JP2010038666A - Ammonia inspecting instrument and sensitivity adjusting method of ammonia inspecting instrument - Google Patents

Ammonia inspecting instrument and sensitivity adjusting method of ammonia inspecting instrument Download PDF

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JP2010038666A
JP2010038666A JP2008200338A JP2008200338A JP2010038666A JP 2010038666 A JP2010038666 A JP 2010038666A JP 2008200338 A JP2008200338 A JP 2008200338A JP 2008200338 A JP2008200338 A JP 2008200338A JP 2010038666 A JP2010038666 A JP 2010038666A
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ammonia
saliva
indicator layer
coating
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JP5266940B2 (en
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Ichiro Nakajima
一郎 中島
Masao Ishikawa
正夫 石川
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Lion Corp
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<P>PROBLEM TO BE SOLVED: To provide an ammonia inspecting instrument for precisely detecting and measuring ammonia in saliva in a short time by simple operation, and an ammonia inspecting method. <P>SOLUTION: The ammonia inspecting instrument has an indicator layer 2, which causes color reaction by ammonia, on a support 1. The indicator layer is covered with a film 4 formed from a covering agent aqueous solution containing a polyvinylpyrrolidone and a surfactant and adjusted to a pH of 2.0-5.0 (25°C), so that the dry mass of the film is 25-50 mass% of the indicator layer and detects or measures ammonia in saliva. As a result, the saliva being a sample is used as a specimen as it is without performing dilution operation to precisely detect or measure ammonia in the saliva in a short time by simple operation and an aspect from safety or an aspect from environment is also good. Further, a bad breath or the number of bacteria in the saliva can be estimated from the detected or measured result of ammonia in the saliva and sanitariness in the oral cavity can be judged using the detected or measured result as an index. <P>COPYRIGHT: (C)2010,JPO&INPIT

Description

本発明は、唾液中に含まれるアンモニアの検出又はその濃度の測定を、唾液(検体)の希釈操作を行うことなく迅速かつ簡便に、精度良く行うことができるアンモニア検査具、及びその感度調整方法に関する。   The present invention relates to an ammonia test device capable of detecting ammonia contained in saliva or measuring the concentration thereof quickly, simply and accurately without performing a dilution operation of saliva (specimen), and a sensitivity adjustment method thereof. About.

口腔内の清潔度に影響する因子として、プラーク(歯垢)や歯石の存在、舌苔の付着量、唾液の濁度、口腔内の細菌数などが考えられている。これら因子を簡便にチェックできる方法として、例えばプラーク、歯石、舌苔付着量については、歯垢染色剤のエリスロシン、フロキシンなどの色素や、蛍光色素のフルオレセインナトリウム、新しい歯垢と古い歯垢を色分けする2色性歯垢染色剤ツートン(株式会社モリタ製)などを用い、染色の有無等により判別する方法がある。   Factors affecting the cleanliness of the oral cavity include the presence of plaque (plaque) and tartar, the amount of tongue coating, turbidity of saliva, the number of bacteria in the oral cavity, and the like. As a method that can easily check these factors, for example, for plaque, tartar, and tongue coating, pigments such as erythrosine and phloxine, the fluorescent dye fluorescein sodium, and new and old plaques are color-coded. There is a method of discriminating the presence or absence of staining using a dichroic plaque stain agent Totone (manufactured by Morita Co., Ltd.).

しかし、これらの染色を利用した方法は、使用する色素による着色部位の選択性が低く、唇や粘膜細胞などの染色する必要がない部位も染色されてしまうことや、退色に長時間を要することなどから審美面でも問題があった。   However, the methods using these dyeings have low selectivity of the colored portion depending on the dye used, and portions that do not need to be stained, such as lips and mucosal cells, are also stained, and it takes a long time to fade. There was also a problem with aesthetics.

唾液の濁度測定による検査方法としては、唾液性状検査用キット及び口腔内疾患判定方法(特許文献1:特開2004−108976号公報参照)が提案され、唾液の濁度が口臭との間に密接な相関があることが示されている。しかし、この方法は唾液中の不溶性物質量を視覚的に判定するものであるが、唾液の成分が均等に分散し難いことが測定値のばらつきの原因となり、精度に劣るものであった。   As an inspection method by measuring the turbidity of saliva, a saliva property inspection kit and an oral disease determination method (see Patent Document 1: Japanese Patent Laid-Open No. 2004-108976) are proposed, and the turbidity of saliva is between bad breath and It is shown that there is a close correlation. However, this method visually determines the amount of insoluble substances in saliva. However, it is difficult to evenly disperse the components of saliva, resulting in variations in measured values and inferior accuracy.

口腔内の細菌数を調べる方法としては、一般に試料を一定倍数に希釈・分散させ、培養後のコロニー数をカウントする方法が行われているが、この方法は希釈倍数に個人差が影響したり、培地調製や培養時間に長時間を要するなど、操作が面倒であるといった問題点があった。   As a method of examining the number of bacteria in the oral cavity, generally, a method is used in which a sample is diluted and dispersed to a fixed multiple and the number of colonies after culture is counted, but this method is influenced by individual differences in the diluted multiple. In addition, there is a problem that the operation is troublesome, for example, it takes a long time to prepare a medium and culture time.

特定細菌に対するモノクローナル抗体を用いた口腔内の細菌量の測定(特許文献2:特開昭60−73463号公報、特許文献3:特開昭62−211558号公報参照)、DNAやRNAプローブを用いた細菌や細胞数の測定方法(特許文献4:特開昭61−257200号公報参照)なども提案されている。しかし、これらの方法は、特殊かつ高価な試薬を用いるため集団検診や健康教育などで広範囲の人々が使用するには、経済的に問題があった。   Measurement of the amount of bacteria in the oral cavity using a monoclonal antibody against a specific bacterium (Patent Document 2: JP-A-60-73463, Patent Document 3: JP-A-62-211558), using a DNA or RNA probe A method for measuring the number of bacteria and cells (see Japanese Patent Application Laid-Open No. Sho 61-257200) has also been proposed. However, since these methods use special and expensive reagents, they are economically problematic for use by a wide range of people in group medical examinations and health education.

一方、アンモニアが口臭や唾液中の細菌数といった因子と高い相関を示すこと(非特許文献1:J.Dent.Res.Abstracts #1830,2006参照)が知られている。そこで、出願人は、唾液中のアンモニアを指標とすることで口腔内の清潔度を推測することが可能であると考え、唾液中のアンモニアを測定する手段について検討した。しかし、公知のアンモニア検査紙などのアンモニアを検出又は測定する検査手段は、水質検査や血中のアンモニア濃度の測定には適しているものの、その感度が高いために唾液中のアンモニアを簡単に精度良く検出又は測定するには不適であった。   On the other hand, it is known that ammonia has a high correlation with factors such as bad breath and the number of bacteria in saliva (see Non-Patent Document 1: J. Dent. Res. Abstracts # 1830, 2006). Therefore, the applicant considered that it is possible to estimate the cleanliness in the oral cavity by using ammonia in saliva as an index, and studied means for measuring ammonia in saliva. However, while the detection means for detecting or measuring ammonia, such as the known ammonia test paper, is suitable for water quality testing and measurement of ammonia concentration in blood, its sensitivity is high, so it is easy to accurately measure ammonia in saliva. It was unsuitable to detect or measure well.

従って、唾液中のアンモニアを簡便かつ短時間で、精度よく検出又は測定することができ、唾液中のアンモニアを指標として口腔内の清潔度を推測するのに有用な検査手段の開発が望まれる。   Therefore, it is desired to develop a test means that can detect or measure ammonia in saliva easily and accurately in a short time and that is useful for estimating the cleanliness of the oral cavity using ammonia in saliva as an index.

特開2004−108976号公報JP 2004-108976 A 特開昭60−73463号公報JP 60-73463 A 特開昭62−211558号公報JP-A-62-211558 特開昭61−257200号公報JP-A-61-257200 特開昭58−193459号公報Japanese Patent Laid-Open No. 58-193459 J.Dent.Res.Abstracts #1830,2006J. et al. Dent. Res. Abstracts # 1830, 2006

本発明は、上記事情に鑑みなされたもので、短時間でかつ簡易な操作で、精度良く、唾液中のアンモニアを検出又はその濃度を測定できるアンモニア検査具、及びその感度調整方法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 provides an ammonia test tool capable of detecting ammonia in saliva or measuring the concentration thereof in a short time and with a simple operation, and a sensitivity adjustment method thereof. With the goal.

本発明者らは上記目的を達成するため鋭意研究を重ねた結果、支持体上に、アンモニアにより呈色反応する指示薬層を有するアンモニア検査具であって、前記指示薬層が、ポリビニルピロリドンと界面活性剤とを含有しpH2.0〜5.0(25℃)に調整された被覆剤水溶液で形成された皮膜で被覆されてなり、該皮膜の乾燥質量が指示薬層の25〜50質量%であることにより、指示薬層の感度が調整されて、試料の唾液を希釈操作することなくそのまま検体として使用して、短時間でかつ簡易な操作で、精度良く、唾液中のアンモニアを検出又はその濃度を測定できるアンモニア検査具が得られることを見出した。   As a result of intensive studies to achieve the above object, the inventors of the present invention provide an ammonia test tool having an indicator layer that is colored by ammonia on a support, and the indicator layer has a surface activity with polyvinylpyrrolidone. And a coating formed with a coating aqueous solution adjusted to pH 2.0 to 5.0 (25 ° C.), and the dry mass of the coating is 25 to 50% by mass of the indicator layer Thus, the sensitivity of the indicator layer is adjusted, and the saliva of the sample is used as it is as a specimen without diluting operation, and ammonia in saliva is detected or its concentration is accurately detected in a short time and with simple operation. It has been found that an ammonia tester that can be measured is obtained.

即ち、本発明者らは口腔内の清潔度を判断する指標として、口臭や唾液中の細菌数といった因子と高い相関を示すアンモニアに注目し、唾液中のアンモニアを検出又は測定する検査手段について検討した。
液体試料中のアンモニア又は尿素の濃度を測定するための分析具は、特許文献5:特開昭58−193459号公報等に提案され、水質検査や血中のアンモニア濃度を測定するためのアンモニア検査紙は種々市販されている。
例えば、アミチェック(商品名、(株)京都第一科学製)は、アミノ酸代謝異常、肝機能異常、腎機能異常などの病態把握を目的に血中、血清又は血漿中のアンモニアを測定するものである。これは、その添付文書からアンモニア測定濃度範囲は0.1〜4μg/mLと考えられ、血中アンモニアの基準値が0.18〜0.70μg/mLであることから、適度な測定濃度範囲となる。簡易水質検査試験紙のアクアチェックA(商品名、バイエルメディカル(株)製)は、0.1〜10μg/mLのアンモニアが測定できる。テストスティックアンモニア(商品名、(株)ニッソー製)は、0.1〜5μg/mLのアンモニアが測定でき、熱帯魚や観賞魚の水槽中の水質検査に好ましい測定濃度の範囲となっている。
That is, the present inventors focused on ammonia showing a high correlation with factors such as bad breath and the number of bacteria in saliva as an index for judging the cleanliness of the oral cavity, and examined an inspection means for detecting or measuring ammonia in saliva. did.
An analyzer for measuring the concentration of ammonia or urea in a liquid sample is proposed in Patent Document 5: Japanese Patent Laid-Open No. 58-193259, etc., and an ammonia test for measuring water quality and blood ammonia concentration. Various papers are commercially available.
For example, Amicheck (trade name, manufactured by Kyoto Daiichi Kagaku Co., Ltd.) measures ammonia in blood, serum, or plasma for the purpose of understanding pathological conditions such as abnormal amino acid metabolism, abnormal liver function, and abnormal renal function. It is. From the package insert, it is considered that the ammonia measurement concentration range is 0.1 to 4 μg / mL, and the blood ammonia reference value is 0.18 to 0.70 μg / mL. Become. Aqua Check A (trade name, manufactured by Bayer Medical Co., Ltd.), a simple water quality test paper, can measure 0.1 to 10 μg / mL of ammonia. Test stick ammonia (trade name, manufactured by Nisso Co., Ltd.) can measure 0.1 to 5 μg / mL of ammonia, and is in a range of measurement concentration preferable for water quality inspection in aquarium of tropical fish and ornamental fish.

しかしながら、成人唾液中のアンモニア濃度は約10〜1,000μg/mLの範囲(J.Dent.Res.Abstracts #1830,2006参照)であるため、市販検査紙は測定感度が高すぎるために唾液中のアンモニアを精度良く検出又は測定するには不適であった。なお、メルコクアントアンモニウムテスト(商品名、MERCK社製)は、測定範囲が0.1〜400μg/mLで、より高濃度までアンモニア測定が可能ではあるが、有毒なヨウ化水銀(II)を使用することから安全面、環境面で問題があった。
これらの市販アンモニア検査紙のアンモニア測定範囲、更には唾液中のアンモニア濃度は、表1に示すとおりである。
However, since the ammonia concentration in the adult saliva is in the range of about 10 to 1,000 μg / mL (see J. Dent. Res. Abstracts # 1830, 2006), the commercially available test paper is too sensitive to the measurement in the saliva. It was unsuitable for accurately detecting or measuring ammonia. In addition, the merquaqua ammonium test (trade name, manufactured by MERCK) has a measuring range of 0.1 to 400 μg / mL and can measure ammonia up to a higher concentration, but uses toxic mercury (II) iodide. As a result, there were problems in terms of safety and environment.
Table 1 shows the ammonia measurement range of these commercially available ammonia test papers and the ammonia concentration in saliva.

Figure 2010038666
Figure 2010038666

口中から採取した唾液を予め適当濃度まで希釈してこの希釈唾液を検体として使用すれば、上記市販品を用いて唾液中のアンモニアを検出又は測定することは可能であるが、唾液を希釈する操作は手間がかかり面倒であり、工程が煩雑となって処理時間もかかり、これらの要因が測定精度へ悪影響を及ぼす場合もある。集団検診や健康教育事業などで行う検査は、簡便かつ安価で短時間に検査結果が得られることが望ましい。   If saliva collected from the mouth is diluted to an appropriate concentration in advance and this diluted saliva is used as a sample, it is possible to detect or measure ammonia in the saliva using the above-mentioned commercial product, but the operation of diluting saliva Is cumbersome and cumbersome, and the process becomes complicated and takes a long time. These factors may adversely affect the measurement accuracy. It is desirable that examinations performed in group examinations, health education projects, etc. are simple and inexpensive and can obtain examination results in a short time.

本発明のアンモニア検査具によれば、上記課題を解決でき、検査具の判定部位(指示薬層)を特定の被覆剤水溶液に浸漬し、乾燥することにより得られる皮膜で被覆することにより、アンモニアと指示薬との反応による指示薬層の発色までの展開時間が調整され、判定感度が下がることによって、唾液を希釈することなくそのまま検体として使用して判定部位に直接接触させることで、アンモニアを検出又はその濃度を精度良く、簡単な操作で測定することができる。   According to the ammonia test tool of the present invention, the above-mentioned problems can be solved, and by coating with a film obtained by immersing the determination part (indicator layer) of the test tool in a specific coating solution and drying it, ammonia and The development time until the color development of the indicator layer due to the reaction with the indicator is adjusted and the judgment sensitivity is lowered, so that the saliva is used as it is as a specimen without diluting it, and ammonia is detected or its Concentration can be measured with high accuracy and simple operation.

従って、本発明は、下記のアンモニア検査具及びその感度調整方法を提供する。
(i)支持体上に、アンモニアにより呈色反応する指示薬層を有するアンモニア検査具であって、前記指示薬層が、ポリビニルピロリドンと界面活性剤とを含有しpH2.0〜5.0(25℃)に調整された被覆剤水溶液で形成された皮膜で被覆されてなり、該皮膜の乾燥質量が指示薬層の25〜50質量%であり、唾液中のアンモニアを検出又は測定するためのものであることを特徴とするアンモニア検査具。
(ii)唾液中のアンモニアを検出又は測定して口腔内の清潔度を推測するためのものである上記アンモニア検査具。
(iii)支持体上に、アンモニアにより呈色反応する指示薬層を有するアンモニア検査具の前記指示薬層を、ポリビニルピロリドンと界面活性剤とを含有しpH2.0〜5.0(25℃)に調整された被覆剤水溶液に浸漬後、乾燥させ、乾燥質量が指示薬層の25〜50質量%である皮膜で被覆して感度を調整することを特徴とする、唾液中のアンモニアを検出又は測定するためのアンモニア検査具の感度調整方法。
Accordingly, the present invention provides the following ammonia test tool and sensitivity adjustment method thereof.
(I) An ammonia test tool having an indicator layer that reacts with ammonia on a support, wherein the indicator layer contains polyvinylpyrrolidone and a surfactant and has a pH of 2.0 to 5.0 (25 ° C. ) And a coating formed with a coating aqueous solution prepared in the above, and the dry mass of the coating is 25 to 50% by mass of the indicator layer, and is for detecting or measuring ammonia in saliva. An ammonia tester characterized by that.
(Ii) The above-described ammonia test tool for detecting or measuring ammonia in saliva to estimate the cleanliness of the oral cavity.
(Iii) The indicator layer of the ammonia tester having an indicator layer that reacts with color by ammonia on the support is adjusted to pH 2.0 to 5.0 (25 ° C.) containing polyvinylpyrrolidone and a surfactant. In order to detect or measure ammonia in saliva, which is characterized by adjusting the sensitivity by immersing in a coating aqueous solution, drying and coating with a film whose dry mass is 25 to 50% by mass of the indicator layer Sensitivity adjustment method for ammonia testing tools.

本発明のアンモニア検査具、及びその感度調整方法によれば、試料の唾液を希釈操作することなくそのまま検体として使用して、短時間でかつ簡易な操作で、精度良く、唾液中のアンモニアを検出又は測定でき、安全面や環境面も良好である。更に、本発明によれば、唾液中のアンモニアの検出又は測定結果から、口臭や唾液中の内細菌数等が推測でき、これを指標として口腔内清潔度を判断することが可能である。   According to the ammonia test tool of the present invention and its sensitivity adjustment method, the saliva of the sample is used as it is as a sample without diluting, and ammonia in saliva is detected accurately in a short time and with a simple operation. Or it can be measured, and the safety and environmental aspects are also good. Furthermore, according to the present invention, the bad breath, the number of bacteria in the saliva, and the like can be estimated from the detection or measurement result of ammonia in the saliva, and the oral cleanliness can be determined using this as an index.

以下、本発明につき更に詳細に説明すると、本発明のアンモニア検査具は、支持体上に、アンモニアにより呈色反応する指示薬層を有するアンモニア検査具であって、前記指示薬層が、特定の被覆剤水溶液で形成された皮膜で被覆されてなる。   Hereinafter, the present invention will be described in more detail. The ammonia test tool of the present invention is an ammonia test tool having an indicator layer that is colored and reacted with ammonia on a support, and the indicator layer is a specific coating agent. It is coated with a film formed with an aqueous solution.

ここで、本発明で使用される被覆剤水溶液は、ポリビニルピロリドンと界面活性剤とを含有する水溶液であり、pH2.0〜5.0(25℃)に調整される。   Here, the aqueous coating agent solution used in the present invention is an aqueous solution containing polyvinylpyrrolidone and a surfactant, and is adjusted to pH 2.0 to 5.0 (25 ° C.).

ポリビニルピロリドンは、皮膜形成成分としての高分子物質であり、平均分子量が1万〜36万、特に1万〜16万のものが好ましく、平均分子量が1万に満たないと粘度安定性が低く、36万を超えると粘度安定性は高いものの、沈殿が起こるなどの品質上の問題が発生する場合がある。
なお、上記平均分子量の測定は、分子量と相関する粘度特性値(K)で、毛細管粘度計により測定される相対粘度値(25℃)を下記のFikentscher(フィケンチャー)の式に適用して計算した値である。

Figure 2010038666
Polyvinylpyrrolidone is a polymer substance as a film-forming component, and preferably has an average molecular weight of 10,000 to 360,000, particularly 10,000 to 160,000. If the average molecular weight is less than 10,000, the viscosity stability is low, If it exceeds 360,000, the viscosity stability is high, but quality problems such as precipitation may occur.
The average molecular weight was measured by applying the relative viscosity value (25 ° C.) measured by a capillary viscometer to the following Fikentscher formula using the viscosity characteristic value (K) correlated with the molecular weight. Value.
Figure 2010038666

ポリビニルピロリドンは市販品を使用でき、例えばルビスコールK15(平均分子量1万)、K30(平均分子量4万)、K60(平均分子量16万)、K90(平均分子量36万)(いずれもBASFジャパン(株)製)が挙げられ、これらの1種を単独で用いても、あるいは2種以上を組み合わせて用いても良い。   A commercially available product can be used for polyvinylpyrrolidone, for example, Rubiscol K15 (average molecular weight 10,000), K30 (average molecular weight 40,000), K60 (average molecular weight 160,000), K90 (average molecular weight 360,000) (all of which are BASF Japan Ltd.) These may be used singly or in combination of two or more.

ポリビニルピロリドンの配合量は、被覆剤水溶液全体の10〜40%、特に25〜40%(質量%、以下同様。)、とりわけ26〜38%が好ましい。10%に満たないと、唾液のアンモニア判定時の濃度差が見づらく、40%を超えると、検査紙の指示薬層とアンモニアの反応に時間が3分以上かかり、迅速な判定ができない場合がある。   The blending amount of polyvinyl pyrrolidone is preferably 10 to 40%, particularly 25 to 40% (mass%, the same shall apply hereinafter), particularly 26 to 38%, based on the total aqueous coating agent solution. If it is less than 10%, it is difficult to see the difference in the concentration of saliva in ammonia, and if it exceeds 40%, the reaction between the indicator layer of the test paper and the ammonia takes 3 minutes or more, and quick determination may not be possible.

被覆剤には更に界面活性剤を配合する。界面活性剤を配合することで、アンモニア検査紙の指示薬層の被覆が行いやすくなり有利である。
界面活性剤としては、アニオン性界面活性剤、ノニオン性界面活性剤、カチオン性界面活性剤等を使用できる。例えば、ラウリル硫酸塩等のアルキル硫酸塩、ラウロイルサルコシン酸塩、アルキルアリールポリエチレングリコール、アミノ酸糖エステル化合物、脂肪酸糖エステル、塩化セチルピリジニウム塩などが挙げられる
A surfactant is further blended in the coating agent. By adding a surfactant, it is easy to coat the indicator layer of the ammonia test paper, which is advantageous.
As the surfactant, an anionic surfactant, a nonionic surfactant, a cationic surfactant, or the like can be used. For example, alkyl sulfates such as lauryl sulfate, lauroyl sarcosinate, alkylaryl polyethylene glycol, amino acid sugar ester compounds, fatty acid sugar esters, cetylpyridinium chloride and the like can be mentioned.

これらの中では、特にアルキル硫酸塩、ラルロイルサルコシン酸塩等のアニオン性界面活性剤、アルキルアリールポリエチレングリコール等のノニオン性界面活性剤が、被覆剤及び界面活性剤の安定性を保つ上で好ましい。   Of these, anionic surfactants such as alkyl sulfates and ralloyl sarcosinates, and nonionic surfactants such as alkylaryl polyethylene glycols are preferred for maintaining the stability of the coating agent and surfactant. .

界面活性剤の配合量は、被覆剤水溶液全体の0.3〜1.2%、特に0.5〜1.0%が好ましい。0.3%に満たないと、被覆剤による膜が形成しにくく、1.2%を超えると被覆剤の安定性に問題が発生する場合がある。   The compounding amount of the surfactant is preferably 0.3 to 1.2%, particularly preferably 0.5 to 1.0% of the whole coating solution. If it is less than 0.3%, it is difficult to form a film by the coating agent, and if it exceeds 1.2%, a problem may occur in the stability of the coating agent.

被覆剤には、更に必要に応じて、ゲルろ過剤であるセファデックスG−25、G−50、G−100(GEヘルスケア バイオサイエンス(株)製)等の公知成分を適宜添加してもよい。   If necessary, a known component such as Sephadex G-25, G-50, or G-100 (manufactured by GE Healthcare Biosciences), which is a gel filtration agent, may be added to the coating agent as necessary. Good.

本発明において、被覆剤水溶液のpHは2.0〜5.0、好ましくは2.0〜4.6の範囲に設定する。この範囲にpH調整することで、指示薬層に含まれる試薬の変色を効果的に抑えることができる。pHが5.0を超えると指示薬層の安定性の低下により変色が生じ、pHが2.0に満たないと、指示薬層の発色度が低下しアンモニア判定が行いにくくなる場合がある。
なお、pH調整には必要に応じてpH調整剤を用いることができる。pH調整剤としては、酢酸、リン酸、塩酸、クエン酸、乳酸、グルコン酸等の酸又はその塩が使用できる。
In the present invention, the pH of the aqueous coating solution solution is set in the range of 2.0 to 5.0, preferably 2.0 to 4.6. By adjusting the pH to this range, the color change of the reagent contained in the indicator layer can be effectively suppressed. If the pH exceeds 5.0, discoloration occurs due to a decrease in the stability of the indicator layer. If the pH is less than 2.0, the color development degree of the indicator layer may be reduced, and ammonia determination may be difficult.
In addition, a pH adjuster can be used for pH adjustment as needed. As the pH adjuster, an acid such as acetic acid, phosphoric acid, hydrochloric acid, citric acid, lactic acid, gluconic acid or a salt thereof can be used.

本発明のアンモニア検査具は、支持体上に、アンモニアにより呈色反応する指示薬層を有するアンモニア検査具の前記指示薬層が、上記被覆剤水溶液で形成された皮膜で被覆され、皮膜の乾燥質量が指示薬層の乾燥質量の25〜50%であるものである。   In the ammonia test tool of the present invention, the indicator layer of the ammonia test tool having an indicator layer that reacts with color by ammonia is coated on a support with a film formed of the aqueous coating solution, and the dry mass of the film is It is 25 to 50% of the dry mass of the indicator layer.

ここで、支持体上にアンモニアにより呈色反応する指示薬層を有するアンモニア検査具としては、紙、プラスチック等の支持体の表面上の一部又は全面に指示薬を含む層を有するものであればその材質や成分、構造などに特に制限はなく、支持体上に指示薬層と、唾液中のアンモニアをガス化するアルカリ性緩衝液を含む担体とを有するアンモニア検査具であってもよく、公知のアンモニア検査紙等のアンモニア検査具で、安全面や環境面に問題のないものを使用することができる。   Here, as an ammonia tester having an indicator layer that reacts with color by ammonia on the support, if it has a layer containing an indicator on part or the entire surface of the support such as paper, plastic, etc. There are no particular restrictions on the material, components, structure, etc., and it may be an ammonia tester having an indicator layer on a support and a carrier containing an alkaline buffer that gasifies ammonia in saliva, and is a known ammonia test. Ammonia testing instruments such as paper can be used that have no safety or environmental problems.

上記アンモニア検査具として具体的には、市販品を使用でき、アミチェック(商品名、(株)京都第一科学製)、アクアチェックA(商品名、バイエルメディカル(株)製)、テストスティックアンモニア(商品名、(株)ニッソー製)等が挙げられる。   Specifically, a commercially available product can be used as the above-described ammonia test tool, such as Amicheck (trade name, manufactured by Kyoto Daiichi Kagaku Co., Ltd.), Aqua Check A (trade name, manufactured by Bayer Medical Co., Ltd.), Test Stick Ammonia. (Trade name, manufactured by Nisso Corporation).

なお、アンモニア検査具の支持体の形状は、使用性の点から通常スティック状で幅3〜7mm、長さ50〜100mm、厚さ0.2〜0.4mmのものが望ましく、特に幅5mm、長さ82mm、厚さ0.25mmのものが好適である。   In addition, the shape of the support of the ammonia test tool is preferably a stick-like shape with a width of 3 to 7 mm, a length of 50 to 100 mm, and a thickness of 0.2 to 0.4 mm from the viewpoint of usability. Those having a length of 82 mm and a thickness of 0.25 mm are preferred.

指示薬層に含まれる指示薬は、例えばブロムチモールブルー、チモールブルー、ブロムフェノールレット、フェノールレッド、ブロムクレゾールグリーンなどが使用可能であり、市販のアンモニア検査具に使用されている指示薬を用いることができる。
指示薬層の形状は全面積9〜49mm2のものが好ましく、特に25mm2のものが好適である。
As the indicator contained in the indicator layer, for example, bromthymol blue, thymol blue, bromophenollet, phenol red, bromocresol green and the like can be used, and an indicator used in a commercially available ammonia test device can be used.
Are preferable shape of the total area 9~49Mm 2 of the indicator layer, it is suitable in particular those of 25 mm 2.

本発明において、支持体上の指示薬層を被覆剤水溶液で形成された皮膜で被覆する方法は、特に限定されず、前記指示薬層を被覆剤水溶液中に60〜600秒間浸漬し、引き上げた後、室温下で24〜72時間風乾し作製する方法、あるいは、被覆剤水溶液を指示薬層上に滴下して指示薬層表面の全面がコートされたのを確認後、室温下で5〜60分間放置し、その後、室温下で24〜72時間風乾し作製する方法などを採用できる。   In the present invention, the method of coating the indicator layer on the support with the coating formed with the aqueous coating solution is not particularly limited. After the indicator layer is immersed in the aqueous coating solution for 60 to 600 seconds and pulled up, A method of air-drying for 24 to 72 hours at room temperature, or after dripping an aqueous coating solution onto the indicator layer and confirming that the entire surface of the indicator layer has been coated, leave it at room temperature for 5 to 60 minutes, Thereafter, a method of air-drying at room temperature for 24-72 hours can be employed.

被覆剤水溶液により形成される被覆剤皮膜は、乾燥質量が指示薬層の25〜50%、好ましくは28〜47%の範囲であり、これにより、1分程度の短時間で唾液中のアンモニアを希釈操作なく判定できる。乾燥質量が25%未満では、ブランクの色調(指示薬層)が、黄色からうす黄緑に変化し、視覚判定し難くなり、50%を超えると判定に要する時間が長くなって短時間での判定が困難になる。
更に、被覆剤皮膜の乾燥質量は1〜3mg、特に1.3〜2.6mgが好ましい。
なお、上記乾燥質量とは、指示薬層又は被覆剤皮膜を40℃で2日間乾燥させた後の質量である。
乾燥質量が上記範囲となる皮膜は、10〜38%の被覆剤(ポリビニルピロリドン)を含有する被覆剤水溶液を用いて皮膜を形成することで得ることができる。
The coating film formed by the aqueous coating solution has a dry mass in the range of 25 to 50%, preferably 28 to 47%, of the indicator layer, thereby diluting ammonia in saliva in a short time of about 1 minute. Judgment without operation If the dry mass is less than 25%, the color tone of the blank (indicator layer) changes from yellow to light yellowish green, making visual judgment difficult, and if it exceeds 50%, the judgment takes a long time and judgment takes a short time. Becomes difficult.
Further, the dry mass of the coating film is preferably 1 to 3 mg, particularly preferably 1.3 to 2.6 mg.
In addition, the said dry mass is a mass after drying an indicator layer or a coating film for 2 days at 40 degreeC.
A film having a dry mass within the above range can be obtained by forming a film using an aqueous coating solution containing 10 to 38% of a coating agent (polyvinylpyrrolidone).

本発明のアンモニア検査具の具体例を図1〜3に示す。図1,2は、スティック状の支持体1上に指示薬層2と担体(アルカリ層)3とを有するアンモニア検査紙(市販のアンモニア検査紙、アクアチェックA(商品名、バイエルメディカル(株)製)の指示薬層2が、本発明にかかわる被覆剤水溶液で形成された皮膜4で被覆されたものであり、図1は概略断面図、図2は分解斜視図である。更に、図1,2に示すアンモニア検査紙は、図3の分解斜視図に示すように、皮膜4上を唾液浸入防止カバー5で被覆し、唾液の浸入部位を限定してもよい。   Specific examples of the ammonia testing tool of the present invention are shown in FIGS. 1 and 2 show an ammonia test paper (commercially available ammonia test paper, Aqua Check A (trade name, manufactured by Bayer Medical Co., Ltd.) having an indicator layer 2 and a carrier (alkali layer) 3 on a stick-like support 1. 1) is coated with a coating 4 formed of the aqueous coating solution according to the present invention, Fig. 1 is a schematic sectional view, Fig. 2 is an exploded perspective view, and Figs. As shown in the exploded perspective view of FIG. 3, the ammonia test paper shown in FIG. 3 may be coated with a saliva intrusion prevention cover 5 to limit the saliva infiltration site.

本発明のアンモニア検査具は、試料の唾液を、被覆剤皮膜で被覆された指示薬層(判定部位)に滴下し、一定時間経過後に指示薬層の色調を判別することで、唾液中のアンモニアの存在の有無、あるいはアンモニアの濃度を定量することができる。   The ammonia test device of the present invention drops the sample saliva onto the indicator layer (determination site) coated with the coating film, and determines the color tone of the indicator layer after a certain period of time, whereby the presence of ammonia in the saliva The presence or absence of ammonia or the concentration of ammonia can be quantified.

検体に使用する唾液は、人の唾液、あるいは動物等の唾液であってもよく、安静時唾液、刺激唾液(ガムやワックスを咀嚼後、一定時間内に回収した唾液)、吐出唾液(一定量の蒸留水を口腔内に含み一定時間後に吐出した唾液)のいずれをも使用できる。   The saliva used for the specimen may be human saliva or animal saliva, resting saliva, stimulated saliva (saliva collected within a certain period of time after chewing gum or wax), discharged saliva (a certain amount) Any of the above-mentioned distilled water contained in the oral cavity and discharged after a predetermined time can be used.

唾液を用いた検査条件は特に制限されないが、本発明のアンモニア検査具と唾液2mLを、30秒間撹拌後、30〜120秒放置し、使用した市販のアンモニア検査具(例えばアクアチェックA等)の色見本を基準に判定することができる。判定は、唾液と接触反応させた後、30秒〜1分間で判定できる。   Although the test conditions using saliva are not particularly limited, the ammonia test tool of the present invention and 2 mL of saliva are stirred for 30 seconds and then left for 30 to 120 seconds, and the commercially available ammonia test tool used (for example, Aqua Check A) is used. The determination can be made based on the color sample. Determination can be performed in 30 seconds to 1 minute after contact reaction with saliva.

以下、実験例、実施例及び比較例を挙げて本発明をより詳細に説明するが、本発明はこれらの実施例に制限されるものではない。なお、下記例に示す%は特にことわらない限り質量%を意味する。   EXAMPLES Hereinafter, although an experimental example, an Example, and a comparative example are given and this invention is demonstrated in detail, this invention is not restrict | limited to these Examples. In the following examples, “%” means “% by mass” unless otherwise specified.

〔実験例〕
被覆剤に用いる成分として、表2に示す高分子化合物のカルボキシメチルセルロースナトリウムとポリビニルピロリドンについて、溶解性、溶液のpHを下記方法で調べた。結果を表2に示した。
[Experimental example]
As components used for the coating agent, the solubility of the polymer compounds carboxymethyl cellulose and polyvinyl pyrrolidone shown in Table 2 and the pH of the solution were examined by the following methods. The results are shown in Table 2.

溶解性の評価方法;
被覆剤は、高分子化合物(ポリビニルピロリドン又はカルボキシメチルセルロースナトリウム)の水溶液であり、調製時に、界面活性剤はじめpH調整剤を混合することができる。12時間スターラーで撹拌後、溶解性を視覚で判定し、下記基準で評価した。
○; 完全に溶解した
×; 不溶物が残った
pHの測定方法;
pHは、被覆剤水溶液中にpH電極(HORIBA社製 pHメーター D−51)を入れ、室温下のpH値を測定した。
Method for evaluating solubility;
The coating agent is an aqueous solution of a polymer compound (polyvinyl pyrrolidone or carboxymethyl cellulose sodium), and a surfactant and a pH adjuster can be mixed during preparation. After stirring with a stirrer for 12 hours, the solubility was visually determined and evaluated according to the following criteria.
○: Completely dissolved ×; Method for measuring pH of insoluble matter remaining;
For pH, a pH electrode (pH meter D-51, manufactured by HORIBA) was placed in the aqueous coating solution, and the pH value at room temperature was measured.

Figure 2010038666
Figure 2010038666

表2の結果から、唾液中のアンモニアを判定するには、適度な皮膜形成が必要であり、被覆剤の濃度を20%に調整して評価した結果、カルボキシメチルセルロースナトリウムは、ポリビニルピロリドンに比べ溶解性が悪く、アンモニア検査具の被覆剤に用いる高分子物質としてはポリビニルピロリドンが好適であることがわかった。   From the results in Table 2, it is necessary to form an appropriate film in order to determine ammonia in saliva. As a result of evaluating the concentration of the coating agent adjusted to 20%, sodium carboxymethylcellulose is dissolved compared to polyvinylpyrrolidone. It was found that polyvinyl pyrrolidone was suitable as a polymer material used for the coating material of the ammonia test device because of its poor properties.

〔実施例、比較例〕
市販のアンモニア検査紙、アクアチェックA(商品名、バイエルメディカル(株)製)の指示薬層(面積は5.2mm×5.2mm=27mm2、重量は5.2mg)を用い、また、被覆剤成分としてポリビニルピロリドン(BASFジャパン(株)製、ルビスコールK30、表中、PVPと略す。)、ラウリル硫酸ナトリウム(東邦化学工業(株)製、表中、SDSと略す。)、pH調整剤の10%酢酸水溶液又は10%リン酸水溶液を用い、表3に示す組成の被覆剤水溶液を調製し、下記方法で被覆剤処理したアンモニア検査紙を作製して評価した。結果を表4,5に示す。
Examples and comparative examples
A commercially available ammonia test paper, Aquacheck A (trade name, manufactured by Bayer Medical Co., Ltd.) is used as an indicator layer (area: 5.2 mm × 5.2 mm = 27 mm 2 , weight: 5.2 mg), and coating agent As ingredients, polyvinylpyrrolidone (BASF Japan Co., Ltd., Rubiscol K30, abbreviated as PVP in the table), sodium lauryl sulfate (Toho Chemical Industries, Ltd., abbreviated as SDS in the table), pH adjuster Using a 10% aqueous acetic acid solution or a 10% aqueous phosphoric acid solution, a coating aqueous solution having the composition shown in Table 3 was prepared, and an ammonia test paper treated with the coating by the following method was prepared and evaluated. The results are shown in Tables 4 and 5.

被覆剤処理アンモニア検査紙の調製;
表3に示す成分を水に溶解し、そのまま、あるいは10%酢酸水溶液や10%リン酸水溶液でpH調整して水溶液を調製した。
得られた被覆剤水溶液中に室温でアクアチェックAの指示薬層部分を60秒間浸漬し、その後、室温で2日間乾燥して、被覆剤処理検査紙を作製した。
作製した検査紙(実施例1〜4、比較例1〜5)の被覆剤組成、pHと、判定部位の全乾燥質量、被覆剤質量及び被覆率を表3にまとめて示した。なお、pHの測定法、判定部位の全乾燥質量及び被覆剤質量、被覆率の算出法は、下記のとおりである。
Preparation of coating-treated ammonia test paper;
The components shown in Table 3 were dissolved in water, and the aqueous solution was prepared as it was or by adjusting the pH with a 10% acetic acid aqueous solution or a 10% phosphoric acid aqueous solution.
The indicator layer portion of Aquacheck A was immersed in the resulting aqueous coating solution at room temperature for 60 seconds, and then dried at room temperature for 2 days to prepare a coating-treated inspection paper.
Table 3 summarizes the coating composition, pH, total dry mass, coating mass, and coverage of the prepared test papers (Examples 1-4, Comparative Examples 1-5). In addition, the measuring method of pH, the total dry mass and coating material mass of a determination part, and the calculation method of a coverage are as follows.

pHの測定方法;
pHは、被覆剤水溶液中にpH電極(HORIBA社製 pHメーター D−51)を入れ、室温下のpH値を測定した。
全乾燥質量(B);
検査紙の判定部位(被覆剤皮膜が形成された指示薬層)全体の乾燥質量
被覆剤質量(A);
被覆剤皮膜の乾燥質量
被覆率;
上記の全乾燥質量(B)、被覆剤質量(A)から下記式により検査紙の被覆率(指示薬層に対する被覆剤皮膜の乾燥質量の割合(質量比))を求めた。
被覆率(%)=(A/(B−A))×100
pH measurement method;
For pH, a pH electrode (pH meter D-51, manufactured by HORIBA) was placed in the aqueous coating solution, and the pH value at room temperature was measured.
Total dry mass (B);
Dry mass coating material mass (A) of the entire test paper judgment site (indicator layer on which the coating film is formed);
The dry mass coverage of the coating film;
From the above total dry mass (B) and coating mass (A), the coverage of the test paper (ratio (mass ratio) of the dry mass of the coating to the indicator layer) was determined.
Coverage (%) = (A / (BA)) × 100

Figure 2010038666
Figure 2010038666

唾液検体を用いたアンモニア検査紙によるアンモニア検出における反応時間の検討;
3名の成人被験者から採取した安静時唾液を検体とした。
次に、コントロールのアンモニア検査紙と、被覆剤で処理したアンモニア検査紙(実施例3)を用い、アンモニア検査紙の上に検体の唾液(安静時又は刺激時の唾液)2.0mLを滴下し、滴下から1分後と3分後のアンモニア検査紙の色の変化について、視覚判定した。視覚判定は、アクアチェックAの判定基準に従い、下記の視覚評価基準で行った。結果を表4に示す。
なお、本発明では、塩化アンモニウムのアンモニウムイオンが、アルカリ性で、ガス化により、被覆剤処理した皮膜層を通過し、指示薬層で発色する。その際、皮膜層のpHもガス化に作用しているものと考えられる。指示薬層では、アクアチェックAの中に含まれるpH指示薬がアンモニアガスと反応し、1分後の色の変化を視覚判定することで、唾液中のアンモニアを、希釈操作することなく測定ができる。
Examination of reaction time in ammonia detection with ammonia test paper using saliva specimens;
Resting saliva collected from three adult subjects was used as a specimen.
Next, using control ammonia test paper and ammonia test paper treated with a coating agent (Example 3), 2.0 mL of sample saliva (resting or stimulating saliva) was dropped onto the ammonia test paper. The change in the color of the ammonia test paper 1 minute and 3 minutes after the dropping was visually judged. The visual judgment was performed according to the following visual evaluation criteria in accordance with the criteria for Aqua Check A. The results are shown in Table 4.
In the present invention, ammonium ions of ammonium chloride are alkaline, pass through the coating layer treated with the gasification by gasification, and develop color in the indicator layer. At that time, it is considered that the pH of the coating layer also acts on gasification. In the indicator layer, the pH indicator contained in the aqua check A reacts with ammonia gas, and the color change after 1 minute is visually judged, whereby the ammonia in the saliva can be measured without diluting operation.

視覚評価基準(各判定基準におけるアンモニア濃度値、μg/mL);
アンモニア濃度の判定は、アンモニア検査紙とアンモニア標準液又は唾液を1分間反応させた後の色の変化を、アクアチェックAの基準色に従い、下記の6段階で視覚判定した。
− :黄色(0μg/mL) ± :うす黄緑(25μg/mL)
+ :黄緑(50μg/mL) ++ :うす緑(100μg/mL)
+++:緑(400μg/mL) ++++:深緑(900μg/mL)
Visual evaluation criteria (ammonia concentration value in each criterion, μg / mL);
The determination of the ammonia concentration was visually determined in the following 6 stages according to the standard color of Aqua Check A, the color change after the ammonia test paper and ammonia standard solution or saliva were reacted for 1 minute.
−: Yellow (0 μg / mL) ±: Light yellowish green (25 μg / mL)
+: Yellowish green (50 μg / mL) ++: Light green (100 μg / mL)
+++: Green (400 μg / mL) +++++: Dark green (900 μg / mL)

Figure 2010038666
Figure 2010038666

表4の結果から、被覆剤で処理したアンモニア検査紙は、3分後の判定ではアンモニア濃度400μg/mLと900μg/mLとの差に色の変化が認められず(いずれも++++)、視覚的な判定が難しいが、1分後を判定時間に設定すると、100μg/mLから900μg/mLまで色の変化が認められ、短時間かつ正確にアンモニア濃度を視覚判定できることがわかった。   From the results in Table 4, the test paper treated with the coating agent showed no color change in the difference between the ammonia concentration of 400 μg / mL and 900 μg / mL in the determination after 3 minutes (all were +++++), and was visually However, it was found that when 1 minute later was set as the determination time, a color change was recognized from 100 μg / mL to 900 μg / mL, and the ammonia concentration could be visually determined accurately in a short time.

アンモニア検査紙を用いた唾液検体中のアンモニアの検出;
表3に示す組成のアンモニア検査紙(実施例1〜4、比較例1〜5)について、まず、判定評価前のアンモニア検査紙の判定部位(指示薬層)の視覚判定を上記と同様の基準で行った。次に、上記と同様の検体を用いて同様の方法で、判定時間1分でアンモニア検出を行い、同様に評価した。また、検体として水を用いて同様に評価し、その判定結果をブランク値として示した。以上の結果を表5に示す。
Detection of ammonia in saliva samples using ammonia test paper;
For the ammonia test papers (Examples 1 to 4 and Comparative Examples 1 to 5) having the compositions shown in Table 3, first, the visual judgment of the judgment site (indicator layer) of the ammonia test paper before judgment evaluation is performed based on the same criteria as above. went. Next, ammonia was detected by the same method using the same sample as described above, with a determination time of 1 minute, and evaluated in the same manner. Moreover, it evaluated similarly using water as a test substance, and showed the determination result as a blank value. The results are shown in Table 5.

Figure 2010038666
Figure 2010038666

表5の結果から、コントロール検査紙(被覆剤処理なし)は、唾液中アンモニアと瞬時に反応し、1分後にはアンモニア濃度100μg/mLでも測定限界を超え、全ての濃度の視覚評価が++++(深緑)となり、判別できなかった。また、比較例1〜5は、被覆剤処理による遅延効果によりアンモニア濃度の違いで発色の変化が認められるが、アンモニア濃度400μg/mLと900μg/mLとの濃度で差が認められず、視覚判定できなかった。比較例1,2,4の検査紙は、検査前に検査紙がすでに着色しており、水を検体として検査した場合のブランク値にも増加が認められ、アンモニア濃度判定の精度に劣ることがわかった。   From the results in Table 5, the control test paper (without the coating treatment) reacted instantaneously with ammonia in saliva, and after 1 minute the ammonia concentration exceeded 100 μg / mL, and the visual evaluation of all concentrations was +++++ ( Dark green) and could not be identified. In Comparative Examples 1 to 5, a color change was observed due to the difference in ammonia concentration due to the delay effect due to the coating treatment, but no difference was observed between the ammonia concentrations of 400 μg / mL and 900 μg / mL. could not. In the test papers of Comparative Examples 1, 2, and 4, the test paper is already colored before the test, and an increase is also observed in the blank value when water is used as a specimen, which may be inferior in accuracy of ammonia concentration determination. all right.

これらに対して、本発明品(実施例)では、唾液検体と接触させて1分後という短時間で唾液中アンモニアの検出及びその濃度の定量判定が可能であり、ブランク値の増加も認められなかった。よって、本発明にかかわる被覆剤水溶液で被覆したアンモニア検査紙は、唾液を希釈することなく検体として用いて、唾液中のアンモニアを簡単かつ短時間で検出又はその濃度を測定して判定できることが確認できた。   On the other hand, in the products of the present invention (Examples), it is possible to detect ammonia in saliva and determine its concentration quantitatively in a short time of 1 minute after contact with a saliva sample, and an increase in the blank value is also observed. There wasn't. Therefore, it is confirmed that the ammonia test paper coated with the aqueous coating agent solution according to the present invention can be used as a specimen without diluting the saliva, and can detect ammonia in the saliva easily or in a short time by measuring or determining its concentration. did it.

次に、本発明のアンモニア検査具の他の実施例を示す。いずれの検査具も上記実施例と同様に唾液中のアンモニアの存在の有無又はその濃度を迅速かつ簡単に測定できるものであった。   Next, another embodiment of the ammonia test tool of the present invention will be shown. As with the above-described example, all the inspection tools were able to quickly and easily measure the presence or concentration of ammonia in saliva.

〔実施例5〕
被覆剤水溶液組成
ポリビニルピロリドン(ルビスコールK30) 26.0g
ラウリル硫酸ナトリウム 0.7g
pH調整剤(10%リン酸) 0.3mL
水 適量
計 100g
(pH2.0)
市販アンモニア検査紙(バイエルメディカル(株))の指示薬層(面積27mm2、重量5.2mg)を、上記被覆剤に1分間浸し、室温で2日間乾燥した。このときの全乾燥質量(B)は6.70mg、被覆剤質量(A)は1.50mgであり、指示薬層に対し被覆処理し、室温2日間乾燥したときの被覆率は28.8%であった。
Example 5
Coating aqueous solution composition Polyvinylpyrrolidone (Rubicol K30) 26.0 g
Sodium lauryl sulfate 0.7g
pH adjuster (10% phosphoric acid) 0.3mL
Appropriate amount of water
Total 100g
(PH 2.0)
Indicator layer of commercially available ammonia test paper (Bayer Medical Ltd.) (area 27 mm 2, weight 5.2 mg), immersed for one minute in the coating, and dried at room temperature for 2 days. The total dry mass (B) at this time was 6.70 mg, the coating agent mass (A) was 1.50 mg, and the coating rate when the indicator layer was coated and dried at room temperature for 2 days was 28.8%. there were.

〔実施例6〕
被覆剤水溶液組成
ポリビニルピロリドン(ルビスコールK30) 31.0g
ラウリル硫酸ナトリウム 0.7g
pH調整剤(10%酢酸) 0.3mL
水 適量
計 100g
(pH3.5)
市販アンモニア検査紙(バイエルメディカル(株))の指示薬層(面積27mm2、重量5.2mg)を、上記被覆剤に1分間浸し、室温で2日間乾燥した。このときの全乾燥質量(B)は7.10mg、被覆剤質量(A)は1.90mgであり、指示薬層に対し被覆処理し、室温2日間乾燥したときの被覆率は36.5%であった。
Example 6
Coating agent aqueous solution composition Polyvinylpyrrolidone (rubiscol K30) 31.0 g
Sodium lauryl sulfate 0.7g
pH adjuster (10% acetic acid) 0.3mL
Appropriate amount of water
Total 100g
(PH 3.5)
An indicator layer (area 27 mm 2 , weight 5.2 mg) of a commercially available ammonia test paper (Bayer Medical Co., Ltd.) was immersed in the coating agent for 1 minute and dried at room temperature for 2 days. The total dry mass (B) at this time was 7.10 mg, the coating agent mass (A) was 1.90 mg, and the coating rate when the indicator layer was coated and dried at room temperature for 2 days was 36.5%. there were.

〔実施例7〕
被覆剤水溶液組成
ポリビニルピロリドン(ルビスコールK30) 32.0g
ラウリル硫酸ナトリウム 1.0g
pH調整剤(10%酢酸) 0.4mL
水 適量
計 100g
(pH2.8)
市販アンモニア検査紙(バイエルメディカル(株))の指示薬層(面積27mm2、重量5.2mg)を、上記被覆剤に1分間浸し、室温で2日間乾燥した。このときの全乾燥質量(B)は7.10mg、被覆剤質量(A)は1.90mgであり、指示薬層に対し被覆処理し、室温2日間乾燥したときの被覆率は36.5%であった。
Example 7
Coating agent aqueous solution composition Polyvinylpyrrolidone (rubiscol K30) 32.0 g
Sodium lauryl sulfate 1.0g
pH adjuster (10% acetic acid) 0.4mL
Appropriate amount of water
Total 100g
(PH 2.8)
An indicator layer (area 27 mm 2 , weight 5.2 mg) of a commercially available ammonia test paper (Bayer Medical Co., Ltd.) was immersed in the coating agent for 1 minute and dried at room temperature for 2 days. The total dry mass (B) at this time was 7.10 mg, the coating agent mass (A) was 1.90 mg, and the coating rate when the indicator layer was coated and dried at room temperature for 2 days was 36.5%. there were.

〔実施例8〕
被覆剤水溶液組成
ポリビニルピロリドン(ルビスコールK30) 38.0g
ラウリル硫酸ナトリウム 0.7g
pH調整剤(10%酢酸) 0.1mL
水 適量
計 100g
(pH4.6)
市販アンモニア検査紙(バイエルメディカル(株))の指示薬層(面積27mm2、重量5.2mg)を、上記被覆剤に1分間浸し、室温で2日間乾燥した。このときの全乾燥質量(B)は7.60mg、被覆剤質量(A)は2.40mgであり、指示薬層に対し被覆処理し、室温2日間乾燥したときの被覆率は46.2%であった。
Example 8
Coating agent aqueous solution composition Polyvinylpyrrolidone (Rubicol K30) 38.0 g
Sodium lauryl sulfate 0.7g
pH adjuster (10% acetic acid) 0.1mL
Appropriate amount of water
Total 100g
(PH 4.6)
Indicator layer of commercially available ammonia test paper (Bayer Medical Ltd.) (area 27 mm 2, weight 5.2 mg), immersed for one minute in the coating, and dried at room temperature for 2 days. The total dry mass (B) at this time was 7.60 mg, the coating agent mass (A) was 2.40 mg, and the coating rate when the indicator layer was coated and dried at room temperature for 2 days was 46.2%. there were.

〔実施例9〕
被覆剤水溶液組成
ポリビニルピロリドン(ルビスコールK30) 18.0g
ポリビニルピロリドン(ルビスコールK60) 12.0g
ラウリル硫酸ナトリウム 1.0g
pH調整剤(10%リン酸) 0.2mL
水 適量
計 100g
(pH4.1)
市販アンモニア検査紙(バイエルメディカル(株))の指示薬層(面積27mm2、重量5.2mg)を、上記被覆剤に1分間浸し、室温で2日間乾燥した。このときの全乾燥質量(B)は7.11mg、被覆剤質量(A)は1.91mgであり、指示薬層に対し被覆処理し、室温2日間乾燥したときの被覆率は36.7%であった。
Example 9
Coating agent aqueous solution composition Polyvinylpyrrolidone (rubiscol K30) 18.0 g
Polyvinylpyrrolidone (Rubicol K60) 12.0g
Sodium lauryl sulfate 1.0g
pH adjuster (10% phosphoric acid) 0.2mL
Appropriate amount of water
Total 100g
(PH 4.1)
An indicator layer (area 27 mm 2 , weight 5.2 mg) of a commercially available ammonia test paper (Bayer Medical Co., Ltd.) was immersed in the coating agent for 1 minute and dried at room temperature for 2 days. The total dry mass (B) at this time was 7.11 mg and the coating agent mass (A) was 1.91 mg. The coating rate when the indicator layer was coated and dried for 2 days at room temperature was 36.7%. there were.

〔実施例10〕
被覆剤水溶液組成
ポリビニルピロリドン(ルビスコールK90) 28.0g
ラウリル硫酸ナトリウム 0.8g
pH調整剤(10%酢酸) 0.3mL
水 適量
計 100g
(pH3.5)
市販アンモニア検査紙(バイエルメディカル(株))の指示薬層(面積27mm2、重量5.2mg)を、上記被覆剤に1分間浸し、室温で2日間乾燥した。このときの全乾燥質量(B)は6.80mg、被覆剤質量(A)は1.60mgであり、指示薬層に対し被覆処理し、室温2日間乾燥したときの被覆率は30.7%であった。
Example 10
Coating aqueous solution composition Polyvinylpyrrolidone (rubiscol K90) 28.0 g
0.8g sodium lauryl sulfate
pH adjuster (10% acetic acid) 0.3mL
Appropriate amount of water
Total 100g
(PH 3.5)
An indicator layer (area 27 mm 2 , weight 5.2 mg) of a commercially available ammonia test paper (Bayer Medical Co., Ltd.) was immersed in the coating agent for 1 minute and dried at room temperature for 2 days. The total dry mass (B) at this time was 6.80 mg, and the coating agent mass (A) was 1.60 mg. The coating rate when the indicator layer was coated and dried at room temperature for 2 days was 30.7%. there were.

〔実施例11〕
被覆剤水溶液組成
ポリビニルピロリドン(ルビスコールK60) 28.0g
ラウリル硫酸ナトリウム 0.8g
セファデックスG−25 2.0g
pH調整剤(10%酢酸) 0.3mL
水 適量
計 100g
(pH3.5)
市販アンモニア検査紙(バイエルメディカル(株))の指示薬層(面積27mm2、重量5.2mg)を、上記被覆剤に1分間浸し、室温で2日間乾燥した。このときの全乾燥質量(B)は7.51mg、被覆剤質量(A)は2.31mgであり、指示薬層に対し被覆処理し、室温2日間乾燥したときの被覆率は44.5%であった。
Example 11
Coating agent aqueous solution composition Polyvinylpyrrolidone (rubiscol K60) 28.0 g
0.8g sodium lauryl sulfate
Sephadex G-25 2.0g
pH adjuster (10% acetic acid) 0.3mL
Appropriate amount of water
Total 100g
(PH 3.5)
An indicator layer (area 27 mm 2 , weight 5.2 mg) of a commercially available ammonia test paper (Bayer Medical Co., Ltd.) was immersed in the coating agent for 1 minute and dried at room temperature for 2 days. The total dry mass (B) at this time is 7.51 mg, the coating agent mass (A) is 2.31 mg, and the coating rate is 44.5% when the indicator layer is coated and dried at room temperature for 2 days. there were.

本発明のアンモニア検査具の一実施例を示す断面図である。It is sectional drawing which shows one Example of the ammonia test | inspection tool of this invention. 本発明のアンモニア検査具の一実施例を示す分解斜視図である。It is a disassembled perspective view which shows one Example of the ammonia test | inspection tool of this invention. 本発明のアンモニア検査具の他の一実施例を示す分解斜視図である。It is a disassembled perspective view which shows another Example of the ammonia test | inspection tool of this invention.

符号の説明Explanation of symbols

1 支持体
2 指示薬層
3 担体(アルカリ層)
4 皮膜(被覆剤)
5 唾液浸入防止カバー
1 Support 2 Indicator Layer 3 Carrier (Alkali Layer)
4 Film (coating material)
5 Saliva infiltration prevention cover

Claims (3)

支持体上に、アンモニアにより呈色反応する指示薬層を有するアンモニア検査具であって、前記指示薬層が、ポリビニルピロリドンと界面活性剤とを含有しpH2.0〜5.0(25℃)に調整された被覆剤水溶液で形成された皮膜で被覆されてなり、該皮膜の乾燥質量が指示薬層の25〜50質量%であり、唾液中のアンモニアを検出又は測定するためのものであることを特徴とするアンモニア検査具。   An ammonia tester having an indicator layer that reacts with ammonia on a support, wherein the indicator layer contains polyvinylpyrrolidone and a surfactant and is adjusted to pH 2.0 to 5.0 (25 ° C.). It is coated with a film formed with the aqueous coating agent solution, the dry mass of the film is 25 to 50% by mass of the indicator layer, and is for detecting or measuring ammonia in saliva Ammonia testing tool. 唾液中のアンモニアを検出又は測定して、口腔内の清潔度を推測するためのものである請求項1記載のアンモニア検査具。   The ammonia test tool according to claim 1, which is for detecting or measuring ammonia in saliva and estimating cleanliness in the oral cavity. 支持体上に、アンモニアにより呈色反応する指示薬層を有するアンモニア検査具の前記指示薬層を、ポリビニルピロリドンと界面活性剤とを含有しpH2.0〜5.0(25℃)に調整された被覆剤水溶液に浸漬後、乾燥させ、乾燥質量が指示薬層の25〜50質量%である皮膜で被覆して感度を調整することを特徴とする、唾液中のアンモニアを検出又は測定するためのアンモニア検査具の感度調整方法。   The said test substance layer of the ammonia test device which has the indicator layer which carries out a color reaction with ammonia on a support body contains polyvinylpyrrolidone and a surfactant and is adjusted to pH 2.0 to 5.0 (25 ° C.) Ammonia test for detecting or measuring ammonia in saliva, characterized by adjusting the sensitivity by dipping in an aqueous solution of the agent and then drying and coating with a film having a dry mass of 25 to 50% by mass of the indicator layer How to adjust the sensitivity of the tool.
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JP2012112880A (en) * 2010-11-26 2012-06-14 Kao Corp Method for confirming deodorization effect
JP2021511499A (en) * 2018-01-12 2021-05-06 メイヨ・ファウンデーション・フォー・メディカル・エデュケーション・アンド・リサーチ Systems and methods for the detection and quantification of ammonia and ammonium in fluids
CN114019087A (en) * 2021-10-18 2022-02-08 福建傲农生物科技集团股份有限公司 Method for measuring ammonia absorption amount of zeolite powder

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JP2006258560A (en) * 2005-03-16 2006-09-28 Fuji Photo Film Co Ltd Integrated multilayer analytical element for quantifying creatinine
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