JP5473514B2 - Dental curable material container - Google Patents
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- JP5473514B2 JP5473514B2 JP2009221193A JP2009221193A JP5473514B2 JP 5473514 B2 JP5473514 B2 JP 5473514B2 JP 2009221193 A JP2009221193 A JP 2009221193A JP 2009221193 A JP2009221193 A JP 2009221193A JP 5473514 B2 JP5473514 B2 JP 5473514B2
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本発明は、歯科用硬化性材料を収容する容器であって、温度履歴確認手段が配備されてなる該収容容器に関する。 The present invention relates to a container for storing a dental curable material, which is provided with a temperature history confirmation means.
歯科分野において、歯牙修復材料、歯科用接着剤、義歯床用材料、印象材料等の硬化性材料が広く使用されている。歯科用硬化性材料は、通常、重合性単量体、および重合開始剤の必須成分に、必要に応じて、フィラー、重合禁止剤、溶媒、顔料等が配合された重合性組成物からなる。上記各成分の配合目的は、以下のとおりである。 In the dental field, curable materials such as tooth restoration materials, dental adhesives, denture base materials, and impression materials are widely used. The dental curable material is usually composed of a polymerizable composition in which a filler, a polymerization inhibitor, a solvent, a pigment and the like are blended as necessary with a polymerizable monomer and essential components of a polymerization initiator. The compounding purpose of each of the above components is as follows.
重合性単量体は、マトリックスモノマーと機能性モノマーに大別される。このうちマトリックスモノマーは、重合して硬化体強度を高める性質を付与している。他方、機能性モノマーは、例えば、歯質との接着性を高める酸性基含有重合性単量体や、歯質との浸透性を高める水酸基含有重合性単量体が例示され、斯様に機能性官能基を備えることにより、硬化体に用途に応じた機能性を付与している。さらに、重合開始剤は、これら重合性単量体を重合し、歯科用硬化性材料を硬化する作用を有している。 The polymerizable monomer is roughly classified into a matrix monomer and a functional monomer. Of these, the matrix monomer is imparted with the property of being polymerized to increase the strength of the cured product. On the other hand, examples of the functional monomer include an acidic group-containing polymerizable monomer that increases adhesion to the tooth and a hydroxyl group-containing polymerizable monomer that increases the permeability to the tooth. By providing a functional functional group, the cured body is given functionality according to the application. Further, the polymerization initiator has a function of polymerizing these polymerizable monomers and curing the dental curable material.
歯科用硬化性材料を長期間保管した場合、これら構成成分の変性によって材料の劣化が生じることが避けられない。例えば、
・マトリックスモノマーが変性することにより、硬化体強度が低下する〔例えば、（メタ）アクリレート系重合性単量体における、エステル交換反応やエステル部分の加水分解反応〕。
・機能性モノマーが変性することにより、その用途に必要な機能性が失われる〔例えば、酸性基含有重合性単量体における、酸性基の加水分解反応〕。
・重合開始剤が変性することにより重合率が低下し、硬化体強度が低下する。また、硬化性材料の保管中に重合が開始され、ゲル化が生じる。
・フィラーの変性や分散性低下が生じることにより、操作性が低下し、硬化体強度が低下する。
・溶媒が揮発することにより、相分離等が生じ、操作性が低下する。
・上記いずれかの成分、またはその他の添加剤成分の変性により、前記劣化以外に、変色、臭気等の物理的変化が生じる。
等である。
When a dental curable material is stored for a long period of time, it is inevitable that the material will deteriorate due to the modification of these components. For example,
-When the matrix monomer is modified, the strength of the cured product is reduced [for example, transesterification reaction or hydrolysis reaction of an ester moiety in a (meth) acrylate polymerizable monomer].
-Modification of the functional monomer results in the loss of functionality necessary for the intended use (for example, hydrolysis reaction of acidic groups in acidic group-containing polymerizable monomers).
-When the polymerization initiator is modified, the polymerization rate decreases, and the cured product strength decreases. Further, polymerization starts during storage of the curable material, and gelation occurs.
-When the filler is modified or the dispersibility is lowered, the operability is lowered and the cured body strength is lowered.
-When the solvent is volatilized, phase separation or the like occurs, and operability decreases.
-Modification of any of the above components or other additive components causes physical changes such as discoloration and odor in addition to the above-described deterioration.
Etc.
こうした変性は、各成分の自己変化の他に、共存する複数成分の化学反応により生じることも多い。したがって、歯科用硬化性材料の製品形態は、構成成分の全てを一包装に混合するのではなく、共存可能な成分を、使用時まで分包しておき、使用時にこれらを一材に混合する形態もとられている。しかし、それでも、包装数が多いと操作ステップが多くなり商品価値を低下させるため、これを理想どおりに貫くことは難しく、保管方法の遵守を前提に、劣化に対する安全係数が必ずしも高くないもの同士も、同じ包装に配合することが、ある程度行われているのが実状である。 Such modification is often caused by a chemical reaction of a plurality of coexisting components in addition to the self-change of each component. Therefore, the product form of the dental curable material does not mix all the components in one package, but wraps the components that can coexist before use and mixes them into one material at the time of use. Form is taken. However, if the number of packages is large, the number of operation steps increases and the value of the product is reduced.Therefore, it is difficult to pass this as ideal, and there are some cases where the safety factor against deterioration is not necessarily high, assuming compliance with the storage method. In fact, it has been done to some extent in the same packaging.
以上から歯科用硬化性材料は、保管中に劣化した状態で患者に臨床適用してしまうリスクが心配され、できるだけ成分の変性が生じないように様々な回避処置が採られている。例えば、光により劣化する歯科用硬化性材料の遮光容器への収容、揮発性成分の蒸散防止のための容器の気密性向上等である（例えば、特許文献１）。また、品質保証期間や冷蔵保存等の保管条件を厳格に定めて対応している。 From the above, dental curable materials are concerned about the risk of being clinically applied to patients in a deteriorated state during storage, and various avoidance measures have been taken so that the components are not denatured as much as possible. For example, accommodation of a dental curable material that deteriorates due to light in a light-shielding container, improvement of hermeticity of the container for preventing evaporation of volatile components, and the like (for example, Patent Document 1). In addition, strict storage conditions such as quality assurance periods and refrigerated storage are stipulated.
しかしながら、冷蔵保存等の保管条件を厳格に定め、その遵守を徹底しても、個々の歯科医においてこれを完璧に守ることは困難である。また、製品の配送において、一時的に高温に曝されることも有り得る（特に、夏場の車中等）。 However, even if strict storage conditions such as refrigerated storage are strictly defined and strictly observed, it is difficult for individual dentists to keep them completely. In addition, the product may be temporarily exposed to high temperatures (particularly in a car in the summer).
したがって、こうした温度履歴を経た歯科用硬化性材料は、成分が変性し十分な性能が発揮できない可能性があるが、外観の観察でこれを正確に察知することは不可能に近かった。これら成分の劣化は、もちろん専門的な物理化学的分析によれば測定可能なものが多いが、高価な分析装置を個々の歯科医において買い揃えることは難しく、このため、歯科医院の現場では、使用して始めて、その歯科用硬化性材料の劣化に気づくことが常であった。場合によっては、劣化していること自体に気づかずそのまま使用し続ける問題も潜在していた。 Therefore, the dental curable material that has undergone such a temperature history may be unable to exhibit sufficient performance due to the modification of the components, but it has been almost impossible to accurately detect this by observation of the appearance. Of course, deterioration of these components is often measurable by professional physicochemical analysis, but it is difficult to purchase expensive analyzers at individual dentists. It was normal to notice the deterioration of the dental curable material only after use. In some cases, there is also a potential problem of continuing to use the product as it is without noticing the deterioration itself.
よって、歯科用硬化性材料の使用前にその材料が使用可能であるかを簡便に判定できれば、極めて有意義であった。 Therefore, if it was possible to easily determine whether the material can be used before using the dental curable material, it was extremely significant.
上記課題に鑑み、本発明者らは検討した結果、歯科用硬化性材料を収容する容器に温度履歴確認手段を配備することにより、上記の課題が解決できることを見出し、本発明を完成するに至った。 In view of the above problems, the present inventors have studied and found that the above problems can be solved by providing a temperature history confirmation means in a container containing a dental curable material, and the present invention has been completed. It was.
すなわち、本発明は、重合性組成物からなる歯科用硬化性材料を収容する容器であって、温度履歴確認手段として温度データロガーが配備され、収容される歯科用硬化性材料の温度と保管期間との関係を示すグラフや相関式が該容器の壁面に帖着したり添付されてなる歯科用硬化性材料収容容器である。 That is, the present invention is a container for storing a dental curable material made of a polymerizable composition, and a temperature data logger is provided as a temperature history confirmation means , and the temperature and storage period of the stored dental curable material Is a dental curable material storage container in which a graph and a correlation equation showing the relationship with the above are attached to or attached to the wall surface of the container.
この歯科用硬化性材料収容容器は、歯科用硬化性材料の充填容器であるのが好適である。 The dental curable material container is preferably a dental curable material filling container.
さらに、この歯科用硬化性材料収容容器は、歯科用硬化性材料を充填した充填容器を収容する外容器であるのが好適である。 Further, the dental curable material storage container is preferably an outer container for storing a filling container filled with a dental curable material.
上記歯科用硬化性材料は、歯牙修復材料、歯科用接着剤、義歯床用材料、印象材料から選ばれる材料であるのが好適である。 The dental curable material is preferably a material selected from a tooth restoration material, a dental adhesive, a denture base material, and an impression material.
本発明の収容容器によれば、収容される歯科用硬化性材料の劣化の有無またはその程度を、使用前に簡単に判別することができる。よって、保管中に品質が劣化した歯科用硬化性材料を、そのまま気づかずに使用する不利益が大幅に低減できる。 According to the storage container of the present invention, it is possible to easily determine whether or not the dental curable material to be stored is deteriorated or not before use. Therefore, the disadvantage of using a dental curable material whose quality has deteriorated during storage without being noticed can be greatly reduced.
本発明の歯科用硬化性材料収容容器には、温度履歴確認手段が配備されてなる。歯科用硬化性材料の劣化の原因になる構成成分の変性は、該材料が収容された容器が冷蔵保存されている限りは、その進行は極めて緩やかであり、少なくとも品質保証期間内であればその性能を低下させるような劣化が引き起こされるほどではない。しかし、該変性反応は一般的に温度依存性があり、保管温度が高まるにつれその変性速度は加速度的に高まり、常温を大きく越える温度に至ると、短時間保持されただけでも、硬化性材料の品質低下を顕著に生じせしめるのが普通である。したがって、その歯科用硬化性材料を収容する容器に温度履歴確認手段が配備されていると、その温度履歴を確認することにより、高温に曝されたかどうかで該材料の品質劣化の有無を簡単に判定することができる。 The dental curable material container of the present invention is provided with temperature history confirmation means. As long as the container in which the material is stored is refrigerated and stored, the progress of the modification of the constituent components causing the deterioration of the dental curable material is extremely slow, and at least within the quality assurance period, Not enough to cause degradation that degrades performance. However, the modification reaction is generally temperature-dependent, and as the storage temperature increases, the modification rate increases at an accelerated rate. It is normal to cause a significant decrease in quality. Therefore, when the temperature history confirmation means is provided in the container for storing the dental curable material, by checking the temperature history, it is possible to easily determine whether or not the quality of the material has deteriorated depending on whether it has been exposed to a high temperature. Can be determined.
温度履歴確認手段としては、小型の温度データロガーを使用する。温度データロガーは、温度センサーにより計測を行ってその計測結果を保存する電子計測器であり、ボタン型や方形型等の種々の形状のものがある。汎用品であっても、最も小さいもので直径（対角線）１ｃｍで厚み５ｍｍ程度の極小のものから市販されている。前記サーモラベルは基本的には歯科用硬化性材料が曝された最高温度しか確認できないのに対し、係る温度データロガーを使用した場合には、記録された温度データを読み取ることで、過去の温度履歴を知ることが可能である。したがって、以下で述べるように劣化の判定をより精緻に行うことができる。 The temperature history confirmation means, to use a small temperature data logger. The temperature data logger is an electronic measuring instrument that measures by a temperature sensor and stores the measurement result, and has various shapes such as a button type and a square type. Even a general-purpose product is commercially available from the smallest one having a diameter (diagonal line) of 1 cm and a minimum thickness of about 5 mm. The thermo label can basically only confirm the maximum temperature at which the dental curable material has been exposed, but when using such a temperature data logger, the recorded temperature data is read to obtain the past temperature. It is possible to know the history. Therefore, as described below, deterioration can be determined more precisely.
すなわち、予め、対象の歯科用硬化性材料の温度と劣化の関係を示すデータを取得しておき、これを温度データロガーに記録された温度の履歴データと比較すれば、歯科用硬化性材料の劣化の状態をより正確に判定できる。具体的には、その歯科用硬化性材料について、０℃から適当な高さの温度までを、所望の間隔（好適には５℃間隔）で温度を違えて、該物性値が、使用不可まで劣化（通常は、初期値の５〜７５％に低下）したと認められるに至る保管期間を夫々測定し、得られた保管温度と劣化期間の関係を先にグラフ化しておく。その上で、該歯科用硬化性材料が収用された容器の温度データロガーの記録データを読み取り、温度ごとの保管期間を求め、各温度での保管期間から、その温度ごとの劣化の進行程度を、前記保管温度と劣化期間の関係を示すグラフから算出し、これを積算することにより、該硬化性材料の劣化の進行程度の全貌をかなりの正確性で推測することができる。 That is, if the data indicating the relationship between the temperature and deterioration of the target dental curable material is acquired in advance and compared with the history data of the temperature recorded in the temperature data logger, the dental curable material The state of deterioration can be determined more accurately. Specifically, with respect to the dental curable material, the temperature is varied from 0 ° C. to an appropriate height at a desired interval (preferably at an interval of 5 ° C.) until the physical property value becomes unusable. The storage period until it is recognized that the deterioration (usually reduced to 5 to 75% of the initial value) is measured, and the relationship between the obtained storage temperature and the deterioration period is graphed first. After that, read the data recorded in the temperature data logger of the container in which the dental curable material was taken, obtain the storage period for each temperature, and from the storage period at each temperature, determine the degree of progress of deterioration for each temperature. By calculating from the graph showing the relationship between the storage temperature and the deterioration period and integrating the calculated values, it is possible to estimate the entire extent of the progress of deterioration of the curable material with considerable accuracy.
なお、上記の保管温度と劣化期間の関係は、グラフ化するだけでなく、アレニウスの式等の従来公知の予測式を使用して相関式化してもよい。この場合、物性値劣化の測定温度としては、０℃から１００℃までの範囲の中の任意の２点以上、好適には３点以上に減らして行うことが可能である。具体的には、測定された保管温度と劣化期間の関係を、保管温度を絶対温度表示でＴ（Ｋ）、劣化期間をｔ（単位は時間、日、週、年等任意）とし、ｌｏｇ（ｔ）と１／Ｔでプロットする。この形式で描いたアレニウスプロットが、式（１）の関係式を満たす場合に、測定に使用した以外の保管温度における劣化期間が、該式（１）より予測可能となる。
式（１）：ｌｏｇ（ｔ）＝a（１／Ｔ）＋ｂ （ａ、ｂは定数）
上記式（１）に対する各測定点の相関係数は０．８以上、好ましくは０．９以上、特に０．９５以上の場合に予測性が良好となり好ましい。
The relationship between the storage temperature and the deterioration period is not only graphed, but may be correlated using a conventionally known prediction formula such as the Arrhenius formula. In this case, the measurement temperature for deterioration of the physical property value can be reduced to any two or more points in the range from 0 ° C. to 100 ° C., preferably to three or more points. Specifically, the relationship between the measured storage temperature and the deterioration period is expressed as follows: log ((storage unit is arbitrary temperature, day, week, year, etc.) Plot at t) and 1 / T. When the Arrhenius plot drawn in this format satisfies the relational expression (1), the deterioration period at the storage temperature other than that used for the measurement can be predicted from the expression (1).
Formula (1): log (t) = a (1 / T) + b (a and b are constants)
When the correlation coefficient at each measurement point with respect to the above formula (1) is 0.8 or more, preferably 0.9 or more, particularly 0.95 or more, the predictability is good, which is preferable.
なお、歯科用硬化性材料収容容器には、斯様に予め作成する温度と保管期間との関係を示すグラフや相関式も、容器の壁面に帖着したり添付する。 Note that the dental curable material container, Such even previously created graphs and correlation equation showing a relationship between the temperature and duration of, you attach or Jogi on the wall of the container.
次に、本発明において、温度履歴確認手段を配備する、歯科用硬化性材料の収容容器について説明する。収容容器は、歯科用硬化性材料の充填容器であれば、該歯科用硬化性材料がペースト状の場合、壷、瓶、シリンジ等が挙げられる。他方、歯科用硬化性材料が液状の場合、投薬瓶、点眼瓶、カップ等が挙げられる。温度履歴確認手段である、温度データロガー等は、係る収容容器のいずれかの壁面に貼着すれば良い。容器が蓋付の場合、上記温度履歴確認手段は、該蓋部分に設けても良い。 Next, in the present invention, a container for a dental curable material provided with a temperature history confirmation means will be described. If the container is a container filled with a dental curable material, when the dental curable material is in a paste form, examples include a bag, a bottle, and a syringe. On the other hand, when the dental curable material is liquid, examples thereof include a prescription bottle, an eye drop bottle, and a cup. What is necessary is just to stick the temperature data logger etc. which are temperature history confirmation means to the wall surface in any one of the storage container which concerns. When the container has a lid, the temperature history confirmation means may be provided in the lid portion.
また、温度履歴確認手段は、斯様に歯科用硬化性材料の直接的な充填容器に帖着する以外に、こうした直接的な充填容器の複数個を収めた配送用の外容器、或いは同一の歯科治療に用いる他の歯科用薬剤や治具と詰め合わせたキット用外容器等に配備しても良い。このように外容器に配備する場合、箱状の外容器の外壁面に帖着しても良いし、内壁面に帖着しても良い。無論、この場合も容器が蓋付であれば、温度履歴確認手段は、該蓋部分に設けても良い。さらに、外容器がキット用外容器の場合、収容される付属器具類、例えば塗布用筆や各種インスツルメント類の側部に帖着して設けても良い。 In addition, the temperature history confirmation means is not only attached to the direct filling container of the dental curable material as described above, but also an outer container for delivery containing a plurality of such direct filling containers, or the same You may arrange | position to the outer container for kits etc. which were packed with other dental chemical | medical agents and jigs used for dental treatment. When deploying to the outer container in this way, it may be attached to the outer wall surface of the box-shaped outer container or may be attached to the inner wall surface. Of course, in this case, if the container has a lid, the temperature history confirmation means may be provided in the lid portion. Furthermore, when the outer container is an outer container for a kit, the outer container may be attached to a side portion of an accessory to be accommodated, for example, a coating brush or various instruments.
本発明の容器に収容される歯科用硬化性材料は、通常は、重合性単量体、および重合開始剤の必須成分に、必要に応じて、フィラー、重合禁止材、溶媒、顔料等が配合された重合性組成物が対象になる。こうした重合組成物からなる歯科用硬化性材料としては、コンポジットレジン等の歯牙修復材料、接着性レジンセメント、グラスアイオノマーセメント、ボンディング材等の歯科用接着剤、即時重合レジンや裏装材等の義歯床用材料、シリコーン印象材、アルジネート系印象材等の印象材料が例示できる。その他、歯科用硬化性材料は、歯科用プライマー等の歯科用前処理剤、ユージノール系仮封材や仮着材等の重合性単量体の重合により硬化する以外の硬化性材料であって良い。 The dental curable material accommodated in the container of the present invention usually contains a filler, a polymerization inhibitor, a solvent, a pigment, etc., as necessary, in the essential components of the polymerizable monomer and the polymerization initiator. The obtained polymerizable composition is an object. Dental curable materials made of such polymerized compositions include dental restoration materials such as composite resins, adhesive resins such as adhesive resin cements, glass ionomer cements and bonding materials, and dentures such as immediate polymerization resins and lining materials. Examples include impression materials such as flooring materials, silicone impression materials, and alginate-based impression materials. In addition, the dental curable material may be a curable material other than that cured by polymerization of a polymerizable monomer such as a dental pretreatment agent such as a dental primer, eugenol-based temporary sealing material or temporary bonding material. .
以下に実施例を挙げて本発明を具体的に説明するが、本発明はこれら実施例に限定されるものではない。 EXAMPLES The present invention will be specifically described below with reference to examples, but the present invention is not limited to these examples.
尚、実施例で実施した象牙質の接着強度測定方法は以下の方法によるものである。 The method for measuring the bond strength of dentin implemented in the examples is as follows.
〔象牙質の接着強度測定方法〕
屠殺後２４時間以内に牛前歯を抜去し、注水下、＃６００のエメリーペーパーで唇面に平行になるように象牙質平面を削り出した。次に、これらの面に圧縮空気を約１０秒間吹き付けて乾燥した後、象牙質平面に直径３ｍｍの孔の開いた両面テープを固定し、ついで厚さ０．５ｍｍ直径８ｍｍの孔の開いたパラフィンワックスを上記円孔上に同一中心となるように固定して模擬窩洞を形成した。この模擬窩洞内に、実施例に記載の歯科用接着剤を塗布し、２０秒間放置後、圧縮空気を約１０秒間吹き付けて乾燥し、歯科用可視光照射器（トクソーパワーライト、トクヤマデンタル社製）にて１０秒間光照射した。更にその上に歯科用コンポジットレジン（エステライトＰクイック、トクヤマデンタル社製）を充填し、可視光線照射器により１０秒間光照射して、接着試験片を作製した。その後、レジンセメント（ビスタイトＩＩ、トクヤマデンタル社製）を用いて、コンポジットレジン上に金属製アタッチメントを接着した。接着試験は、上記接着試験片を３７℃の水に２４時間浸漬後、引張り試験機（オートグラフ、島津製作所製）を用いてクロスヘッドスピード２ｍｍ／ｍｉｎにて引張り、象牙質とコンポジットレジンの引張り接着強度を測定することにより実施した。１試験当り、４本の引張り接着強さを上記方法で測定し、その平均値を接着強度として測定した。
[Method of measuring bond strength of dentin]
Within 24 hours after slaughter, the front teeth of the cow were removed, and the dentinal plane was cut out with water through # 600 emery paper so that it was parallel to the labial surface. Next, the surface was dried by blowing compressed air for about 10 seconds, and then a double-sided tape with a hole having a diameter of 3 mm was fixed to the dentin plane, and then a paraffin having a hole with a thickness of 0.5 mm and a diameter of 8 mm was formed. A simulated cavity was formed by fixing the wax so as to be in the same center on the circular hole. In this simulated cavity, the dental adhesive described in the example was applied, allowed to stand for 20 seconds, dried by blowing compressed air for about 10 seconds, and then a dental visible light irradiator (Tokuso Power Light, Tokuyama Dental Co., Ltd.) For 10 seconds. Further, a dental composite resin (Estellite P Quick, manufactured by Tokuyama Dental Co., Ltd.) was filled thereon, and irradiated with a visible light irradiator for 10 seconds to produce an adhesion test piece. Thereafter, a metal attachment was bonded onto the composite resin using resin cement (Bistite II, manufactured by Tokuyama Dental Co., Ltd.). In the adhesion test, the above-mentioned adhesion test piece was immersed in water at 37 ° C. for 24 hours and then pulled at a crosshead speed of 2 mm / min using a tensile tester (Autograph, manufactured by Shimadzu Corporation), and the dentin and the composite resin were pulled. The measurement was performed by measuring the adhesive strength. Four tensile bond strengths per test were measured by the above method, and the average value was measured as the bond strength.
参考例１
歯科用接着材として、１０質量部の２，２−ビス（４−（２−ヒドロキシ−３−メタクリルオキシプロポキシ）フェニル）プロパン、１０質量部の２−ヒドロキシエチルメタクリレート、１５質量部のトリエチレングリコールジメタクリレート、２５質量部の２−メタクリロイルオキシエチルジハイドロジェンホスフェートとビス（２−メタクリロイルオキシエチル）ハイドロジェンホスフェートの混合物、１０質量部の水、１００質量部のアセトン、５質量部のヒュームドシリカ、０．５質量部のカンファーキノン、０．５質量部のｐ−Ｎ，Ｎ−ジメチルアミノ安息香酸エチル、０．１質量部のヒドロキノンモノメチルエーテルを含む液状の歯科用接着材を調製した。この歯科用接着材について、前記方法により象牙質接着強度を測定したところ、象牙質への接着強度は１５ＭＰａであった。
Reference example 1
As a dental adhesive, 10 parts by weight of 2,2-bis (4- (2-hydroxy-3-methacryloxypropoxy) phenyl) propane, 10 parts by weight of 2-hydroxyethyl methacrylate, 15 parts by weight of triethylene glycol Dimethacrylate, a mixture of 25 parts by weight of 2-methacryloyloxyethyl dihydrogen phosphate and bis (2-methacryloyloxyethyl) hydrogen phosphate, 10 parts by weight of water, 100 parts by weight of acetone, 5 parts by weight of fumed silica A liquid dental adhesive containing 0.5 parts by weight of camphorquinone, 0.5 parts by weight of ethyl p-N, N-dimethylaminobenzoate and 0.1 parts by weight of hydroquinone monomethyl ether was prepared. About this dental adhesive, when the dentin adhesive strength was measured by the said method, the adhesive strength to dentin was 15 MPa.
この歯科用接着材を点眼瓶状容器に充填し、この点眼瓶状容器を０℃か６５℃まで５℃間隔で温度を違えた各温度で、湿度４０％の暗所中に２日間保管し、それぞれについて再度、象牙質接着強度を測定した。結果は、０℃保管の接着強度は１５ＭＰａのままであったものの、５５℃保管から接着強度の低下が顕著化し初め、６０℃保管のものでその接着力は１３ＭＰａになり、上記０℃保管のものに比べて接着強度は１０％を下回るに至っていた。 The dental adhesive is filled in an eye drop bottle container, and the eye drop bottle container is stored at a temperature of 5 ° C. every 0 ° C. or 65 ° C. in a dark place with a humidity of 40% for 2 days. Again, the dentin bond strength was measured for each. As a result, although the adhesive strength at 0 ° C. storage remained at 15 MPa, the decrease in the adhesive strength began to become noticeable from 55 ° C. storage, and the adhesive strength at 13 ° C. was 13 MPa. The adhesive strength was less than 10% compared to that.
上記結果を元に、この歯科用接着材の劣化の閾値温度は６０℃であると決定し、この温度で赤色から白色に変色するサーモラベルを用意した（発色までに要する時間は４８時間のもの）。そして、このサーモラベルを図１に示すようにボトル本体部の周壁面に帖着した点眼瓶状容器を用意し、これに上記歯科用接着材を充填した。この点眼瓶状容器について、夏場の車内に５日間放置した。その後、サーモラベルの表示を確認したところ、サーモラベルは白色に変色しており、点眼瓶状容器内に収容した歯科用接着材が６０℃以上の高温に４８時間以上曝されたことがわかった。この点眼瓶状容器に充填された歯科用接着材について、象牙質接着強度を測定したところ接着強度は１２ＭＰａに低下していた。 Based on the above results, it was determined that the threshold temperature for degradation of this dental adhesive was 60 ° C., and a thermolabel that changed from red to white at this temperature was prepared (the time required for color development was 48 hours) ). Then, as shown in FIG. 1, an eye-drop bottle-like container was prepared in which the thermolabel was attached to the peripheral wall surface of the bottle body, and this was filled with the dental adhesive. This ophthalmic bottle-like container was left in a car in summer for 5 days. Then, when the display of the thermo label was confirmed, the thermo label was discolored in white, and it was found that the dental adhesive contained in the eye drop bottle was exposed to a high temperature of 60 ° C. or more for 48 hours or more. . When the dentin adhesive strength was measured for the dental adhesive filled in the eye drop bottle-like container, the adhesive strength was reduced to 12 MPa.
実施例１
参考例１で用いた歯科用接着材が充填された各点眼瓶状容器について、湿度４０％の暗所中、５０℃、４５℃、４０℃でそれぞれ保管し、各温度において、歯科用接着材の初期の接着強度１５ＭＰａのから２０％減少した閾値（１２ＭＰａ）未満となるまでの保管可能期間を調べたところ、５０℃では１９日、４５℃では３０日、４０℃では５２日を要する結果であった。
この各温度での保存可能期間から、アレニウスプロットを行なったところ、
式Ａ：ｌｏｇ（ｔ（日））＝１０１８３（１／Ｔ）−２８．６
が得られた。上式より１０℃（Ｔ＝２８３Ｋ）における保管可能期間は１６１７日間（４．４年）、２５℃（Ｔ＝２９８Ｋ）における保管可能期間は２６４日間（０．７年）と予測された。
Example 1
Each ophthalmic container filled with the dental adhesive used in Reference Example 1 is stored at 50 ° C., 45 ° C., and 40 ° C. in a dark place with a humidity of 40%, and the dental adhesive is used at each temperature. As a result of examining the storage possible period from the initial adhesive strength of 15 MPa to a threshold value (12 MPa) decreased by 20%, it took 19 days at 50 ° C, 30 days at 45 ° C, and 52 days at 40 ° C. there were.
From the storage period at each temperature, an Arrhenius plot was performed.
Formula A: log (t (days)) = 10183 (1 / T)-28.6
was gotten. From the above formula, the storage period at 10 ° C. (T = 283K) was predicted to be 1617 days (4.4 years), and the storage period at 25 ° C. (T = 298K) was predicted to be 264 days (0.7 years).
次に、上記歯科用接着材が充填された点眼瓶状容器、およびこれと組合わせて使用する歯科用硬化性材料（エステライトＰクイック、トクヤマデンタル社製）が充填されたシリンジ状容器、さらには塗布用筆（マイクロブラシ５０本入りでプラスチック容器に収納）とを、図２に示したキット用外容器に詰め合わせ、該キット用外容器の外壁面に温度データロガーを帖着した。この歯科用接着材キットを、本来冷蔵保存であるところ、２０〜３０℃に大まかに雰囲気が調整されている倉庫に手違いで、１００日間放置された設定で保管した。平均湿度は約４０％であった。 Next, an ophthalmic bottle-shaped container filled with the dental adhesive, and a syringe-shaped container filled with a dental curable material (Estellite P Quick, manufactured by Tokuyama Dental Co., Ltd.) used in combination therewith, Was packed with an application brush (with 50 microbrushes and stored in a plastic container) in the outer container for kit shown in FIG. 2, and a temperature data logger was attached to the outer wall surface of the outer container for kit. This dental adhesive kit was originally stored in a refrigerator, and was stored in a warehouse where the atmosphere was roughly adjusted to 20 to 30 ° C. and was left in a setting that was left for 100 days. The average humidity was about 40%.
１００日経過後、温度データロガーの測定値を解析したところ、実際の最高気温は３２℃であり、最低気温は２４℃であった。３２℃（３０５Ｋ）での保管期間は約７日間、３１℃（３０４Ｋ）での保管期間は約１０日間、３０℃（３０３Ｋ）での保管期間は約１２日間、２９℃（３０２Ｋ）での保管期間は約２５日間、２８℃（３０１Ｋ）での保管期間は約１８日間、２７℃（３００Ｋ）での保管期間は約１２日間、２６℃（２９９Ｋ）での保管期間は約６日間、２５℃（２９８Ｋ）での保管期間は約５日間、２４℃（２９７Ｋ）での保管期間は約５日間であった。 When the measured value of the temperature data logger was analyzed after 100 days, the actual maximum temperature was 32 ° C. and the minimum temperature was 24 ° C. Storage at 32 ° C (305K) is about 7 days, storage at 31 ° C (304K) is about 10 days, storage at 30 ° C (303K) is about 12 days, storage at 29 ° C (302K) Period is about 25 days, storage period at 28 ° C (301K) is about 18 days, storage period at 27 ° C (300K) is about 12 days, storage period at 26 ° C (299K) is about 6 days, 25 ° C The storage period at (298 K) was about 5 days, and the storage period at 24 ° C. (297 K) was about 5 days.
一方、２４℃〜３２℃における１℃刻みの各温度における歯科用接着材の各保管可能期間ｔｉ０は、前記式Ａを使って表１のようにそれぞれ計算される。よって、例えば３２℃に保管された期間が７日間であったことにより、歯科用接着材は、その保管期間の０．０５８倍（５．８％）（ｔｉ／ｔｉ０＝７／１２１により算出）が消費されたと算出できた。これらにより、２４℃〜３２℃におけるΣ（ｔｉ／ｔｉ０）は０．５７５であり、１００日間の保管により約５８％（１５２日（２６４日×０．５７５））もの保管可能期間の消費に当る劣化が進行したことが予測できた。 On the other hand, each storable period t i0 of the dental adhesive at each temperature in increments of 1 ° C. from 24 ° C. to 32 ° C. is calculated using Table A as shown in Table 1. Therefore, for example, since the period of storage at 32 ° C. was 7 days, the dental adhesive was 0.058 times (5.8%) of the storage period (t i / t i0 = 7/121 ) Calculation) was consumed. As a result, Σ (t i / t i0 ) at 24 ° C. to 32 ° C. is 0.575, and consumption for a storage period of about 58% (152 days (264 days × 0.575)) by storage for 100 days. It was possible to predict that the deterioration that occurred was advancing.
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