検査用として好適な口腔用製品を提供することを目的とする。 The present invention has been made in view of the above circumstances, and an object of the present invention is to provide an oral product that can visually and clearly grasp the saliva buffering capacity and is suitable for testing the saliva buffering capacity.

本発明者らは上記目的を達成するため鋭意検討を行った結果、(A)アントシアニン系色素粉末と、(B)5〜40℃で固体の無機塩基とを含有する粉体組成物が、防湿容器に充填された口腔用製品によって、上記課題、目的を達成できることを知見した。即ち、本発明では、上記口腔用製品が、特に使用時に上記防湿容器から取り出した粉体組成物を、水に溶解して液体製剤として使用し、この液体製剤で洗口するなどして口腔内に適用すると、製剤の色変化から唾液の緩衝作用の強さを判別して唾液緩衝能を視覚的に明確かつ簡単に把握することができ、また、製品の保存時には上記粉体組成物の退色を経時でも抑えて経時安定性を与えることもできること、よって、個人の唾液緩衝能の検査に応用可能であることを知見し、本発明をなすに至った。 As a result of earnest studies to achieve the above object, the present inventors have found that a powder composition containing (A) anthocyanin pigment powder and (B) a solid inorganic base at 5 to 40° C. is moisture-proof. It was found that the above-mentioned problems and objects can be achieved by the oral cavity product filled in the container. That is, in the present invention, the oral product, in particular, the powder composition taken out from the moisture-proof container at the time of use is dissolved in water to be used as a liquid preparation, and the oral preparation is rinsed with the liquid preparation. When applied to, the saliva buffering ability can be visually clearly and easily grasped by distinguishing the strength of the saliva buffering effect from the color change of the preparation, and the fading of the powder composition above can be observed when the product is stored. The present invention has been completed on the basis of the finding that it is possible to provide stability over time by suppressing the above, and thus it can be applied to the test of saliva buffering capacity of an individual.

フラボノイド系の色素の中でもアントシアニン系色素は、食品添加物として公知でpHによる色調変化が顕著であることも知られているが、安定化が難しく、光、熱等に弱いだけでなく、pHによっても速やかに分解し、退色してしまうこともあった。しかし、本発明では、(A)成分に(B)成分を粉末状態で併用した粉体組成物を防湿容器に充填し、使用時には上記容器から取り出し、水に溶解して液体製剤等として使用することで、(A)成分が適度に安定化し、(A)成分による色の変化度合いによって口腔内の唾液緩衝能を判別する作用を向上でき、これにより、唾液緩衝能を視覚的に分かり易く判別できる優れた判別性を有し、また、保存時には退色が抑制されて経時安定性もよい口腔用製品を得ることができた。この場合、特に好ましくは(A)及び(B)成分の量比を示す(A)/(B)が質量比として特定範囲であり、更には液体製剤のpHが特定範囲であると、唾液緩衝能の判別が一層分かり易く、より優れた作用効果を付与できた。
本発明の作用効果は、(A)及び(B)成分の併用によって特異的に得られ、(A)又は(B)成分を欠くと劣り、また、(A)及び(B)成分が併用されていても、不適切な容器に充填された場合は劣るものであった。後述の比較例に示すように、(A)成分又は(B)成分を欠くと唾液緩衝能の分かり易さが劣った(比較例1〜3、5〜7)。なお、(A)成分を欠く場合は、(A)成分と同様にフラボノイド系の色素であるウコン色素のクルクミンや、(A)成分と同様にポリフェノール類であるコチニール色素のカルミン酸を含み、水溶液pHが適切であっても、唾液緩衝能の分かり易さが劣り(比較例2、3)、(B)成分を欠く場合は、塩基であるモノエタノールアミン(液体の有機塩基)や水酸化ナトリウム水溶液(液体の無機塩基)を含み、水溶液pHが適切であっても、唾液緩衝能の分かり易さが劣った(比較例5、6、7)。また、(A)、(B)成分が併用されていても、充填容器が非防湿の場合は、唾液緩衝能の分かり易さが劣った(比較例4)。これに対して、実施例に示す本発明の口腔用製品は、唾液緩衝能の分かり易さが優れ、また、経時安定性(退色のなさ)も良かった。
Among the flavonoid pigments, the anthocyanin pigment is known as a food additive and is also known to have a remarkable change in color tone due to pH, but it is difficult to stabilize and is not only weak against light and heat, but also depending on the pH. It also decomposed quickly and sometimes faded. However, in the present invention, the powder composition in which the component (A) and the component (B) are used together in a powder state is filled in a moisture-proof container, taken out from the container at the time of use, and dissolved in water to be used as a liquid preparation or the like. As a result, the component (A) is moderately stabilized, and the effect of distinguishing the saliva buffering capacity in the oral cavity can be improved by the degree of color change due to the component (A), and thus the saliva buffering capacity can be visually recognized easily. It was possible to obtain an oral product which has excellent discriminating ability and which is suppressed in fading during storage and has good stability over time. In this case, it is particularly preferable that (A)/(B), which represents the amount ratio of the components (A) and (B), be in a specific range as a mass ratio, and further that the pH of the liquid preparation be in a specific range. It was possible to more easily understand the discrimination of Noh, and it was possible to give more excellent effects.
The effect of the present invention is specifically obtained by the combined use of the components (A) and (B), and is poor when the component (A) or (B) is lacking, and the components (A) and (B) are used in combination. However, it was inferior when filled in an inappropriate container. As shown in Comparative Examples described later, when the component (A) or the component (B) was lacking, the saliva buffering ability was poorly understood (Comparative Examples 1 to 3 and 5 to 7). When the component (A) is lacking, curcumin, which is a turmeric pigment that is a flavonoid-based pigment as in the component (A), and carminic acid, which is a cotinyl pigment that is a polyphenol as in the component (A), are used, Even if the pH is appropriate, the saliva buffering ability is poorly understood (Comparative Examples 2 and 3), and when the component (B) is lacking, monoethanolamine (liquid organic base) or sodium hydroxide, which is a base, is used. Even if the pH of the aqueous solution was appropriate, including the aqueous solution (liquid inorganic base), the saliva buffering ability was inferior (Comparative Examples 5, 6, and 7). In addition, even if the components (A) and (B) were used in combination, the saliva buffering ability was poorly understood when the filling container was non-moisture proof (Comparative Example 4). On the other hand, the oral products of the present invention shown in the Examples were excellent in the saliva buffering ability, and were stable in time (no discoloration).

本発明では、上記粉体組成物に、更に、(C)5〜40℃で固体の湿潤剤を配合することで、口腔内保湿効果を付与でき、また更に、(D)5〜40℃で固体の殺菌抗菌剤を配合することで、口臭抑制効果を付与することもでき、これらによって、口腔内のケアを同時に行うことも可能である。 In the present invention, an oral moisturizing effect can be imparted to the powder composition by further adding (C) a solid wetting agent at 5 to 40°C, and further (D) at 5 to 40°C. By incorporating a solid bactericidal antibacterial agent, it is possible to impart a breath odor suppressing effect, and by these, it is possible to simultaneously perform oral care.

従って、本発明は、下記の口腔用製品を提供する。
〔1〕
(A)アントシアニン系色素粉末、及び
(B)5〜40℃で固体の無機塩基
を含有する粉体組成物が、防湿容器に充填された口腔用製品。
〔2〕
(B)5〜40℃で固体の無機塩基が、炭酸ナトリウム、炭酸カリウム、炭酸水素ナトリウム、炭酸水素カリウム、リン酸2水素ナトリウム、リン酸水素2ナトリウム、水酸化ナトリウム、水酸化カリウム及び水酸化リチウムから選ばれる1種以上の無機塩基粉末である〔1〕に記載の口腔用製品。
〔3〕
(B)5〜40℃で固体の無機塩基が、炭酸ナトリウム、炭酸カリウム、水酸化ナトリウム及び水酸化カリウムから選ばれる〔2〕に記載の口腔用製品。
〔4〕
(A)/(B)が質量比として0.01〜12.5である〔1〕〜〔3〕のいずれかに記載の口腔用製品。
〔5〕
粉体組成物が、更に、(C)5〜40℃で固体の湿潤剤を含有する〔1〕〜〔4〕のいずれかに記載の口腔用製品。
〔6〕
粉体組成物が、更に、(D)5〜40℃で固体の殺菌抗菌剤を含有する〔1〕〜〔5〕のいずれかに記載の口腔用製品。
〔7〕
防湿容器が、アルミニウム蒸着が施された防湿フイルムで形成された密封可能な容器又は乾燥剤が内包された密封可能な合成樹脂製容器である〔1〕〜〔6〕のいずれかに記載の口腔用製品。
〔8〕
使用時に防湿容器から取り出した粉体組成物を水に溶解して液体製剤として使用される〔1〕〜〔7〕のいずれかに記載の口腔用製品。
〔9〕
液体製剤の25℃におけるpHが8〜10である〔8〕に記載の口腔用製品。
〔10〕
液体製剤が洗口剤である〔8〕又は〔9〕に記載の口腔用製品。
〔11〕
唾液緩衝能の検査用である〔1〕〜〔10〕のいずれかに記載の口腔用製品。
Therefore, the present invention provides the following oral products.
[1]
An oral product in which a moisture-proof container is filled with a powder composition containing (A) anthocyanin-based pigment powder and (B) a solid inorganic base at 5 to 40°C.
[2]
(B) The solid inorganic base at 5 to 40° C. is sodium carbonate, potassium carbonate, sodium hydrogencarbonate, potassium hydrogencarbonate, sodium dihydrogenphosphate, disodium hydrogenphosphate, sodium hydroxide, potassium hydroxide and hydroxylation. The oral product according to [1], which is one or more inorganic base powders selected from lithium.
[3]
(B) The oral product according to [2], wherein the inorganic base solid at 5 to 40° C. is selected from sodium carbonate, potassium carbonate, sodium hydroxide and potassium hydroxide.
[4]
(A)/(B) is 0.01-12.5 as a mass ratio, The product for oral cavity in any one of [1]-[3].
[5]
The oral product according to any one of [1] to [4], wherein the powder composition further contains (C) a wetting agent that is solid at 5 to 40°C.
[6]
The oral product according to any one of [1] to [5], wherein the powder composition further contains (D) a bactericidal antibacterial agent which is solid at 5 to 40°C.
[7]
The oral cavity according to any one of [1] to [6], wherein the moisture-proof container is a sealable container formed of a moisture-proof film having aluminum vapor deposition or a sealable synthetic resin container containing a desiccant. For products.
[8]
The oral product according to any one of [1] to [7], which is used as a liquid preparation by dissolving the powder composition taken out from the moisture-proof container at the time of use in water.
[9]
The oral product according to [8], wherein the liquid formulation has a pH of 8 to 10 at 25°C.
[10]
The oral product according to [8] or [9], wherein the liquid preparation is a mouthwash.
[11]
The oral product according to any one of [1] to [10], which is for testing saliva buffering capacity.

本発明によれば、唾液の緩衝能を視覚的に把握でき、また、保存時には退色が抑制されて経時安定性も良く、唾液緩衝能の検査用として好適な口腔用製品を提供できる。この口腔用製品は、唾液緩衝能を明確かつ簡単に把握でき、更に、優れた口腔内保湿効果、口臭抑制効果を与えることも可能であり、唾液緩衝能のチェック及び口腔ケア一体型の製品として使用することもできる。 ADVANTAGE OF THE INVENTION According to this invention, the buffering ability of saliva can be grasped|ascertained visually, fading is suppressed at the time of storage, stability over time is also good, and the oral cavity product suitable for a test|inspection of saliva buffering ability can be provided. This oral product can clearly and easily grasp the saliva buffering capacity, and can also give an excellent oral moisturizing effect and bad breath control effect. It can also be used.

以下、本発明につき更に詳述する。本発明の口腔用製品は、(A)アントシアニン系色素粉末、及び(B)5〜40℃で固体の無機塩基を含有する粉体組成物が、防湿容器に充填されたものである。この口腔用製品は、唾液緩衝能の検査用として好適である。 Hereinafter, the present invention will be described in more detail. The oral cavity product of the present invention is obtained by filling a moisture-proof container with (A) anthocyanin-based pigment powder and (B) a powder composition containing a solid inorganic base at 5 to 40°C. This oral product is suitable for testing saliva buffering capacity.

(A)アントシアニン系色素は、花・果実・葉等植物界において広く存在する水溶性の色素の総称であり、赤、紫、青等の色を呈する。アントシアニジンがアグリコンとして糖や糖鎖と結びついた配糖体の形で存在する。シソ、ハツカダイコン、赤キャベツ、赤カブ、紫イモ等に多く含まれる。アントシアニン系色素は、食品添加物として公知であり、特にpH6〜10で色調が変化し、一般的には酸性で赤色、アルカリ性で青色を呈する性質を有している。 The (A) anthocyanin pigment is a general term for water-soluble pigments widely existing in the plant kingdom such as flowers, fruits, and leaves, and exhibits colors such as red, purple, and blue. Anthocyanidins exist as aglycones in the form of glycosides linked to sugars and sugar chains. It is abundant in perilla, radish, red cabbage, red turnip, purple potato, etc. Anthocyanin dyes are known as food additives, and in particular, the color tone changes at pH 6 to 10, and generally has the property of exhibiting red color when acidic and blue color when alkaline.

(A)アントシアニン系色素は市販品を使用でき、これを含む色素を用いてもよい。具体的には、食品添加物として汎用されている商品である、三栄源エフ・エフ・アイ株式会社製のサンレッドYM(紫イモ色素43質量%/クエン酸(結晶)7質量%/デキストリン50質量%)や、サンレッドRCU(赤キャベツ色素36質量%/クエン酸(結晶)4質量%/粉末水飴60質量%)等の製品が好ましい。
なお、(A)成分に代えて、アントシアニン系色素と同様にフラボノイド系であってもウコン色素のクルクミンを使用した場合、あるいはアントシアニン系色素と同様にポリフェノール類であってもコチニール色素のカルミン酸を使用した場合、あるいはラック色素を使用した場合は、pH6〜10における色変化が不明瞭で、唾液緩衝能を判断することができず把握できない(後述の比較例2、3参照)
As the (A) anthocyanin dye, a commercially available product may be used, and a dye containing this may be used. Specifically, San Red YM (purple potato dye 43 mass%/citric acid (crystal) 7 mass%/dextrin 50) manufactured by San-Ei Gen FFI Co., Ltd., which is a widely used food additive. %) and Sun Red RCU (red cabbage pigment 36% by mass/citric acid (crystal) 4% by mass/powdered starch syrup 60% by mass) and the like are preferable.
Incidentally, instead of the component (A), when curcumin, which is a turmeric dye even if it is a flavonoid system like an anthocyanin dye, is used, or when carminic acid is a cotinyl dye, even when it is a polyphenol like an anthocyanin dye. When it is used or when the rack dye is used, the color change at pH 6 to 10 is unclear, and the saliva buffering capacity cannot be determined and cannot be grasped (see Comparative Examples 2 and 3 described later).

(A)成分の配合量は、粉体組成物全体の0.06〜41.6%(質量%、以下同様)が好ましく、より好ましくは0.13〜39.5%である。
更に、粉体組成物が(A)及び(B)成分を含み、(C)及び(D)成分を含まない場合、(A)成分の配合量は、粉体組成物全体の1.0〜41.6%、特に18.0〜39.5%が好ましい。また、粉体組成物が(A)、(B)及び(C)成分、更には(D)成分を含む場合、(A)成分の配合量は、粉体組成物全体の0.06〜2.5%、特に0.13〜0.65%が好ましい。
(A)成分の配合量が上記範囲内であると、色変化が明瞭で唾液緩衝能の判別性が十分に優れる。
The blending amount of the component (A) is preferably 0.06 to 41.6% (mass %, the same applies below) of the entire powder composition, and more preferably 0.13 to 39.5%.
Further, when the powder composition contains the components (A) and (B) and does not contain the components (C) and (D), the amount of the component (A) to be added is 1.0 to 10% of the total amount of the powder composition. 41.6%, especially 18.0 to 39.5% is preferable. Further, when the powder composition contains the components (A), (B) and (C), and further the component (D), the blending amount of the component (A) is 0.06 to 2 of the entire powder composition. 0.5%, particularly 0.13 to 0.65% is preferable.
When the blending amount of the component (A) is within the above range, the color change is clear and the saliva buffering ability is sufficiently distinguished.

また、(A)成分の使用量は、粉体組成物を20mLの水に溶かして使用する場合、好ましくは0.2〜20mg、特に1〜10mg、とりわけ1.0〜5.0mgであり、これを満たす範囲内で粉体組成物中への(A)成分の配合量を設定することが望ましい。上記範囲内であると、色変化が明瞭で唾液緩衝能がより判別し易く、また、十分な経時安定性が得られる。 When the powder composition is used by dissolving it in 20 mL of water, the amount of the component (A) is preferably 0.2 to 20 mg, particularly 1 to 10 mg, and especially 1.0 to 5.0 mg. It is desirable to set the blending amount of the component (A) in the powder composition within the range that satisfies this. Within the above range, the color change is clear, the saliva buffering capacity is more easily discriminated, and sufficient temporal stability is obtained.

(B)成分は、5〜40℃で固体の無機塩基である。本発明では、(B)成分によって、(A)成分による唾液緩衝能を判別する作用が改善する。また、(B)成分は、粉体組成物を水に溶解後の液体製剤のpHを調整する作用を有する。(B)成分に代えて、不適切な塩基、例えば有機塩基や5〜40℃で液体の無機塩基等を使用すると、粉体組成物を水に溶解後の水溶液pHが適切であっても、唾液緩衝能を満足に判別できず、また、粉体組成物の経時安定性(退色のなさ)が悪くなり、本発明の作用効果が得られない。 The component (B) is a solid inorganic base at 5 to 40°C. In the present invention, the component (B) improves the action of discriminating the saliva buffering ability of the component (A). Further, the component (B) has a function of adjusting the pH of the liquid preparation after the powder composition is dissolved in water. If an inappropriate base such as an organic base or an inorganic base that is liquid at 5 to 40° C. is used instead of the component (B), even if the pH of the aqueous solution after dissolving the powder composition in water is appropriate, The saliva buffering capacity cannot be satisfactorily discriminated, and the temporal stability (no discoloration) of the powder composition deteriorates, so that the effects of the present invention cannot be obtained.

(B)5〜40℃で固体の無機塩基は、炭酸又はリン酸のアルカリ金属塩(水素塩でもよい)、アルカリ金属の水酸化物を用いることができ、アルカリ金属はナトリウム、カリウム、ナトリウム等である。特に炭酸のアルカリ金属塩、アルカリ金属の水酸化物が好ましく、炭酸のアルカリ金属塩がより好ましい。
(B)成分は、例えば炭酸ナトリウム、炭酸カリウム、炭酸水素ナトリウム、炭酸水素カリウム、リン酸2水素ナトリウム、リン酸水素2ナトリウム、水酸化ナトリウム、水酸化カリウム、水酸化リチウム等が挙げられ、これらから選ばれる1種又は2種以上の無機塩基粉末を使用できる。これらの中でも、粉末として均一に混合が可能で、色調変化による唾液緩衝能の分かり易いpH8〜10(25℃)まで上げることができる点で、炭酸ナトリウム、炭酸カリウム、炭酸水素ナトリウム、水酸化ナトリウム、水酸化カリウムが好ましく、特に、少量で最も色調変化による唾液緩衝能の分かり易いpH8.5〜10(25℃)まで上げることができる観点から、炭酸ナトリウム、炭酸カリウム、水酸化ナトリウム、水酸化カリウムがより好ましい。とりわけ、潮解性の低さの観点から炭酸ナトリウムが好ましい。
(B) As the inorganic base which is solid at 5 to 40° C., an alkali metal salt of carbonic acid or phosphoric acid (or a hydrogen salt may be used) or an alkali metal hydroxide may be used, and the alkali metal is sodium, potassium, sodium or the like. Is. Particularly, an alkali metal salt of carbonic acid and a hydroxide of alkali metal are preferable, and an alkali metal salt of carbonic acid is more preferable.
Examples of the component (B) include sodium carbonate, potassium carbonate, sodium hydrogen carbonate, potassium hydrogen carbonate, sodium dihydrogen phosphate, disodium hydrogen phosphate, sodium hydroxide, potassium hydroxide, lithium hydroxide, and the like. One or more inorganic base powders selected from the above can be used. Among these, sodium carbonate, potassium carbonate, sodium hydrogen carbonate, sodium hydroxide can be uniformly mixed as a powder, and can be raised to pH 8 to 10 (25° C.) where the saliva buffering ability due to color tone change is easy to understand. , Potassium hydroxide is preferable, and especially sodium carbonate, potassium carbonate, sodium hydroxide, and hydroxide can be raised from the viewpoint that the saliva buffering capacity due to the change in color tone can be easily raised to pH 8.5 to 10 (25° C.). More preferred is potassium. Especially, sodium carbonate is preferable from the viewpoint of low deliquescent property.

(B)成分の配合量は、(A)成分の配合量に応じて調整することが好ましく、特に両成分の量比が適切になる範囲内であることがより好ましい。(B)成分の配合量は、粉体組成物全体の0.04〜97.8%が好ましく、より好ましくは0.08〜58%である。
更に、粉体組成物が(A)及び(B)成分を含み、(C)及び(D)成分を含まない場合、(B)成分の配合量は、粉体組成物全体の3.3〜97.8%、特に9.0〜58.0%が好ましい。また、粉体組成物が(A)及び(B)成分に加えて、(C)成分、更には(D)成分を含む場合、(B)成分の配合量は、粉体組成物全体の0.04〜1.5%、特に0.08〜0.4%が好ましい。
(B)成分の配合量が上記範囲内であると、唾液緩衝能を十分に分かり易く判別できる。
The blending amount of the component (B) is preferably adjusted according to the blending amount of the component (A), and particularly preferably within the range where the ratio of the amounts of the two components is appropriate. The content of the component (B) is preferably 0.04 to 97.8%, and more preferably 0.08 to 58% of the total powder composition.
Furthermore, when the powder composition contains the components (A) and (B) and does not contain the components (C) and (D), the blending amount of the component (B) is 3.3 to 10% of the total amount of the powder composition. 97.8%, particularly 9.0 to 58.0% is preferable. When the powder composition contains the components (C) and (D) in addition to the components (A) and (B), the content of the component (B) is 0 in the whole powder composition. 0.04 to 1.5%, especially 0.08 to 0.4% is preferable.
When the blending amount of the component (B) is within the above range, the saliva buffering capacity can be determined sufficiently easily.

また、(B)成分の使用量は、粉体組成物を20mLの水に溶かして使用する際、好ましくは0.2〜200mg、特に0.4〜80mgであり、これを満たす範囲内で粉体組成物中への(B)成分の配合量を設定することが望ましい。上記範囲内であると、色変化が明瞭で唾液緩衝能がより判別し易く、また、十分な経時安定性が得られる。
更に、(B)成分として炭酸ナトリウム、炭酸カリウム、水酸化ナトリウム、水酸化リチウム及び水酸化カリウムから選ばれる無機塩基を用いる場合、これらの使用量は、粉体組成物を20mLの水に溶かして使用する際、0.2〜4.0mgが好ましく、0.4〜2.0mgがより好ましい。この範囲内であると、唾液緩衝能を十分に分かり易く判別できる。使用量が0.2mg未満又は4.0mgを超えると、水に溶解した際に目的とするpH領域の水溶液が得られず唾液緩衝能が判別できない場合がある。
また、(B)成分として水素塩である炭酸水素ナトリウム、炭酸水素カリウム、リン酸2水素ナトリウム、リン酸水素2ナトリウムから選ばれる無機塩基を用いる場合、これらの使用量は、粉体組成物を20mLの水に溶かして使用する際、20〜200mgが好ましく、40〜80mgがより好ましい。この範囲内であると、唾液緩衝能を十分に分かり易く判別できる。使用量が20mg未満では、水に溶解した際に目的とするpH領域の水溶液が得られず唾液緩衝能が判別できない場合があり、200mgを超えると、水への溶解性が劣る場合がある。
In addition, the amount of the component (B) used is preferably 0.2 to 200 mg, particularly 0.4 to 80 mg when the powder composition is dissolved in 20 mL of water and used. It is desirable to set the blending amount of the component (B) in the body composition. Within the above range, the color change is clear, the saliva buffering capacity is more easily discriminated, and sufficient temporal stability is obtained.
Furthermore, when an inorganic base selected from sodium carbonate, potassium carbonate, sodium hydroxide, lithium hydroxide and potassium hydroxide is used as the component (B), these are used in such amounts that the powder composition is dissolved in 20 mL of water. When used, it is preferably 0.2 to 4.0 mg, more preferably 0.4 to 2.0 mg. Within this range, the saliva buffering capacity can be discriminated sufficiently easily. If the amount used is less than 0.2 mg or more than 4.0 mg, an aqueous solution having a desired pH range cannot be obtained when dissolved in water, and the saliva buffering capacity may not be determined.
When an inorganic base selected from hydrogen salts such as sodium hydrogencarbonate, potassium hydrogencarbonate, sodium dihydrogenphosphate, and disodium hydrogenphosphate is used as the component (B), the amount of these used depends on the powder composition. When used by dissolving in 20 mL of water, 20 to 200 mg is preferable, and 40 to 80 mg is more preferable. Within this range, the saliva buffering capacity can be discriminated sufficiently easily. If the amount used is less than 20 mg, an aqueous solution having a desired pH range may not be obtained when dissolved in water, and the saliva buffering capacity may not be discriminated. If it exceeds 200 mg, solubility in water may be poor.

本発明において、(A)成分と(B)成分との量比を示す(A)/(B)は、特に唾液緩衝能の判別し易さの点から、質量比として0.01〜12.5が好ましく、より好ましくは0.31〜4.33である。上記範囲内であると、唾液緩衝能の分かり易さがより優れる。 In the present invention, (A)/(B), which indicates the amount ratio of the component (A) and the component (B), is 0.01 to 12. as a mass ratio, particularly from the viewpoint of easy discrimination of saliva buffering capacity. 5 is preferable, and 0.31 to 4.33 is more preferable. Within the above range, the saliva buffering ability is more easily understood.

本発明では、粉体組成物に(A)及び(B)成分に加えて、更に(C)5〜40℃で固体の湿潤剤を配合することが好ましい。(C)成分を添加すると、優れた口腔内保湿効果を付与することができる。 In the present invention, in addition to the components (A) and (B), the powder composition preferably further comprises (C) a solid wetting agent at 5 to 40°C. By adding the component (C), an excellent effect of moisturizing in the oral cavity can be imparted.

(C)5〜40℃で固体の湿潤剤は、例えばソルビトール、トレハロース、キシリトール、マルチトール、ラクチトール、エリスリトール等の糖アルコールの1種又は2種以上を用いることができ、これらの粉末が好ましい。中でも、溶解性の観点から、ソルビトール、キシリトール、トレハロースが好ましく、ソルビトール、キシリトールがより好ましい。 As the wetting agent (C) solid at 5 to 40° C., one or more sugar alcohols such as sorbitol, trehalose, xylitol, maltitol, lactitol, and erythritol can be used, and powders thereof are preferable. Of these, sorbitol, xylitol, and trehalose are preferable, and sorbitol and xylitol are more preferable, from the viewpoint of solubility.

(C)成分は、市販品を用いることができる。具体的には、ソルビット(D−ソルビトール、LTS−P G−3、三菱商事フードテック株式会社製)、トレハロース(林原株式会社製)、キシリトール(キシリット粉末、三菱商事フードテック株式会社製)等を使用できる。 As the component (C), a commercially available product can be used. Specifically, sorbit (D-sorbitol, LTS-PG-3, manufactured by Mitsubishi Corporation Foodtech Co., Ltd.), trehalose (manufactured by Hayashibara Corporation), xylitol (xylitol powder, manufactured by Mitsubishi Corporation Foodtech Co., Ltd.), etc. Can be used.

(C)成分を配合する場合、その配合量は、粉体組成物全体の90.0〜99.81%が好ましい。
更に、(C)成分を配合し、(D)成分を含まない場合、(C)成分の配合量は、粉体組成物全体の93.0〜99.81%が好ましく、より好ましくは95.7〜99.5%が好ましい。また、(D)成分を含む場合、(C)成分の配合量は、粉体組成物全体の92.7〜98.7%が好ましく、より好ましくは96.7〜98.6%である。
(C)成分の配合量が上記範囲内であると、十分な保湿効果を付与できる。
When the component (C) is blended, its blending amount is preferably 90.0 to 99.81% of the entire powder composition.
Furthermore, when the component (C) is blended and the component (D) is not included, the blending amount of the component (C) is preferably 93.0 to 99.81% of the entire powder composition, and more preferably 95. 7-99.5% is preferable. When the component (D) is included, the content of the component (C) is preferably 92.7 to 98.7%, and more preferably 96.7 to 98.6% of the entire powder composition.
When the blending amount of the component (C) is within the above range, a sufficient moisturizing effect can be imparted.

(C)成分の使用量は、粉体組成物を20mLの水に溶かして使用する際、好ましくは100〜4,000mg、特に500〜4,000mg、とりわけ500〜2,000mgであり、これを満たす範囲内で粉体組成物中への(C)成分の配合量を設定することが望ましい。上記範囲内であると、十分な保湿効果が得られる。前記含有量が100mg以上であると、唾液緩衝能の判別性がより向上し、保湿効果が十分に得られる。4,000mg以下であると、水への溶解性を十分に確保できる。 The amount of the component (C) used is preferably 100 to 4,000 mg, particularly 500 to 4,000 mg, and especially 500 to 2,000 mg when the powder composition is used by dissolving it in 20 mL of water. It is desirable to set the blending amount of the component (C) in the powder composition within the range that satisfies the above conditions. Within the above range, a sufficient moisturizing effect can be obtained. When the content is 100 mg or more, the discriminability of the saliva buffering capacity is further improved, and the moisturizing effect is sufficiently obtained. When it is 4,000 mg or less, the solubility in water can be sufficiently ensured.

本発明では、粉体組成物に、更に(D)5〜40℃で固体の殺菌抗菌剤を配合できる。(D)成分を添加すると、優れた口臭抑制効果を付与することもできる。
(D)5〜40℃で固体の殺菌抗菌剤は、口腔用として公知の殺菌剤、抗菌剤を使用できる。例えば、塩化セチルピリジニウム、塩化ベンザルコニウム、塩化ベンゼトニウム、塩酸クロルヘキシジン、塩化ベルベリン等のカチオン性殺菌剤、塩酸アルキルジアミノエチルグリシン等の両性殺菌抗菌剤や、グルコン酸銅、銅クロロフィリンナトリウム、硫酸銅、塩化亜鉛、クエン酸亜鉛等の殺菌抗菌作用を有する水溶性の銅化合物、亜鉛化合物が挙げられ、これらから選ばれる1種又は2種以上を使用でき、これらの粉末が好ましい。これらの中でも、少量で殺菌抗菌効果の高い塩化セチルピリジニウム、塩化ベンザルコニウム、塩化ベンゼトニウムが好ましい。
In the present invention, a solid germicidal antibacterial agent (D) at 5 to 40°C can be further added to the powder composition. By adding the component (D), it is possible to impart an excellent effect of suppressing bad breath.
As the sterilizing and antibacterial agent (D) solid at 5 to 40°C, known bactericidal agents and antibacterial agents for oral cavity can be used. For example, cetylpyridinium chloride, benzalkonium chloride, benzethonium chloride, chlorhexidine hydrochloride, cationic fungicides such as berberine chloride, amphoteric fungicides such as alkyldiaminoethylglycine hydrochloride, copper gluconate, sodium copper chlorophyllin, copper sulfate, Examples thereof include water-soluble copper compounds and zinc compounds having a germicidal antibacterial action such as zinc chloride and zinc citrate, and one or more selected from these can be used, and powders thereof are preferable. Among these, cetylpyridinium chloride, benzalkonium chloride, and benzethonium chloride, which have a small amount and have a high bactericidal and antibacterial effect, are preferable.

(D)成分を配合する場合、その配合量は、粉体組成物全体の0.19〜1.23%が好ましく、より好ましくは0.20〜1.0%である。上記範囲内であると、十分な口臭抑制効果を付与できる。 When the component (D) is blended, the blending amount thereof is preferably 0.19 to 1.23%, and more preferably 0.20 to 1.0%, based on the entire powder composition. Within the above range, a sufficient bad breath suppressing effect can be imparted.

(D)成分の使用量は、粉体組成物を20mLの水に溶かして使用する際、好ましくは0.2〜50mg、特に1.0〜50mg、とりわけ1.5〜20mgであり、これを満たす範囲内で粉体組成物中への(D)成分の配合量を設定することが望ましい。上記範囲内であると、十分な口臭抑制効果が得られる。前記使用量が0.2mg以上であると、十分な口臭抑制効果が得られ、50mg以下であると、水への溶解性を十分に確保できる。 The amount of component (D) used is preferably 0.2 to 50 mg, particularly 1.0 to 50 mg, and especially 1.5 to 20 mg when the powder composition is used by dissolving it in 20 mL of water. It is desirable to set the blending amount of the component (D) in the powder composition within the range that satisfies the condition. Within the above range, a sufficient bad breath suppressing effect can be obtained. When the amount used is 0.2 mg or more, a sufficient breath odor suppressing effect can be obtained, and when the amount is 50 mg or less, sufficient solubility in water can be secured.

本発明において、粉体組成物の総量は、粉体組成物を水20mLに溶かして使用する際、上記各成分の使用量を合計した量の範囲内とすることができる。
(A)及び(B)成分の合計量は、粉体組成物を水20mLに溶かして使用する際、好ましくは0.4〜400mgの範囲である。
(A)及び(B)成分に加えて(C)成分を配合する場合、これらの合計量は、粉体組成物を水20mLに溶かして使用する際、好ましくは100.4〜4,220mgの範囲である。
(A)及び(B)成分に加えて(C)及び(D)成分を配合する場合、これらの合計量は、粉体組成物を水20mLに溶かして使用する際、好ましくは100.6〜4,270mgの範囲である。
In the present invention, the total amount of the powder composition can be within the range of the total amount of the components used when the powder composition is dissolved in 20 mL of water and used.
The total amount of components (A) and (B) is preferably in the range of 0.4 to 400 mg when the powder composition is used by dissolving it in 20 mL of water.
When the component (C) is blended in addition to the components (A) and (B), the total amount thereof is preferably 100.4 to 4,220 mg when the powder composition is dissolved in 20 mL of water before use. It is a range.
When the components (C) and (D) are blended in addition to the components (A) and (B), the total amount thereof is preferably 100.6 to 10 when the powder composition is used by dissolving it in 20 mL of water. It is in the range of 4,270 mg.

本発明にかかわる粉体組成物には、本発明の効果を損なわない範囲で、上記成分以外にも口腔用として使用し得る公知成分を配合できる。例えば、デンプン、カラギナン、ジェランガム、キサンタンガム等の天然高分子物質、口腔内組成物に使用可能なカルボキシメチルセルロースナトリウム、ヒドロキシプロピルメチルセルロース等の合成高分子物質、デキストリン等の多糖類、エキス類、香料が挙げられ、これらは1種単独で又は2種以上を組み合わせて使用し得る。
なお、防湿容器に充填する粉体組成物の総量は、唾液緩衝能の判別し易さ及び経時安定性の点から、100〜4,200mgが好ましく、500〜2,100mgがより好ましい。
In the powder composition according to the present invention, known components that can be used for the oral cavity can be added in addition to the above components within a range that does not impair the effects of the present invention. For example, starch, carrageenan, gellan gum, natural polymeric substances such as xanthan gum, sodium carboxymethyl cellulose usable for oral composition, synthetic polymeric substances such as hydroxypropylmethyl cellulose, polysaccharides such as dextrin, extracts, and fragrances. These may be used alone or in combination of two or more.
The total amount of the powder composition to be filled in the moisture-proof container is preferably 100 to 4,200 mg, more preferably 500 to 2,100 mg, from the viewpoint of easy determination of saliva buffering capacity and stability over time.

本発明にかかわる粉体組成物を充填、封入する防湿容器は、防湿性があれば特に限定されないが、アルミニウム蒸着が少なくとも容器内層に施されたフイルム等の防湿フイルムで形成された密封可能なフイルム状容器や、シリカゲル、アルミナゲル等の乾燥剤が内包された密封可能な合成樹脂(例えばポリエチレン、ポリプロピレン等)製の袋状容器が好ましい。この乾燥剤が内包された容器に粉体組成物を充填する場合は、上記乾燥剤と共に収容し、梱包することが望ましい。これらのような防湿容器を用いることで、(A)成分による粉体組成物の退色を経時においても十分に防止して安定化でき、しかも、唾液緩衝能の判別性を改善することができる。中でも、粉体組成物の経時安定性(退色のなさ)及び製造性の観点から、上記防湿フイルムで形成された密封可能なフイルム状容器が好ましい。なお、防湿容器は粉体組成物を充填後に、シーラー等を用いて密封包装することが好ましい。
防湿容器は市販品を使用でき、例えば、防湿フイルムであるアルミニウム蒸着フイルムとしては、凸版印刷株式会社製のJYK5K5、HNZ8K5、東レフイルム加工株式会社製のVM−CPP、VM−OPP、VM−PET等が挙げられ、これらで形成された容器を用いることができる。
The moisture-proof container filled and sealed with the powder composition according to the present invention is not particularly limited as long as it has moisture-proof property, but a sealable film formed of a moisture-proof film such as a film in which aluminum vapor deposition is applied to at least the inner layer of the container. It is preferable to use a cylindrical container or a bag-shaped container made of a sealable synthetic resin (for example, polyethylene, polypropylene, etc.) containing a desiccant such as silica gel or alumina gel. When the powder composition is filled in a container containing the desiccant, it is desirable to store and package the powder composition together with the desiccant. By using such a moisture-proof container, discoloration of the powder composition due to the component (A) can be sufficiently prevented and stabilized even over time, and the discriminability of saliva buffering ability can be improved. Of these, a sealable film-like container formed of the moisture-proof film is preferable from the viewpoint of stability over time (no discoloration) and manufacturability of the powder composition. The moisture-proof container is preferably hermetically packaged with a sealer or the like after filling the powder composition.
As the moisture-proof container, a commercially available product can be used. For example, as an aluminum vapor deposition film which is a moisture-proof film, JYK5K5, HNZ8K5 manufactured by Toppan Printing Co., Ltd., VM-CPP, VM-OPP, VM-PET manufactured by Toray Film Co., Ltd., etc. And a container formed of these can be used.

本発明の口腔用製品は、口腔内に使用時に粉体組成物を水に溶解して液体製剤として使用することが好ましく、洗口剤として使用することがより好ましい。この場合、口腔用製品は、防湿容器を開封して充填、密封された粉体組成物を全て取り出し、適量の水に溶解させて液体の口腔用製剤として使用できる。
粉体組成物は、上記各成分の使用量を満たす範囲で、適量の水に溶解させて使用することが好ましい。粉体組成物が(C)成分を含む場合は、2〜250倍量、特に25〜200倍量の水に溶解させて使用することが好ましく、(C)成分を含まない場合は、500〜20,000倍量、特に1,000〜10,000倍量の水に溶解させて使用することが好ましい。
The oral product of the present invention is preferably used as a liquid preparation by dissolving the powder composition in water when used in the oral cavity, and more preferably used as a mouthwash. In this case, the oral product can be used as a liquid oral preparation by opening the moisture-proof container, filling and taking out all the sealed powder composition, and dissolving it in an appropriate amount of water.
The powder composition is preferably used by dissolving it in an appropriate amount of water within a range satisfying the use amounts of the above components. When the powder composition contains the component (C), it is preferably dissolved in water in an amount of 2 to 250 times, particularly 25 to 200 times, and when the powder composition does not contain the component (C), it is 500 to It is preferable to use it after dissolving it in 20,000-fold amount, especially 1,000-10,000-fold amount of water.

上記水に溶解後の液体製剤のpH(25℃)は8〜10、特に8.5〜10であることが、唾液緩衝能の分かり易さの点から好ましい。上記範囲内であると、唾液緩衝能の分かり易さがより優れる。 The pH (25° C.) of the liquid preparation after dissolution in water is preferably 8 to 10, particularly 8.5 to 10 from the viewpoint of easy understanding of saliva buffering ability. Within the above range, the saliva buffering ability is more easily understood.

本発明の口腔用製品は、上記のように液体製剤で使用し、例えば液体製剤5〜50mLを口に含み、通常の方法で口腔内を数回濯いで吐き出し、その際の色の変化から、個人の唾液緩衝能を判断、把握することができる。唾液緩衝能は、青に近いほど緩衝力が弱く、赤に近くなるにつれて緩衝力が強いと判断することができる。10〜30mLを口に含むのが、唾液緩衝能が判断し易い観点から望ましい。 The oral product of the present invention is used in a liquid formulation as described above, for example, 5 to 50 mL of the liquid formulation is contained in the mouth, and the oral cavity is rinsed and exhaled several times by a usual method, and the color change at that time causes a change. It is possible to judge and grasp the saliva buffering capacity of an individual. It can be determined that the saliva buffering power is weaker as it is closer to blue and stronger as it is closer to red. It is desirable to contain 10 to 30 mL in the mouth from the viewpoint of easy judgment of the saliva buffering capacity.

以下、実施例及び比較例を示し、本発明を具体的に説明するが、本発明は下記の実施例に制限されるものではない。なお、下記の例において%は特に断らない限りいずれも質量%を示す。 Hereinafter, the present invention will be specifically described by showing Examples and Comparative Examples, but the present invention is not limited to the following Examples. In the following examples,% means mass% unless otherwise specified.

[実施例、比較例]
表1〜8に示す成分を用いて下記方法で組成物を調製し、容器に入れ包装して口腔用製品を得た。得られた口腔用製品について、唾液緩衝能の分かり易さ及び経時安定性(退色のなさ)を下記方法で評価した。更に、表5、6に示す口腔用製品については、下記方法で口腔内保湿効果を評価し、表7、8に示す口腔用製品については、下記方法で口腔内保湿効果及び口臭抑制効果を評価した。結果を表1〜8に併記した。
[Examples and Comparative Examples]
A composition was prepared by using the components shown in Tables 1 to 8 by the following method, put into a container and packaged to obtain an oral product. With respect to the obtained oral products, the intelligibility of saliva buffering ability and the stability over time (no discoloration) were evaluated by the following methods. Further, the oral products shown in Tables 5 and 6 were evaluated for the oral moisturizing effect by the following method, and the oral products shown in Tables 7 and 8 were evaluated for the oral moisturizing effect and the bad breath suppressing effect by the following methods. did. The results are also shown in Tables 1-8.

<製造方法>
実施例1〜10、12〜31及び比較例1〜3、5〜7の製造方法:
表に示す量の(A)、(B)成分、更には(C)、(D)成分を各々、精密天秤(MS−TS分析天びん、メトラートレード社製)を用いて秤量して組成物(粉体)を調製した後、容器のアルミニウム蒸着フイルム(構成;最外層から順次、ポリエチレンテレフタレート12μm/アルミニウム7μm/無軸延伸ポリプロピレン40μm、品名:HNZ8K5、凸版印刷(株)製))で形成されたフイルム状容器(以下、アルミ蒸着フイルムと略記)に充填し、シーラー(富士インパルス(株)製、型式:FIK−300)を用いて密封して包装した。比較例については上記方法に準じて組成物を調製し、同様に容器に充填し、密封して包装した。なお、比較例1〜3、5の組成物は粉体であるが、比較例6、7の組成物は液状であった。
実施例11の製造方法:
表に示す量の(A)、(B)成分を各々、精密天秤(MS−TS分析天びん、メトラートレード社製)を用いて秤量して組成物(粉体)を調製した後、容器のポリエチレン袋(商品CD:FPE−B9−80(50mm×70mm、厚み40μm)、ジャストコーポレーション(株)製)に、ポリエチレン袋(商品CD:FPE−S−40(40mm×55mm、厚み40μm)、ジャストコーポレーション(株)製)に入れて封をしたシリカゲル(関東化学(株)製)0.5gと共に充填し(以下、シリカゲル内包ポリエチレン袋と略記)、密封して包装した。
比較例4の製造方法:
表に示す量の(A)、(B)成分を各々、精密天秤(MS−TS分析天びん、メトラートレード社製)を用いて秤量して組成物(粉体)を調製した後、容器のポリエチレン袋(商品CD:FPE−S−40(40mm×55mm、厚み40μm)ジャストコーポレーション(株)製)に充填し、密封して包装した。
<Manufacturing method>
Manufacturing method of Examples 1-10, 12-31 and Comparative Examples 1-3, 5-7:
The amounts of the components (A) and (B) shown in the table, and further the components (C) and (D), were weighed using a precision balance (MS-TS analytical balance, manufactured by METTLER TRADE Co., Ltd.) to obtain a composition ( Powder), and formed with an aluminum vapor-deposited film (constitution; polyethylene terephthalate 12 μm/aluminum 7 μm/axially stretched polypropylene 40 μm, product name: HNZ8K5, manufactured by Toppan Printing Co., Ltd.)) in order from the outermost layer. A film-like container (hereinafter abbreviated as an aluminum vapor-deposited film) was filled and hermetically sealed using a sealer (manufactured by Fuji Impulse Co., Ltd., model: FIK-300). For Comparative Example, a composition was prepared according to the above method, similarly filled in a container, sealed and packaged. The compositions of Comparative Examples 1 to 5 were powders, whereas the compositions of Comparative Examples 6 and 7 were liquids.
Manufacturing method of Example 11:
The components (A) and (B) in the amounts shown in the table were each weighed using a precision balance (MS-TS analytical balance, manufactured by METTLER TRADE CO., LTD.) to prepare a composition (powder), and then polyethylene in the container. A bag (product CD: FPE-B9-80 (50 mm×70 mm, thickness 40 μm), manufactured by Just Corporation), a polyethylene bag (product CD: FPE-S-40 (40 mm×55 mm, thickness 40 μm), Just Corporation) 0.5 g of silica gel (manufactured by Kanto Kagaku Co., Ltd.) placed in and sealed in (manufactured by K.K.) was filled (hereinafter abbreviated as silica gel-containing polyethylene bag), and sealed and packaged.
Manufacturing method of Comparative Example 4:
The components (A) and (B) in the amounts shown in the table were each weighed using a precision balance (MS-TS analytical balance, manufactured by METTLER TRADE CO., LTD.) to prepare a composition (powder), and then polyethylene in the container. A bag (product CD: FPE-S-40 (40 mm×55 mm, thickness 40 μm) manufactured by Just Corporation Co., Ltd.) was filled, sealed and packaged.

また、各例の口腔用製品の容器を開封して組成物を取り出し、25℃の水道水20mLに溶解させた後の水溶液のpH(25℃)をコンパクトPHメーターLAQUAtwin−PH−22B、株式会社堀場製作所製によって測定し、表に併記した。 In addition, the container of the oral cavity product of each example was opened, the composition was taken out, and the pH (25° C.) of the aqueous solution after being dissolved in 20 mL of tap water at 25° C. was adjusted to Compact PH meter LAQUATwin-PH-22B, Inc. Measured by Horiba, Ltd., and also shown in the table.

<唾液緩衝能の分かり易さの緩衝能の評価方法>
各例の口腔用製品の容器を開封して組成物を取り出し、25℃の水道水20mLに溶解させた。被験者9名がそれぞれ、得られた水溶液20mLを口に含み、口腔内を10回濯いだ後、吐き出し、製剤の色の変化から唾液の緩衝能を判断した。なお、容器から取り出し水に溶かした水溶液(口に含んで使用する前)は、青色であった。
唾液の緩衝能は、青色に近いほど緩衝力が弱く、赤色に近くなるにつれて緩衝力が強いと判定した。この唾液の緩衝能の判断において、「緩衝能の視覚的な分かり易さ(製剤の色の変化の分かり易さ)」を評価し、色の変化が鮮明ではっきり認識できて唾液の緩衝能が分かり易いものを合格であると判断し、合格と判断した人数から下記基準で緩衝能の分かり易さを評価した。
評価基準
◎:6名以上が分かり易いと評価した
○:4〜5名が分かり易いと評価した
×:3名以下が分かり易いと評価した
<Evaluation method of saliva buffering ability for easy understanding>
The container of the oral product of each example was opened, the composition was taken out, and dissolved in 20 mL of tap water at 25°C. Each of the nine test subjects contained 20 mL of the obtained aqueous solution in their mouth, rinsed the inside of the mouth 10 times, then vomited, and judged the saliva buffering capacity from the color change of the preparation. The aqueous solution taken out of the container and dissolved in water (before containing it in the mouth for use) was blue.
Regarding the buffer capacity of saliva, it was judged that the closer it was to blue, the weaker the buffering capacity was, and the closer it was to red, the stronger the buffering capacity was. In this judgment of the buffer capacity of saliva, "visual easiness of buffer capacity (ease of recognizing color change of preparation)" was evaluated, and the color change was clearly and clearly recognized and the buffer capacity of saliva was improved. The ones that were easy to understand were judged to be acceptable, and the ease of understanding of the buffer capacity was evaluated based on the following criteria from the number of people who were judged to be acceptable.
Evaluation Criteria ◎: 6 or more people evaluated it as easy to understand ○: 4-5 people evaluated it as easy to understand ×: 3 people or less evaluated it as easy to understand

<経時安定性(退色のなさ)の評価方法>
各例の口腔用製品を室温で一週間保存後、容器を開封して組成物を取り出し、調製直後の組成物と比較した組成物の外観変化(退色のなさ)を判断し、下記基準で経時安定性(退色のなさ)を評価した。
評価基準
○:変化がなく退色が認められない
×:退色が認められる
<Evaluation method of stability over time (no fading)>
After the oral products of each example were stored at room temperature for one week, the container was opened and the composition was taken out, and the appearance change (no discoloration) of the composition compared with the composition immediately after preparation was judged, and the time elapsed according to the following criteria. Stability (no fading) was evaluated.
Evaluation criteria ○: No change and no fading observed ×: Fading observed

<口腔内保湿効果の評価方法>
実施例18〜31の口腔用製品について、各製品の容器を開封して組成物を取り出し、25℃の水道水20mLに溶解させた。被験者9名がそれぞれ、得られた水溶液20mLを口に含み、口腔内を10回濯いだ後、吐き出し、「口腔内が保湿された感じ」を評価した。使用前に比べて口腔内が保湿されたと感じられるものを合格であると判断し、合格と判断した人数から下記基準で口腔内保湿効果を評価した。
評価基準
◎:8名以上が使用後に保湿感を感じると評価した
○:6〜7名が使用後に保湿感を感じると評価した
△:4〜5名が使用後に保湿感を感じると評価した
×:3名以下が使用後に保湿感を感じると評価した
<Evaluation method of oral moisturizing effect>
Regarding the oral products of Examples 18 to 31, the container of each product was opened and the composition was taken out and dissolved in 20 mL of tap water at 25°C. Each of the nine test subjects contained 20 mL of the obtained aqueous solution in their mouth, rinsed the inside of the oral cavity 10 times, and then spit out to evaluate the "moisturized feeling in the oral cavity". Those that felt that the oral cavity was moisturized compared to before use were judged to be acceptable, and the oral moisturizing effect was evaluated based on the following criteria from the number of people judged to be acceptable.
Evaluation Criteria ⊚: Eight or more people evaluated that they felt moisturizing feeling after use ○: 6 to 7 people evaluated that they felt moisturized feeling after use Δ: 4 to 5 people evaluated that they felt moisturized feeling after use × : 3 or less people evaluated that they felt moisturizing feeling after use.

<口臭抑制効果の評価方法>
実施例25〜31の口腔用製品について、各製品の容器を開封して組成物を取り出し、25℃の水道水20mLに溶解させた。被験者9名がそれぞれ、得られた水溶液20mLを口に含み、口腔内を10回濯いだ後、吐き出し、「口臭が抑制された感じ」を評価した。使用前に比べて口臭が抑制されたと感じられたものを合格であると判断し、合格と判断した人数から下記基準で口臭抑制効果を評価した。
評価基準
◎:8名以上が使用後に口臭が抑制された感じがすると評価した
○:6〜7名が使用後に口臭が抑制された感じがすると評価した
△:4〜5名が使用後に口臭が抑制された感じがすると評価した
×:3名以下が使用後に口臭が抑制された感じがすると評価した
<Evaluation method of bad breath control effect>
Regarding the oral products of Examples 25 to 31, the container of each product was opened and the composition was taken out and dissolved in 20 mL of tap water at 25°C. Each of the nine test subjects contained 20 mL of the obtained aqueous solution in their mouth, rinsed the inside of the mouth 10 times, then vomited, and evaluated "feeling that bad breath was suppressed". Those who felt that bad breath was suppressed compared to before use were judged to be acceptable, and the bad breath suppressing effect was evaluated based on the following criteria from the number of people judged to be acceptable.
Evaluation Criteria ⊚: Eight or more people evaluated that the bad breath was suppressed after use. ○: 6 to 7 people evaluated that the bad breath was suppressed after use. Δ: 4 to 5 people felt the bad breath after use. It was evaluated that it felt suppressed. ×: 3 or less people evaluated that they felt that bad breath was suppressed after use.

使用原料の詳細を下記に示す。
(A)粉末サンレッドYM(商品名、アントシアニン系色素43%含有、三栄源エフ・
エフ・アイ株式会社製)
粉末サンレッドRCU(商品名、アントシアニン系色素36%含有、三栄源エフ
・エフ・アイ株式会社製)
カルミン酸(粉末、コチニール色素、比較成分、三栄源エフ・エフ・アイ株式会社製)
クルクミン(粉末、ウコン色素、比較成分、三栄源エフ・エフ・アイ株式会社製)
(B)炭酸ナトリウム(粉末、富士フイルム和光純薬株式会社製)
炭酸水素ナトリウム(粉末、富士フイルム和光純薬株式会社製)
水酸化ナトリウム(粉末、富士フイルム和光純薬株式会社製)
水酸化カリウム(粉末、富士フイルム和光純薬株式会社製)
モノエタノールアミン(比較成分)(液体の有機塩基、東京化成工業株式会社製)
10%水酸化ナトリウム水溶液(比較成分)(富士フイルム和光純薬株式会社製)
(C)ソルビット(粉末、D−ソルビトール、LTS−P G−3、三菱商事フードテッ
ク株式会社製)
トレハロース(粉末、林原株式会社製)
キシリトール(キシリット粉末、三菱商事フードテック株式会社製)
(D)塩化セチルピリジニウム(粉末、富士フイルム和光純薬株式会社製)
塩化ベンザルコニウム(粉末、富士フイルム和光純薬株式会社製)
Details of the raw materials used are shown below.
(A) Powder Sun Red YM (trade name, containing 43% anthocyanin dye, Sanei Gen F.
(Manufactured by FI Corporation)
Powder Sun Red RCU (trade name, containing 36% anthocyanin dye, Sanei Gen F
・F-I Co., Ltd.)
Carminic acid (powder, cochineal dye, comparative ingredient, Saneigen FFI Corporation)
Curcumin (powder, turmeric pigment, comparative ingredient, Sanei Gen FFI Co., Ltd.)
(B) Sodium carbonate (powder, manufactured by Fujifilm Wako Pure Chemical Industries, Ltd.)
Sodium hydrogen carbonate (powder, manufactured by Fujifilm Wako Pure Chemical Industries, Ltd.)
Sodium hydroxide (powder, manufactured by Fujifilm Wako Pure Chemical Industries, Ltd.)
Potassium hydroxide (powder, manufactured by Fujifilm Wako Pure Chemical Industries, Ltd.)
Monoethanolamine (comparative component) (liquid organic base, manufactured by Tokyo Chemical Industry Co., Ltd.)
10% sodium hydroxide aqueous solution (comparative component) (manufactured by FUJIFILM Wako Pure Chemical Industries, Ltd.)
(C) Solbit (powder, D-sorbitol, LTS-PG-3, Mitsubishi Foodstuff
KU Co., Ltd.)
Trehalose (powder, manufactured by Hayashibara Co., Ltd.)
Xylitol (Xylit powder, manufactured by Mitsubishi Corporation Foodtech Co., Ltd.)
(D) Cetylpyridinium chloride (powder, manufactured by Fujifilm Wako Pure Chemical Industries, Ltd.)
Benzalkonium chloride (powder, manufactured by Fujifilm Wako Pure Chemical Industries, Ltd.)

Figure 2020097536

*;アントシアニン系色素の純分量(以下同様)
**;(A)成分のアントシアニン系色素としての量/(B)成分量(以下同様)
Figure 2020097536

*: Pure amount of anthocyanin dye (same below)
**: Amount of component (A) as anthocyanin dye/amount of component (B) (same below)

Figure 2020097536
Figure 2020097536

Figure 2020097536
Figure 2020097536

Figure 2020097536
***;液状の組成物
Figure 2020097536
*** Liquid composition

Figure 2020097536
Figure 2020097536

Figure 2020097536
Figure 2020097536

Figure 2020097536
Figure 2020097536

Figure 2020097536
Figure 2020097536

Claims (11)

(A)アントシアニン系色素粉末、及び
(B)5〜40℃で固体の無機塩基
を含有する粉体組成物が、防湿容器に充填された口腔用製品。
An oral product in which a moisture-proof container is filled with a powder composition containing (A) anthocyanin-based pigment powder and (B) a solid inorganic base at 5 to 40°C.
(B)5〜40℃で固体の無機塩基が、炭酸ナトリウム、炭酸カリウム、炭酸水素ナトリウム、炭酸水素カリウム、リン酸2水素ナトリウム、リン酸水素2ナトリウム、水酸化ナトリウム、水酸化カリウム及び水酸化リチウムから選ばれる1種以上の無機塩基粉末である請求項1記載の口腔用製品。 (B) The solid inorganic base at 5 to 40° C. is sodium carbonate, potassium carbonate, sodium hydrogencarbonate, potassium hydrogencarbonate, sodium dihydrogenphosphate, disodium hydrogenphosphate, sodium hydroxide, potassium hydroxide and hydroxylation. The oral product according to claim 1, which is one or more kinds of inorganic base powder selected from lithium. (B)5〜40℃で固体の無機塩基が、炭酸ナトリウム、炭酸カリウム、水酸化ナトリウム及び水酸化カリウムから選ばれる請求項2記載の口腔用製品。 The oral product according to claim 2, wherein the inorganic base (B) which is solid at 5 to 40°C is selected from sodium carbonate, potassium carbonate, sodium hydroxide and potassium hydroxide. (A)/(B)が質量比として0.01〜12.5である請求項1〜3のいずれか1項記載の口腔用製品。 The oral product according to any one of claims 1 to 3, wherein (A)/(B) has a mass ratio of 0.01 to 12.5. 粉体組成物が、更に、(C)5〜40℃で固体の湿潤剤を含有する請求項1〜4のいずれか1項記載の口腔用製品。 The oral composition according to any one of claims 1 to 4, wherein the powder composition further contains (C) a wetting agent that is solid at 5 to 40°C. 粉体組成物が、更に、(D)5〜40℃で固体の殺菌抗菌剤を含有する請求項1〜5のいずれか1項記載の口腔用製品。 The oral product according to any one of claims 1 to 5, wherein the powder composition further contains (D) a bactericidal antibacterial agent which is solid at 5 to 40°C. 防湿容器が、アルミニウム蒸着が施された防湿フイルムで形成された密封可能な容器又は乾燥剤が内包された密封可能な合成樹脂製容器である請求項1〜6のいずれか1項記載の口腔用製品。 The oral cavity according to any one of claims 1 to 6, wherein the moisture-proof container is a sealable container formed of a moisture-proof film having aluminum vapor deposition or a sealable synthetic resin container containing a desiccant. Product. 使用時に防湿容器から取り出した粉体組成物を水に溶解して液体製剤として使用される請求項1〜7のいずれか1項記載の口腔用製品。 The oral product according to any one of claims 1 to 7, which is used as a liquid preparation by dissolving the powder composition taken out of the moisture-proof container at the time of use in water. 液体製剤の25℃におけるpHが8〜10である請求項8記載の口腔用製品。 The oral product according to claim 8, wherein the pH of the liquid preparation at 25°C is 8 to 10. 液体製剤が洗口剤である請求項8又は9記載の口腔用製品。 The oral product according to claim 8 or 9, wherein the liquid preparation is a mouthwash. 唾液緩衝能の検査用である請求項1〜10のいずれか1項記載の口腔用製品。 The oral product according to any one of claims 1 to 10, which is for testing saliva buffering ability.
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WO2022138144A1 (en) * 2020-12-23 2022-06-30 小林製薬株式会社 Oral composition

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JPH11302142A (en) * 1998-04-24 1999-11-02 Sunstar Inc Food composition for prevention and treatment of periodontal disease, oral composition and pharmaceutical composition
JP2009530014A (en) * 2006-03-22 2009-08-27 高砂香料工業株式会社 Deodorant composition
JP2015500348A (en) * 2011-12-19 2015-01-05 コルゲート・パーモリブ・カンパニーColgate−Palmolive Company Liquid activation system

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JPH11302142A (en) * 1998-04-24 1999-11-02 Sunstar Inc Food composition for prevention and treatment of periodontal disease, oral composition and pharmaceutical composition
JP2009530014A (en) * 2006-03-22 2009-08-27 高砂香料工業株式会社 Deodorant composition
JP2015500348A (en) * 2011-12-19 2015-01-05 コルゲート・パーモリブ・カンパニーColgate−Palmolive Company Liquid activation system

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2022138144A1 (en) * 2020-12-23 2022-06-30 小林製薬株式会社 Oral composition

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