JP2022190418A - Dental resin material, and antibacterial artificial tooth - Google Patents
Dental resin material, and antibacterial artificial tooth Download PDFInfo
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- 239000004851 dental resin Substances 0.000 title claims abstract description 66
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- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical class [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 111
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Abstract
Description
特許法第３０条第２項適用申請有り 令和２年６月３０日発行の「神奈川歯科大学学会雑誌」第５５巻 第１号、第５７～６７頁にて公開 令和３年１月１日発行の「アポロニア２１」 Ｊａｎ．２０２１ Ｎｏ．３２５、第８８～９２頁にて公開Applied for the application of Article 30, Paragraph 2 of the Patent Act Published on June 30, 2020, "Journal of Kanagawa Dental University" Vol. 55, No. 1, pages 57-67 January 1, 2020 "Apollonia 21" published by Japan Jan. 2021 No. 325, published on pages 88-92
本発明は、歯科用樹脂材料及び抗菌性義歯に関する。 The present invention relates to a dental resin material and an antibacterial denture.
歯科領域の二大疾患である齲蝕と歯周病は、いずれも口腔常在菌により惹起されることが明らかにされている。即ち、ミュータンス連鎖球菌をはじめとする口腔常在菌とそれらの代謝産物によって構成されるプラーク細菌が齲蝕誘発の直接的原因であり、Ｐｏｒｐｈｙｒｏｍｏｎａｓ ｇｉｎｇｉｖａｌｉｓをはじめとする嫌気性グラム陰性菌の歯肉縁下における増殖が歯肉の炎症あるいは歯周組織破壊の原因となる。従って、プラークを構成する細菌の増殖を抑制することがこれらの疾患の予防に重要であることは明らかである。 Caries and periodontal disease, two major diseases in the dental field, have been clarified to be caused by oral bacteria. That is, plaque bacteria composed of oral resident bacteria such as Streptococcus mutans and their metabolites are the direct cause of caries induction, and anaerobic Gram-negative bacteria such as Porphyromonas gingivalis are in the subgingival gingiva. Proliferation in the gingiva causes gingival inflammation or periodontal tissue destruction. Therefore, it is clear that suppressing the growth of plaque-constituting bacteria is important for the prevention of these diseases.
また、義歯性口内炎は、義歯や床矯正装置などの可撤性床装置と関連した床下粘膜の炎症であり、口腔内の微生物が深く関わり、義歯床粘膜面にみられるＣａｎｄｉｄａ ａｂｉｃａｎｓを主体とするデンチャープラークが義歯性口内炎の重要な因子であることが報告されている。デンチャープラークの主要構成菌は、通性嫌気性グラム陽性球菌と通性嫌気性グラム陽性桿菌であると報告されている。また、義歯性口内炎とＣａｎｄｉｄａ及びＳｔａｐｈｙｌｏｃｏｃｃｕｓとの相関や、デンチャープラーク中から高頻度にＣａｎｄｉｄａ ａｌｂｉｃａｎｓを主体とするＣａｎｄｉｄａ属の菌種が検出されることが報告されている。 In addition, denture stomatitis is an inflammation of the subfloor mucosa associated with removable floor appliances such as dentures and orthodontic appliances. Microorganisms in the oral cavity are deeply involved. Denture plaque has been reported to be an important factor in denture stomatitis. The major constituents of denture plaque are reported to be facultative anaerobic Gram-positive cocci and facultative anaerobic Gram-positive bacilli. In addition, it has been reported that there is a correlation between denture stomatitis and Candida and Staphylococcus, and that Candida albicans, which is the main constituent, is frequently detected in denture plaques.
デンチャープラークの為害性として、義歯性口内炎や口角炎等の生体に対する為害作用のみならず、義歯材料への侵入やこれに伴う義歯材料の劣化に伴いデンチャープラークの堆積が助長され、さらなる義歯性口内炎等の増悪が懸念される。 The harmful effects of denture plaque include not only denture stomatitis and angular stomatitis, but also denture stomatitis and denture stomatitis. There is concern about aggravation such as
特に、樹脂を成形した義歯の周囲は細菌が繁殖しやすい環境であり、齲蝕原因菌や歯周病原因菌が口腔内に存在すると、義歯の周囲は特にこれらの細菌が繁殖しやすく、義歯周辺の健康な歯が損なわれる原因ともなる。また、歯周病患者は、歯周病原因菌によって生産されるメチルメルカプタン等による強い口臭を有することが多い。そのため、義歯を常に清潔に保持する必要がある。 In particular, the area around resin-molded dentures is an environment where bacteria can easily grow. It also causes damage to the healthy teeth of many. In addition, periodontal disease patients often have strong bad breath due to methyl mercaptan and the like produced by periodontal disease-causing bacteria. Therefore, it is necessary to keep the dentures clean at all times.
しかしながら、例えば、自分では義歯の清掃ができない高齢者等は、介助者による手助けが必要であるが、介助者がいなかったり、必ずしも行き届いた清掃ができなかったりという状況もある。義歯の清掃を怠ると、免疫力が低下した高齢者等では、口腔内の細菌や食物の残りかすが気管にはいって誤嚥性肺炎を発症する危険性が高くなる。義歯を清潔に保つことは、齲蝕や歯周病の予防だけでなく誤嚥性肺炎などの予防にもつながる。 However, for example, elderly people who cannot clean their dentures by themselves need help from a caregiver, but there are situations in which there is no caregiver or they cannot always clean their dentures thoroughly. If cleaning of dentures is neglected, there is an increased risk of aspiration pneumonia caused by bacteria in the oral cavity and leftover food particles entering the trachea in elderly people with weakened immune systems. Keeping dentures clean not only prevents caries and periodontal disease but also prevents aspiration pneumonia.
そこで、義歯を形成する樹脂に有機系抗菌剤組成物を均一混合して成形した義歯が提案され、主要な歯周病原因菌や齲蝕原因菌を長期に渡って抑制できることが報告されている（特許文献１）。 Therefore, it has been proposed to form dentures by uniformly mixing an organic antibacterial agent composition into a denture-forming resin, and it has been reported that major periodontal disease-causing bacteria and caries-causing bacteria can be inhibited over a long period of time ( Patent document 1).
一方、抗菌活性を示し、かつ人体に対して安全な無機材料としては、銀や酸化チタン、酸化マグネシウム、酸化カルシウム、酸化亜鉛等が知られている。衛生管理製品や繊維製品の分野では、樹脂組成物に抗菌性や殺菌性を付与した製品の開発・研究が行われている。歯科領域では、今後の超高齢化社会を見据えた全身管理との関係においても、口腔細菌の増殖を長期に阻害する歯科材料の開発は必須であると考えられる。 On the other hand, silver, titanium oxide, magnesium oxide, calcium oxide, zinc oxide, and the like are known as inorganic materials that exhibit antibacterial activity and are safe for the human body. In the fields of sanitary products and textile products, research and development are being conducted on products obtained by imparting antibacterial and bactericidal properties to resin compositions. In the field of dentistry, it is considered essential to develop dental materials that inhibit the growth of oral bacteria for a long period of time, even in relation to systemic management in anticipation of the future super-aging society.
酸化亜鉛は、光触媒活性、紫外線吸収活性、殺菌、抗菌、消臭等の機能を有することが知られている。
特許文献２及び３には、酸化亜鉛粉末の表面に表面処理を施して酸化亜鉛の光触媒活性を抑制し、紫外線吸収活性、殺菌、抗菌、消臭等の機能を維持した表面処理酸化亜鉛粉末が開示されている。
Zinc oxide is known to have functions such as photocatalytic activity, ultraviolet absorption activity, sterilization, antibacterial and deodorant properties.
本発明は、歯科用樹脂材料として使用可能な機械的特性及び化学的特性を備え、歯周病原因菌、齲蝕原因菌、真菌等に対する持続的な抗菌性を有し、デンチャープラークの付着を抑制できる、又はメチルメルカプタン等の口臭原因物質を低減することができる歯科用樹脂材料、及びそれを用いて作製される歯科用物品、特に抗菌性義歯を提供することを主たる目的とする。 The present invention has mechanical and chemical properties that can be used as a dental resin material, has persistent antibacterial properties against periodontal disease-causing bacteria, cariogenic bacteria, fungi, etc., and suppresses adhesion of denture plaque. It is a main object of the present invention to provide a dental resin material capable of reducing halitosis-causing substances such as methyl mercaptan, and dental articles, particularly antibacterial dentures, made using the same.
本発明者らは、人体に対して安全であり、一般的な細菌に対して有効な無機系抗菌剤として知られる酸化亜鉛粉末の表面を改質して、樹脂中での分散性を向上させた表面改質酸化亜鉛粉末が歯周病原因菌、齲蝕原因菌、真菌等の口腔内細菌に対しても抗菌性を示すことを見出した。 The present inventors improved the dispersibility in resin by modifying the surface of zinc oxide powder, which is known as an inorganic antibacterial agent that is safe for the human body and effective against common bacteria. It was found that the surface-modified zinc oxide powder also exhibits antibacterial properties against oral bacteria such as periodontal disease-causing bacteria, cariogenic bacteria, and fungi.
前述した有機系抗菌剤組成物を用いた抗菌性義歯は、口腔内で長期に渡って唾液等にさらされることで、特に義歯表面近くに存在する有機系抗菌剤化合物の分解が進み、義歯の抗菌性が低下する懸念がある。これに対し無機系抗菌剤は口腔内でも分解することがなく、長期に渡って抗菌性が持続するという利点を有する。 Antibacterial dentures using the above-mentioned organic antibacterial agent composition are exposed to saliva and the like in the oral cavity for a long period of time, and the decomposition of the organic antibacterial agent compounds present near the denture surface progresses, and the dentures become damaged. There is a concern that the antibacterial properties will decrease. On the other hand, inorganic antibacterial agents do not decompose even in the oral cavity, and have the advantage of maintaining antibacterial properties over a long period of time.
本発明者らは、歯科で用いられる樹脂、特に義歯形成用の樹脂に表面改質酸化亜鉛粉末を均一に分散させて成形した抗菌性を有する歯科用樹脂材料、それを用いて作製される抗菌性義歯を完成させた。 The present inventors have developed an antibacterial dental resin material that is formed by uniformly dispersing surface-modified zinc oxide powder in a resin used in dentistry, particularly a resin for forming dentures, and an antibacterial resin material produced using the same. completed the denture.
また、本発明者らは、前記表面改質酸化亜鉛粉末を含有する樹脂からなる歯科用樹脂材料が、歯周病患者の強い口臭の原因物質であるメチルメルカプタン等を低減できることを見出した。 In addition, the present inventors have found that a dental resin material comprising a resin containing the surface-modified zinc oxide powder can reduce methyl mercaptan and the like, which are causative agents of strong bad breath in patients with periodontal disease.
さらに、本発明者らは、前記表面改質酸化亜鉛粉末を含有する樹脂からなる歯科用樹脂材料が、デンチャープラークの原因となる細菌の付着を抑制することも見出した。 Furthermore, the present inventors have also found that a dental resin material comprising a resin containing the surface-modified zinc oxide powder suppresses adhesion of bacteria that cause denture plaque.
長期又は長時間に渡って口腔内に配置される歯科用物品、特に義歯が、抗菌性を有するだけでなく、メチルメルカプタン等の強い口臭の原因物質を分解したり、デンチャープラークの付着を抑制する機能を有することで、歯周病等の悪化を抑制し、口臭を低減することが期待できる。 Dental articles, especially dentures, which are placed in the oral cavity for a long time or for a long time, not only have antibacterial properties, but also decompose strong bad breath causative substances such as methyl mercaptan and suppress adhesion of denture plaque. By having the function, it can be expected to suppress deterioration of periodontal disease and the like and reduce bad breath.
本発明者らは、歯科用樹脂材料、特に義歯用の樹脂に表面改質酸化亜鉛粉末を分散させて成形した歯科用樹脂材料、特に義歯によって、歯周病や齲蝕の原因菌を長期に渡って抑制でき、メチルメルカプタン等の口臭物質を低減でき、デンチャープラークの付着を抑制できることを見出し、本発明を完成させた。
The present inventors discovered that a dental resin material, especially a dental resin material, especially a denture, which is formed by dispersing surface-modified zinc oxide powder in a resin for dentures, can prevent periodontal disease and caries-causing bacteria for a long period of time. The present invention has been completed on the basis of the finding that it is possible to suppress oral malodorous substances such as methyl mercaptan and the like, and that adhesion of denture plaque can be suppressed.
本発明によれば、以下の歯科用樹脂材料、抗菌性義歯等が提供される。
１．表面改質された酸化亜鉛粉末を分散させた歯科用樹脂材料。
２．前記酸化亜鉛粉末の平均粒径が、１～５００ｎｍの範囲である、１に記載の歯科用樹脂材料。
３．前記表面改質が、硫化亜鉛皮膜による被覆である、１に記載の歯科用樹脂材料。
４．前記表面改質が、カップリング剤による被覆である、１に記載の歯科用樹脂材料。
５．前記表面改質が、酸化亜鉛粉末表面の部分被覆である、１～４のいずれかに記載の歯科用樹脂材料。
６．前記硫化亜鉛又はカップリング剤の被覆量が、０．１～３０質量％である、３又は４に記載の歯科用樹脂材料。
７．前記表面改質された酸化亜鉛粉末の配合量が、０．１～１０質量％である、１～５のいずれかに記載の歯科用樹脂材料。
８．歯冠用材料、コンポジットレジン、歯科充填用材料、レジンセメント、歯科用接着剤・合着材、フィッシャーシーラント、コーティング材、クラウン・ブリッジ・インレー用レジン、支台築造材、義歯用レジン、義歯床用レジン、義歯床補修用レジン、歯ブラシの毛用、歯ブラシの柄用、又はマウスピース用レジンである、１～７のいずれかに記載の歯科用樹脂材料。
９．歯周病原因菌、齲蝕原因菌及び／又は真菌の増殖を抑制する、１～８のいずれかに記載の歯科用樹脂材料。
１０．デンチャープラークの付着を抑制する、１～９のいずれかに記載の歯科用樹脂材料。
１１．口臭原因物質を低減する、１～１０のいずれかに記載の歯科用樹脂材料。
１２．１～１１のいずれかに記載の歯科用樹脂材料からなる抗菌性義歯。
１３．１～１１のいずれかに記載の歯科用樹脂材料からなるナイトガード。
According to the present invention, the following dental resin material, antibacterial denture, etc. are provided.
1. A dental resin material in which surface-modified zinc oxide powder is dispersed.
2. 2. The dental resin material according to 1, wherein the average particle size of the zinc oxide powder is in the range of 1 to 500 nm.
3. 2. The dental resin material according to 1, wherein the surface modification is coating with a zinc sulfide film.
4. 2. The dental resin material according to 1, wherein the surface modification is coating with a coupling agent.
5. 5. The dental resin material according to any one of 1 to 4, wherein the surface modification is partial coating of the zinc oxide powder surface.
6. 5. The dental resin material according to 3 or 4, wherein the coating amount of the zinc sulfide or coupling agent is 0.1 to 30% by mass.
7. 6. The dental resin material according to any one of 1 to 5, wherein the content of the surface-modified zinc oxide powder is 0.1 to 10% by mass.
8. Crown materials, composite resins, dental filling materials, resin cements, dental adhesives/luting materials, fisher sealants, coating materials, crown/bridge/inlay resins, abutment building materials, denture resins, denture bases 8. The dental resin material according to any one of 1 to 7, which is a resin for dental implants, a resin for repairing a denture base, a resin for toothbrush bristles, a toothbrush handle, or a mouthpiece.
9. 9. The dental resin material according to any one of 1 to 8, which inhibits growth of periodontal disease-causing bacteria, cariogenic bacteria and/or fungi.
10. 10. The dental resin material according to any one of 1 to 9, which suppresses adhesion of denture plaque.
11. 11. The dental resin material according to any one of 1 to 10, which reduces halitosis-causing substances.
12. An antibacterial denture made of the dental resin material according to any one of 1 to 11.
13. A night guard made of the dental resin material according to any one of 1 to 11.
本発明によれば、歯周病原因菌、齲蝕原因菌、真菌等に対する持続的な抗菌性を有し、かつ、メチルメルカプタン等の口臭原因物質を低減できる、又はデンチャープラークの付着を抑制できる歯科用樹脂材料、及びそれを用いて作製される歯科用物品、特に抗菌性義歯を提供することができる。
According to the present invention, there is provided a dental treatment that has sustained antibacterial properties against periodontal disease-causing bacteria, caries-causing bacteria, fungi, etc., and that can reduce halitosis-causing substances such as methyl mercaptan, or suppress the adhesion of denture plaque. and dental articles, particularly antibacterial dentures, made using the same.
本発明の歯科用樹脂材料は、表面改質された酸化亜鉛粉末を分散させた樹脂からなることを特徴とする。
ここで、「歯科用樹脂材料」とは、主として歯科で口腔内に用いる物品を形成するための樹脂材料をいう。「歯科用樹脂材料」の形態（性状）は、成形・固化を行う前は、特に限定されず、粉体状、粒子状、ビーズ状、ペレット状、ペースト状、固形状等のいずれであってもよく、固化した後は特定の形状を有する。
「歯科用樹脂材料」からなる、あるいはこれを用いて製造される物品の例としては、例えば、義歯、義歯床、歯ブラシの毛、歯ブラシの柄、ナイトガード、マウスピース等が挙げられ、特に義歯、義歯床であることが好ましい。
The dental resin material of the present invention is characterized by comprising a resin in which surface-modified zinc oxide powder is dispersed.
As used herein, the term "dental resin material" refers to a resin material mainly used for forming articles used in the oral cavity in dentistry. The form (property) of the "dental resin material" before molding and solidification is not particularly limited, and may be powder, particle, bead, pellet, paste, solid, or the like. It is also good and has a certain shape after solidifying.
Examples of articles made of or manufactured using the "dental resin material" include, for example, dentures, denture bases, toothbrush bristles, toothbrush handles, night guards, mouthpieces, etc., especially dentures. , preferably a denture base.
本発明でいう「歯科用樹脂材料」とは、上記物品の他、広く歯科治療や口腔ケアにおいて使用される樹脂製の歯科材料全般をも包含するものであり、例えば、歯冠用レジン、人工歯等の歯冠用材料、コンポジットレジン、根管充填材、ボンディング材等の歯科充填用材料、レジンセメント、矯正用接着材等の歯科用接着材・合着材、フィッシャーシーラント、コーティング材、クラウン・ブリッジ・インレー用レジン、支台築造材、義歯床用レジン、義歯床補修用レジン等が挙げられる。治療の過程で一時的に使用する充填物や補綴物や、長期に渡って口腔内で使用されるいわゆる入れ歯や、インプラントの代替歯部分、義歯床等を含む。
また、「義歯」とは、いわゆる入れ歯、インプラントの代替歯部分、義歯床を含む。
The term "dental resin material" as used in the present invention includes, in addition to the above articles, resin dental materials in general that are widely used in dental treatment and oral care. Crown materials for teeth, dental filling materials such as composite resins, root canal filling materials, bonding materials, resin cements, dental adhesives and luting materials such as orthodontic adhesives, fisher sealants, coating materials, crowns・Resins for bridges and inlays, abutment building materials, resins for denture bases, resins for denture base repairs, etc. It includes fillings and prostheses used temporarily in the course of treatment, so-called dentures used in the oral cavity over a long period of time, substitute tooth parts for implants, denture bases, and the like.
In addition, "dentures" include so-called dentures, replacement tooth portions of implants, and denture bases.
本発明の歯科用樹脂材料は、そのベースとなる材料（レジン等）に、表面改質酸化亜鉛粉末を添加し、均一に混合した流動性のある状態、即ち、患部に適用する前及び後の、硬化する前の段階のもの、及び硬化した後のものも含む。 The dental resin material of the present invention is prepared by adding a surface-modified zinc oxide powder to a base material (resin, etc.) and uniformly mixing the resulting fluid state, that is, before and after application to the affected area. , before curing, and after curing.
「酸化亜鉛」は、一般的な細菌に対する抗菌性を有する無機系抗菌剤として用いられているが、これまで義歯や補綴修復物等の歯科用樹脂材料に用いられることは無かった。 "Zinc oxide" is used as an inorganic antibacterial agent having antibacterial properties against general bacteria, but has never been used for dental resin materials such as dentures and prosthetic restorations.
また、３８０ｎｍ以下の紫外線を吸収することから、紫外線吸収剤としても知られている。酸化亜鉛は、紫外線を吸収すると光触媒作用により、酸化・還元力を発揮する。特に、酸化亜鉛の酸化力により樹脂が酸化され劣化が促進されるという問題点がある。 It is also known as an ultraviolet absorber because it absorbs ultraviolet rays of 380 nm or less. Zinc oxide exhibits oxidizing and reducing power through photocatalytic action when it absorbs ultraviolet rays. In particular, there is a problem that the oxidizing power of zinc oxide oxidizes the resin and promotes deterioration.
本発明における、酸化亜鉛粉末の「表面改質」とは、酸化亜鉛粉末の表面を部分的に被覆処理することで、歯周病原因菌、齲蝕原因菌や真菌に対する抗菌性、口臭の脱臭効果は損なうことなく、酸化亜鉛の光触媒活性を抑制し、樹脂中での分散性を向上させるための加工をいう。 In the present invention, the “surface modification” of zinc oxide powder means that the surface of zinc oxide powder is partially coated to provide antibacterial properties against periodontal disease-causing bacteria, cariogenic bacteria and fungi, and deodorizing effect on bad breath. is a process that suppresses the photocatalytic activity of zinc oxide and improves its dispersibility in resin without damaging it.
本発明における、酸化亜鉛粉末の「表面改質」方法としては、例えば、特許文献２及び３に記載されている方法が挙げられる。
特許文献２に記載の硫化処理は、酸化亜鉛粉末を硫化水素又は亜硫酸ガスと接触させて、酸化亜鉛粉末の表面を硫化させ、酸化亜鉛粉末の表面を硫化亜鉛で被覆する方法である。具体的には、酸化亜鉛粉末をガラス容器に入れ、これを振動させながら、硫化水素ガス又は亜硫酸ガスを流通させて接触させる。
In the present invention, the method of "surface modification" of zinc oxide powder includes, for example, the methods described in
The sulfurization treatment described in Patent Document 2 is a method of contacting zinc oxide powder with hydrogen sulfide or sulfurous acid gas to sulfurize the surface of the zinc oxide powder and coating the surface of the zinc oxide powder with zinc sulfide. Specifically, zinc oxide powder is placed in a glass container, and hydrogen sulfide gas or sulfurous acid gas is circulated to bring it into contact while vibrating it.
特許文献３に記載のカップリング剤による被覆処理は、酸化亜鉛粉末の表面にカップリング剤を被覆処理し、被覆酸化亜鉛粉末とする方法である。
酸化亜鉛粉末表面へのカップリング剤の被覆処理は、酸化亜鉛粉末の水中又は非水溶媒中のスラリーを攪拌しつつカップリング剤を添加する湿式法；高速回転が可能なヘンシェルミキサーやハイスピードミキサー等で酸化亜鉛粉末を高速攪拌しつつカップリング剤をスプレーまたは滴下する乾式法；酸化亜鉛粉末を入れた反応容器内に窒素等の不活性ガスでキャリーしたカップリング剤を導入し、被覆処理する気相法のいずれでもよい。
The coating treatment with a coupling agent described in
The coating treatment of the coupling agent on the surface of the zinc oxide powder is a wet method in which the coupling agent is added while stirring the slurry of the zinc oxide powder in water or a non-aqueous solvent; Henschel mixer or high speed mixer capable of rotating at high speed. A dry method in which a coupling agent is sprayed or dropped while the zinc oxide powder is stirred at high speed with a method such as the following: A coupling agent carried by an inert gas such as nitrogen is introduced into a reaction vessel containing the zinc oxide powder, and the coating is performed. Any vapor phase method may be used.
カップリング剤としては、シラノール基、エポキシ基、メタクリル基、ビニル基、メルカプト基、アミノ基等を持つシランカップリング剤を使用することができる。また、シランカップリング剤以外のチタン系、アルミニウム系、ジルコニウム系、ジルコアルミネート系等のその他のカップリング剤あるいはシラン等を使用してもよい。 A silane coupling agent having a silanol group, an epoxy group, a methacryl group, a vinyl group, a mercapto group, an amino group, or the like can be used as the coupling agent. In addition to the silane coupling agent, other coupling agents such as titanium, aluminum, zirconium, and zircoaluminate, or silane may be used.
酸化亜鉛粉末の平均粒径は、１～５００ｎｍの範囲であることが好ましく、１０～４００ｎｍであることがより好ましく、５０～３００ｎｍであることがさらに好ましい。上記範囲内であれば、歯科用樹脂への分散性が損なわれず、均一に混合できる。 The average particle size of the zinc oxide powder is preferably in the range of 1 to 500 nm, more preferably 10 to 400 nm, even more preferably 50 to 300 nm. If it is within the above range, the dispersibility in the dental resin is not impaired, and uniform mixing can be achieved.
酸化亜鉛粉末のＢＥＴ法による比表面積は、１０～５００ｍ２／ｇの範囲であることが好ましく、１０～４００ｍ２／ｇがより好ましく、２０～３００ｍ２／ｇがさらに好ましい。 The specific surface area of the zinc oxide powder by the BET method is preferably in the range of 10 to 500 m 2 /g, more preferably 10 to 400 m 2 /g, even more preferably 20 to 300 m 2 /g.
酸化亜鉛粉末の表面を部分的に被覆するためには、酸化亜鉛粉末の比表面積を考慮して、硫化亜鉛皮膜及びカップリング剤による被覆量を調整すればよく、表面改質酸化亜鉛粉末の使用目的により適宜決定すればよい。
歯科用樹脂材料の場合には、被覆量は、０．１～３０質量％の範囲とすることが好ましく、０．２～２０質量％がより好ましく、０．２～１５質量％がさらに好ましい。上記範囲内であれば、樹脂中に均一に分散させ易く、酸化亜鉛の歯周病原因菌、齲蝕原因菌、真菌等への抗菌性が損なわれず、口臭原因物質等の分解性が保持できる。
In order to partially coat the surface of the zinc oxide powder, the coating amount of the zinc sulfide coating and the coupling agent may be adjusted in consideration of the specific surface area of the zinc oxide powder. It may be determined appropriately depending on the purpose.
In the case of a dental resin material, the coating amount is preferably in the range of 0.1 to 30% by mass, more preferably 0.2 to 20% by mass, even more preferably 0.2 to 15% by mass. Within the above range, it is easy to disperse uniformly in the resin, the antibacterial properties of zinc oxide against periodontal disease-causing bacteria, cariogenic bacteria, fungi, etc. are not impaired, and the degradability of halitosis-causing substances, etc. can be maintained.
本発明の歯科用樹脂材料で用いることができる「表面改質酸化亜鉛粉末」の市販品としては、例えば、ＡＤ－ＰＳＪ（株式会社ニッショー化学製）が挙げられる。 Examples of commercial products of the “surface-modified zinc oxide powder” that can be used in the dental resin material of the present invention include AD-PSJ (manufactured by Nissho Chemical Co., Ltd.).
表面改質酸化亜鉛粉末を分散させる基材となる「樹脂」は、特に限定されず、歯科領域で通常に用いられる種類の樹脂を用いることができる。
本発明の歯科用樹脂材料が義歯用材料として用いられる場合、基材となる「樹脂」は義歯用のベースレジンである。
The "resin" serving as the base material for dispersing the surface-modified zinc oxide powder is not particularly limited, and resins commonly used in the dental field can be used.
When the dental resin material of the present invention is used as a denture material, the "resin" serving as a base material is a base resin for dentures.
義歯用のベース材料（レジン）としては、広く使用されている義歯用レジンを用いることができる。義歯用レジンとしては、マイクロウエーブ重合型（電子レンジ）、熱重合（お湯炊き）等が好ましい。義歯用レジンの市販品としては、例えば、ベイシスレジン（山八歯材工業株式会社製、加熱重合型）、アクロン（株式会社ジーシー製、加熱重合型）、アクロンＭＣ（株式会社ジーシー製、マイクロ波重合型）、クイックアクロン（株式会社ジーシー製、加熱重合・ヒートショック型）、ラクソン（株式会社ジーシー製、加熱重合型）、フィットレジン（株式会社松風製、常温重合レジン）、ポアーレジン（株式会社松風製、常温重合レジン）、アーバン（株式会社松風製、加熱重合レジン）等が挙げられる。 Widely used denture resins can be used as the base material (resin) for dentures. As the denture resin, microwave polymerization type (microwave oven), thermal polymerization (hot water boiling), etc. are preferable. Commercially available denture resins include, for example, Basis Resin (manufactured by Yamapachi Dental Industry Co., Ltd., heat polymerization type), Akron (manufactured by GC Corporation, heat polymerization type), Akron MC (manufactured by GC Corporation, microwave Polymerization type), Quick Acron (manufactured by GC Corporation, heat polymerization/heat shock type), Laxon (manufactured by GC Corporation, heat polymerization type), Fit Resin (manufactured by Shofu Co., Ltd., normal temperature polymerization resin), Pore Resin (Shofu Co., Ltd.) and Urban (manufactured by Shofu Co., Ltd., heat polymerization resin).
表面改質酸化亜鉛粉末を義歯形成用樹脂に混合する手段は、当業者が通常用いる方法から適切なものを選択すればよい。例えば、粉（重合開始剤）及び液（重合性単量体）の２成分型の義歯成形用レジンの場合には、液（重合性単量体）に表面改質酸化亜鉛粉末を予め添加し、これを粉（重合開始剤）と混合するか、或いは粉（重合開始剤）に表面改質酸化亜鉛粉末を予め添加し、これを液（重合性単量体）と混合すればよい。
表面改質酸化亜鉛粉末を混合した樹脂材料を成形する手段、及び硬化させる手段も、当業者が通常用いる方法からベース材料に適したものを選択すればよい。
The means for mixing the surface-modified zinc oxide powder with the denture-forming resin may be appropriately selected from methods commonly used by those skilled in the art. For example, in the case of a two-component denture molding resin consisting of a powder (polymerization initiator) and a liquid (polymerizable monomer), surface-modified zinc oxide powder is added to the liquid (polymerizable monomer) in advance. Alternatively, the surface-modified zinc oxide powder may be added to the powder (polymerization initiator) in advance and mixed with the liquid (polymerizable monomer).
The means for molding the resin material mixed with the surface-modified zinc oxide powder and the means for curing may also be selected from methods commonly used by those skilled in the art and suitable for the base material.
また、近年では、３Ｄプリンターを用いた義歯の製造が広まっている。３Ｄプリンターで義歯を製造する場合には、表面改質酸化亜鉛粉末を配合した粉末状又はペレット状の樹脂材料を３Ｄプリントの原料として用い、所望の形状の義歯とすればよい。 Moreover, in recent years, manufacturing of dentures using a 3D printer has spread. When manufacturing dentures with a 3D printer, a powdery or pellet-shaped resin material containing surface-modified zinc oxide powder may be used as a raw material for 3D printing to obtain dentures of a desired shape.
本発明の歯科用樹脂材料中の表面改質酸化亜鉛粉末の配合量は、使用する樹脂や用途によっても異なるが、通常は０．１～１０質量％、好ましくは０．３～５質量％、より好ましくは０．５～３質量％の範囲内である。 The amount of the surface-modified zinc oxide powder to be blended in the dental resin material of the present invention varies depending on the resin used and the application, but is usually 0.1 to 10% by mass, preferably 0.3 to 5% by mass. More preferably, it is within the range of 0.5 to 3% by mass.
本発明の歯科用樹脂材料、及びそれを用いて作製される抗菌性義歯等の歯科用物品には、その用途に応じて、表面改質酸化亜鉛粉末が有する効果が損なわれない範囲で、表面改質酸化亜鉛粉末以外に各種の添加剤が配合されていてもよい。添加剤としては、フィラー、着色剤等の歯科用物品に添加される各種のものが挙げられる。また、本発明の歯科用樹脂材料には、さらに酸化亜鉛以外の無機系抗菌剤や、有機系抗菌剤を配合してもよい。 The dental resin material of the present invention and dental articles such as antibacterial dentures produced using the same may be coated with a surface-modified zinc oxide powder depending on the intended use, as long as the effects of the surface-modified zinc oxide powder are not impaired. Various additives may be blended in addition to the modified zinc oxide powder. Examples of additives include various substances added to dental articles such as fillers and coloring agents. The dental resin material of the present invention may further contain an inorganic antibacterial agent other than zinc oxide, or an organic antibacterial agent.
歯科用樹脂材料、及びそれを用いた義歯等の歯科用物品は、実施例又は試験例に記載の方法に準拠し、用いるベース材料、目的とする歯科用物品に合わせ、当業界で通常用いられる方法で製造することができる。 A dental resin material and a dental article such as a denture using the same are generally used in the art according to the method described in Examples or Test Examples, according to the base material to be used and the intended dental article. can be manufactured by a method.
本発明でいう「抗菌性（antibacterial）」とは、細菌を死滅させる「殺菌性（bactericidal）」乃至、細菌の増殖を抑制する「静菌性（bacteriostatic）」までの範囲を包含するが、「静菌性」であることが好ましい。口腔常在菌を死滅させることなく、口腔内の免疫を保持しつつ、歯周病原因菌、齲蝕原因菌、真菌等の増殖を抑制することが好ましいからである。 The term "antibacterial" as used in the present invention encompasses a range from "bactericidal" that kills bacteria to "bacteriostatic" that suppresses the growth of bacteria. It is preferably "bacteriostatic". This is because it is preferable to suppress the growth of periodontal disease-causing bacteria, cariogenic bacteria, fungi, etc. while maintaining immunity in the oral cavity without killing oral bacteria.
本発明の歯科用樹脂材料からなる抗菌性義歯は、義歯に求められる機械的強度、低い吸水性等の特性を有し、抗菌性だけでなく、デンチャープラークの付着が抑制でき、さらには口臭原因物質であるメチルメルカプタン等の悪臭を低減することができる。 The antibacterial denture made of the dental resin material of the present invention has properties such as mechanical strength and low water absorption required for dentures, and is not only antibacterial, but also suppresses the adhesion of denture plaque, and is a cause of bad breath. It is possible to reduce the bad smell of substances such as methyl mercaptan.
また、ナイトガード等の柔軟性を有する歯科用物品にも、本発明の歯科用樹脂材料を用いることができ、就寝時の歯周病原因菌、齲蝕原因菌、真菌等の増殖を抑制し、発生する口臭原因物質を低減することができる。
In addition, the dental resin material of the present invention can also be used for flexible dental articles such as night guards. It is possible to reduce the substances that cause halitosis.
以下、実施例及び試験例を挙げて、本発明をより具体的に説明するが、本発明はこれらの実施例等によって何ら限定されるものではない。 EXAMPLES The present invention will be described in more detail below with reference to Examples and Test Examples, but the present invention is not limited to these Examples and the like.
実施例１：表面改質酸化亜鉛粉末配合樹脂材料の製造
表面改質酸化亜鉛粉末であるＡＤ－ＰＳＪ（株式会社ニッショー化学製）を、それぞれ１．５質量％、１．０質量％、及び０．５質量％の濃度で、アクリルレジンに配合し、成形した表面改質酸化亜鉛粉末配合樹脂材料（アクリルレジンディスク）を、以下のように作製した。
Example 1: Production of resin material containing surface-modified zinc oxide powder AD-PSJ (manufactured by Nissho Chemical Co., Ltd.), which is a surface-modified zinc oxide powder, was added at 1.5% by mass, 1.0% by mass, and 0% by mass, respectively. A surface-modified zinc oxide powder-blended resin material (acrylic resin disk) was prepared by blending with an acrylic resin at a concentration of 5% by mass and molding it as follows.
直径１７．５ｍｍ、高さ５０ｍｍの円柱状のシリコン型をフラスコに埋没した。ベイシスレジン（山八歯材工業株式会社製、アクリルレジン）の粉末２０ｇと液８．６ｍＬを混和し、室温にて２０分間放置した。餅状になったアクリルレジンをシリコン型に填入し、油圧プレス（ＴＤ－６０７；吉田製作所製）を用いて、４０ｋｇ／ｃｍ２の圧力をかけ固定した。フラスコを水糟（イボ－１；白水貿易株式会社製）に浸潰し、加熱、沸騰後３０分で重合完了とした。 A cylindrical silicon mold with a diameter of 17.5 mm and a height of 50 mm was embedded in the flask. 20 g of powder of Basis resin (manufactured by Yamapachi Dental Industry Co., Ltd., acrylic resin) and 8.6 mL of liquid were mixed and allowed to stand at room temperature for 20 minutes. The mochi-shaped acrylic resin was put into a silicon mold and fixed by applying a pressure of 40 kg/cm 2 using a hydraulic press (TD-607; manufactured by Yoshida Seisakusho). The flask was immersed in water lees (Ibo-1; manufactured by Hakusui Trading Co., Ltd.), heated, and boiled for 30 minutes to complete the polymerization.
水槽からフラスコを取り出し、室温にて３０分間放置後、さらに水中に入れ完全に冷却して、重合したアクリルレジンの掘り出しを行った。掘り出した円柱状のアクリルレジンを、自動回転切断機（ＩＳＯＭＥＴ １１－１１８０ Ｌｏｗ Ｓｐｅｅｄ Ｓａｗ；Ｂｕｅｈｌｅｒ ＬＴＤ．，ＩＬ． Ｕ．Ｓ．Ａ．）を用いて、厚さｌ．２ｍｍとなるように切断した後、上下面を耐水研磨紙＃１０００にて研磨し、直径１７．５±０．５ｍｍ、厚さ１．０±０．２ｍｍに調整したものをアクリルレジンディスクとした。 The flask was taken out of the water bath, left at room temperature for 30 minutes, further immersed in water to cool completely, and the polymerized acrylic resin was dug out. The excavated cylindrical acrylic resin was cut into pieces having a thickness of l. After cutting to 2 mm, the upper and lower surfaces were polished with waterproof abrasive paper #1000 to adjust the diameter to 17.5 ± 0.5 mm and the thickness to 1.0 ± 0.2 mm to obtain an acrylic resin disk. .
作製したアクリルレジンディスクについて、精度０．００１ｍｍのマイクロメーター（Ｍｉｔｕｔｏｙｏ；株式会社シナノ製作所製）にて直径２カ所、厚さ５カ所を計測し、直径及び厚さの平均値よりアクリルレジンディスクの体積Ｖを算出した。 The diameter and thickness of the prepared acrylic resin disk were measured at 2 locations and 5 locations with a micrometer (Mitutoyo; manufactured by Shinano Seisakusho Co., Ltd.) with an accuracy of 0.001 mm. V was calculated.
作製したアクリルレジンディスクをデシケータ内で乾燥させ、２４時間で０．２ｍｇの質量域になるまで、電子天秤（ＡＵＷ１２０Ｄ；島津製作所製）にて繰り返し秤量を行い、恒量となった時点で３７℃の水中に浸潰した。 The prepared acrylic resin disk was dried in a desiccator and repeatedly weighed with an electronic balance (AUW120D; manufactured by Shimadzu Corporation) until the mass range reached 0.2 mg in 24 hours. immersed in water.
試験例１：表面改質酸化亜鉛粉末配合樹脂材料の吸水性試験
表面改質酸化亜鉛粉末を配合することにより、得られる樹脂材料の吸水性が変化するか否かを確認した。
Test Example 1: Water Absorption Test of Resin Material Blended with Surface-Modified Zinc Oxide Powder It was confirmed whether or not the water absorption of the resulting resin material changed by blending the surface-modified zinc oxide powder.
表面改質酸化亜鉛粉末ＡＤ－ＰＳＪを、それぞれ１．５質量％、１．０質量％、及び０．５質量％の濃度で配合したアクリルレジンディスク（試験片）、並びに比較対照として、表面改質酸化亜鉛粉末を配合していないアクリルレジンディスク（対照片）を用いて、吸水性試験を行った。 Acrylic resin discs (test pieces) containing surface-modified zinc oxide powder AD-PSJ at concentrations of 1.5% by mass, 1.0% by mass, and 0.5% by mass, respectively. A water absorption test was conducted using an acrylic resin disk (control piece) containing no zinc oxide powder.
試験片及び対照片のアクリルレジンディスクを、３７℃の水中に１日間、７日間、及び２８日間保管した。各保管期間後に、アクリルレジンディスクを水中から取り出し、乾いたタオルで表面の水分をふき取り、空気中で１５秒間振った後、１分後に秤量した質量をｍ１とした。秤量後、アクリルレジンディスクを再びデシケータ内で乾燥させ、恒量となったときの質量をｍ２とした。得られたアクリルレジンディスクの質量データより、次式に従って吸水量を求めた。尚、アクリルレジンディスク（試験片及び対照片）は、各群５個とした。
Ｗｓｐ＝（ｍ１－ｍ２）／Ｖ
式中、
Ｗｓｐ：吸水量（μｇ／ｍｍ３）
ｍ１：水中浸漬直後のアクリルレジンディスクの質量（μｇ）
ｍ２：アクリルレジンディスクの乾燥質量（μｇ）
Ｖ：アクリルレジンディスクの体積（ｍｍ３）
The acrylic resin discs of test and control specimens were stored in water at 37° C. for 1 day, 7 days, and 28 days. After each storage period, the acrylic resin disc was taken out of the water, wiped off with a dry towel, shaken in the air for 15 seconds, and weighed after 1 minute. After weighing, the acrylic resin disk was dried again in the desiccator, and the mass when it reached a constant weight was defined as m 2 . From the mass data of the obtained acrylic resin disk, the water absorption was determined according to the following formula. Five acrylic resin discs (test piece and control piece) were used in each group.
Wsp = (m1 - m2 )/V
During the ceremony,
W sp : water absorption (μg/mm 3 )
m 1 : mass of acrylic resin disk immediately after immersion in water (μg)
m 2 : Dry mass of acrylic resin disk (μg)
V: Volume of acrylic resin disk (mm 3 )
得られた吸水量の結果を図１のグラフに示す。
図１のグラフから、表面改質酸化亜鉛粉末未配合（対照片）及び表面改質酸化亜鉛粉末未配合のアクリルレジンディスク（試験片）ともに、水中保管１日後に比べ、７日後及び２８日後では、吸水量に差が認められるが、水中保管７日後と２８日後では、吸水量に差は認められなかった。このことから、表面改質酸化亜鉛粉末を配合することは、アクリルレジンの吸水性に影響を与えないことがわかる。
The obtained water absorption results are shown in the graph of FIG.
From the graph in FIG. 1, both the surface-modified zinc oxide powder unblended (control piece) and the surface-modified zinc oxide powder unblended acrylic resin disc (test piece) were stored in water for 7 days and 28 days after storage in water for 1 day. , but there was no difference in water absorption after 7 days and 28 days of storage in water. From this, it can be seen that the addition of the surface-modified zinc oxide powder does not affect the water absorbency of the acrylic resin.
試験例２：表面改質酸化亜鉛粉末を配合した樹脂材料の機械的特性の評価
本発明の抗菌性歯科用材料は、例えば、義歯であれば、口腔内の常に湿った環境下で用いられるため、吸水によって強度が低下しないことを確認した。
表面改質酸化亜鉛粉末を、それぞれ１．５質量％、１．０質量％、及び０．５質量％の濃度で配合した板状アクリルレジン（試験片）、並びに比較対照として、表明改質酸化亜鉛粉末を配合していない板状アクリルレジン（対照片）を用いて３点曲げ試験を行なった。
Test Example 2: Evaluation of Mechanical Properties of Resin Material Blended with Surface-Modified Zinc Oxide Powder The antibacterial dental material of the present invention, for example, in the case of dentures, is used in an environment in which the oral cavity is always moist. , confirmed that the strength does not decrease due to water absorption.
Plate-shaped acrylic resin (test piece) containing surface-modified zinc oxide powder at concentrations of 1.5% by mass, 1.0% by mass, and 0.5% by mass, respectively, and surface-modified oxidized resin for comparison. A three-point bending test was performed using a plate-like acrylic resin (control piece) containing no zinc powder.
試験片及び対照片の板状アクリルレジンは、次の様に作製した。
板状のシリコン型をフラスコに埋没した。ベイシスレジンの粉１０ｇと液４．３ｍＬを混和し、室温で１５分間放置した。餅状になったアクリルレジンを板状のシリコン型に填入し、油圧プレスで４０ｋｇ／ｃｍ２の圧力をかけ固定した。フラスコを水槽に浸潰し加熱、弗騰後３０分で重合完了とした。水中からフラスコを取り出し，室温にて３０分開放置後、さらに水中に入れ完全に冷却し、重合したアクリルレジンの掘り出しを行った。
Plate-shaped acrylic resins for test pieces and control pieces were prepared as follows.
A plate-like silicon mold was embedded in the flask. 10 g of basis resin powder and 4.3 mL of liquid were mixed and left at room temperature for 15 minutes. The rice cake-like acrylic resin was put into a plate-like silicon mold and fixed by applying a pressure of 40 kg/cm 2 with a hydraulic press. The flask was immersed in a water bath and heated, and the polymerization was completed 30 minutes after the flask was heated. The flask was taken out of the water, left to stand at room temperature for 30 minutes, then put into water to cool completely, and the polymerized acrylic resin was dug out.
掘り出した板状のアクリルレジンは．横２５ｍｍ、厚さ３ｍｍとなるように耐水研磨紙＃６００にて研磨し、縦３ｍｍとなるように自動回転切断機にて切断し、縦３ｍｍ×横２５ｍｍ×厚さ３ｍｍの試験片を得た。対照片は、表面改質酸化亜鉛粉末を配合しないこと以外、試験片と同様にして作製した。 The plate-shaped acrylic resin that was dug out. It was polished with water-resistant abrasive paper #600 to a width of 25 mm and a thickness of 3 mm, and cut by an automatic rotary cutting machine to a length of 3 mm to obtain a test piece of 3 mm length × 25 mm width × 3 mm thickness. . A control piece was prepared in the same manner as the test piece, except that the surface-modified zinc oxide powder was not blended.
得られた板状アクリルレジンの試験片及び対照片を、３７℃の水中に１日間、７日間、及び２８日間保管した。各保管期間後に、板状アクリルレジンを水中から取り出し、乾いたタオルで表面の水分をふき取り、試験に供した。 The resulting plate-like acrylic resin test piece and control piece were stored in water at 37° C. for 1 day, 7 days, and 28 days. After each storage period, the plate-shaped acrylic resin was taken out of the water, the water on the surface was wiped off with a dry towel, and the test was performed.
小型卓上試験機（ＥＺＴｅｓｔ；島津製作所製）を用いて、支点問距離２０ｍｍ、クロスヘッドスピード１ｍｍ／ｍｉｎで３点曲げ強さ試験を行い、分析ソフト（ＴＲＡＰＥＺＵＭ２；島津製作所製）により、曲げ強さと曲げ弾性率を算出した。尚、試験片及び対照片は各群１５個とした。
得られた曲げ強さの結果を図２のグラフに、曲げ弾性率の結果を図３のグラフに示す。
Using a small desktop tester (EZTest; manufactured by Shimadzu Corporation), a three-point bending strength test was performed with a fulcrum distance of 20 mm and a crosshead speed of 1 mm / min. A flexural modulus was calculated. 15 test pieces and control pieces were used in each group.
The results of bending strength obtained are shown in the graph of FIG. 2, and the results of bending elastic modulus are shown in the graph of FIG.
図２のグラフから、１日目及び７日目の試験片の曲げ強さは、対照片の曲げ強さよりも劣っていたが、２８日目には、試験片と対照片で差は見られなかった。 From the graph in FIG. 2, the bending strength of the test piece on the 1st and 7th days was inferior to the bending strength of the control piece, but on the 28th day, there was no difference between the test piece and the control piece. I didn't.
図３のグラフから、１日目、７日目及び２８日目のいずれも、試験片と対照片とで曲げ弾性率に差は見られなかった。 From the graph in FIG. 3, there was no difference in flexural modulus between the test piece and the control piece on the 1st day, the 7th day, and the 28th day.
試験例１及び２の結果から、本発明の表面改質酸化亜鉛粉末を配合した歯科用樹脂材料は、口腔内の湿った環境下でも吸水性（膨潤性）が低く、機械的強度が低下することも無く、口腔内で用いられる歯科用樹脂材料として好適であることがわかる。 From the results of Test Examples 1 and 2, the dental resin material containing the surface-modified zinc oxide powder of the present invention has low water absorption (swellability) and low mechanical strength even in a moist environment in the oral cavity. Therefore, it can be seen that it is suitable as a dental resin material used in the oral cavity.
試験例３：表面改質酸化亜鉛粉末の口腔細菌に対する抗菌性試験
表面改質酸化亜鉛粉末であるＡＤ－ＰＳＪの、歯周病原因菌、齲蝕原因菌及び真菌に対する抗菌性を確認する。
Test Example 3: Antimicrobial Activity Test of Surface-Modified Zinc Oxide Powder Against Oral Bacteria The antibacterial activity of AD-PSJ, which is a surface-modified zinc oxide powder, against periodontal disease-causing bacteria, cariogenic bacteria and fungi is confirmed.
（供試菌株）
歯周病原因菌：Ｐｏｒｐｈｙｒｏｍｏｎａｓ ｇｉｎｇｉｖａｌｉｓ（Ｐ．ｇｉｎｇｉｖａｌｉｓ）ＡＴＣＣ３３２７７株
齲蝕原因菌：Ｓｔｒｅｐｔｏｃｏｃｃｕｓ ｍｕｔａｎｓ（Ｓ．ｍｕｔａｎｓ）Ｉｎｇｂｒｉｔｔ株
真菌：Ｃａｎｄｉｄａ ａｌｂｉｃａｎｓ（Ｃ．ａｌｂｉｃａｎｓ）ＡＴＣＣ１０２３１株
(test strain)
Periodontal disease-causing bacteria: Porphyromonas gingivalis (P. gingivalis) ATCC33277 strain Caries-causing bacteria: Streptococcus mutans (S. mutans) Ingbritt strain Fungi: Candida albicans (C. albicans) ATCC10231 strain
Ｐ．ｇｉｎｇｉｖａｌｉｓは、５％ヒツジ脱繊血を含むＢＨＩ血液寒天培地（ＢＨＩ血液平板）を用いて嫌気条件下（７０％ Ｎ２、１５％ Ｈ２、１５％ ＣＯ２）（ＡＮＸ－１；ＨＩＲＡＳＡＷＡ製）３７℃で培養した。
Ｓ．ｍｕｔａｎｓは、ブレインハートインフージョン（ＢＨＩ）ブロス（Ｂｅｃｔｏｎ Ｄｉｃｋｉｎｓｏｎ Ｃｏ．製）にイーストエストラクト（５ｍｇ／ｍＬ）（Ｂｅｃｔｏｎ Ｄｉｃｋｉｎｓｏｎ Ｃｏ．製）、ヘミン（５μｇ／ｍＬ）（和光純薬製）、ビタミンＫ１（１０μｇ／ｍＬ）（和光純薬製）を添加した培地（ＢＨＩ・ＹＨＫ培地）で培養した。
Ｃ．ａｌｂｉｃａｎｓは、普通寒天培地（日水製薬株式会社製）を用いて好気条件下３７℃（アルプ株式会社製）で培養した。
P. gingivalis was grown under anaerobic conditions (70% N 2 , 15% H 2 , 15% CO 2 ) using BHI blood agar medium (BHI blood plate) containing 5% defibrinated sheep blood (ANX-1; manufactured by HIRASAWA). Cultured at 37°C.
S. Mutans is prepared by adding yeast extract (5 mg/mL) (Becton Dickinson Co.), hemin (5 μg/mL) (Wako Pure Chemical Industries), vitamin K to brain heart infusion (BHI) broth (Becton Dickinson Co.). 1 (10 μg/mL) (manufactured by Wako Pure Chemical Industries, Ltd.) was added to the medium (BHI/YHK medium).
C. albicans was cultured under aerobic conditions at 37° C. (manufactured by Alp Co., Ltd.) using a nutrient agar medium (manufactured by Nissui Pharmaceutical Co., Ltd.).
一昼夜培養し、波長５５０ｎｍで吸光度０．６に調整したＰ．ｇｉｎｇｉｖａｌｉｓ（実験開始時生菌数：２．０×１０９±１．０×１０７ＣＦＵ／ｍＬ）、Ｓ．ｍｕｔａｎｓ（実験開始時生菌数：１．０×１０９±１．５×１０８ＣＦＵ／ｍＬ）、及びＣ．ａｌｂｉｃａｎｓ（実験開始時生菌数：３．０×１０７±７．５×１０６ＣＦＵ／ｍＬ）の培養菌液に１％濃度となるよう表面改質酸化亜鉛粉末ＡＤ－ＰＳＪを加え、沈殿しないようスターラーにて撹拌しながら培養し、２４時間まで経時的に生菌数（ＣＦＵ／ｍＬ）を測定した。尚、表面改質酸化亜鉛粉末を添加しない比較対照（ｃｏｎｔｒｏｌ）についても並行して生菌数を測定した。結果をそれぞれ図４～６のグラフに示す。 After culturing overnight, the P. spp. gingivalis (viable cell count at the start of experiment: 2.0×10 9 ±1.0×10 7 CFU/mL), S. gingivalis. mutans (viable cell count at the start of the experiment: 1.0×10 9 ±1.5×10 8 CFU/mL), and C. The surface-modified zinc oxide powder AD-PSJ was added to a culture solution of C. albicans (viable cell count at the start of the experiment: 3.0×10 7 ±7.5×10 6 CFU/mL) to a concentration of 1% to precipitate. Cultivation was performed while stirring with a stirrer so as not to prevent the culture, and the number of viable cells (CFU/mL) was measured over time for up to 24 hours. In addition, the number of viable bacteria was also measured in parallel for a control to which no surface-modified zinc oxide powder was added. The results are shown in the graphs of FIGS. 4-6, respectively.
図４のグラフから、Ｐ．ｇｉｎｇｉｖａｌｉｓは、表面改質酸化亜鉛粉末の添加により生菌数が経時的に減少し、１２時間後以降は生菌は確認されなかったことがわかる。この結果から、表面改質酸化亜鉛粉末は、歯周病原因菌Ｐ．ｇｉｎｇｉｖａｌｉｓに対して強力な抗菌性を有することが確認された。 From the graph in FIG. gingivalis, the addition of the surface-modified zinc oxide powder decreased the number of viable bacteria over time, and no viable bacteria were observed after 12 hours. From these results, the surface-modified zinc oxide powder is effective against periodontal disease-causing bacteria P. gingivalis was confirmed to have strong antibacterial properties.
図５のグラフから、Ｓ．ｍｕｔａｎｓは、表面改質酸化亜鉛粉末の添加により経時的に生菌数の減少したことがわかる。この結果から、表面改質酸化亜鉛粉末は、齲蝕原因菌Ｓ．ｍｕｔａｎｓに対して緩やかな抗菌性を有することが確認された。 From the graph in FIG. It can be seen that the number of viable mutans decreased over time due to the addition of the surface-modified zinc oxide powder. From these results, the surface-modified zinc oxide powder was found to be effective against the cariogenic bacteria S. cerevisiae. It was confirmed to have moderate antibacterial activity against mutans.
図６のグラフから、Ｃ．ａｌｂｉｃａｎｓは、表面改質酸化亜鉛粉末を添加した場合でも経時的に生菌数は緩やかに増加していたが、表面改質酸化亜鉛粉末を添加していない比較対照に比べて増殖が抑制されたことがわかる。この結果から、表面改質酸化亜鉛粉末は、真菌Ｃ．ａｌｂｉｃａｎｓに対して増殖抑制効果を有することが確認された。 From the graph of FIG. 6, C.I. albicans, the number of viable bacteria gradually increased over time even when the surface-modified zinc oxide powder was added, but the growth was suppressed compared to the control to which the surface-modified zinc oxide powder was not added. I understand. The results indicate that the surface-modified zinc oxide powder is effective against the fungus C. It was confirmed to have a growth inhibitory effect on S. albicans.
試験例４：表面改質酸化亜鉛粉末を配合した歯科用樹脂材料への口腔細菌の付着抑制試験
表面改質酸化亜鉛粉末を配合した歯科用樹脂材料に、プラークの付着抑制効果があることを確認する。
Test Example 4: Test of inhibition of adhesion of oral bacteria to dental resin material containing surface-modified zinc oxide powder Confirmation that dental resin material containing surface-modified zinc oxide powder has an effect of inhibiting plaque adhesion do.
表面改質酸化亜鉛粉末ＡＤ－ＰＳＪを、それぞれ１．０質量％、及び０．５質量％の濃度で配合したアクリルレジンディスク（試験片）を用いて、プラーク付着性試験を行った。
Ｐ．ｇｉｎｇｉｖａｌｉｓ、Ｓ．ｍｕｔａｎｓ、及びＣ．ａｌｂｉｃａｎｓの各培養菌液１００μＬを加えた液体培地５ｍＬに、アクリルレジンディスクを浸潰し、１８時間培養した。培養後、アクリルレジンディスクを１％リン酸緩衝生理食塩水（ＰＢＳ）で３回洗浄した。アクリルレジンディスクを５ｍＬのＰＢＳに浸漬させ、Ｔｒａｎｓｓｏｎｉｃ Ｔ７８０（超音波洗浄機；Ｅｌｍａ Ｓｃｈｍｉｄｂａｕｅｒ ＧｍｂＨ製）を用いて１分間の超音波処理によりアクリルレジンディスクから細菌を剥離した。剥離した細菌懸濁液を希釈して寒天培地へ塗抹、培養を行い、生菌数を測定した。結果を図７のグラフに示す。
A plaque adhesion test was performed using acrylic resin discs (test pieces) containing the surface-modified zinc oxide powder AD-PSJ at concentrations of 1.0% by mass and 0.5% by mass, respectively.
P. gingivalis, S. mutans, and C.I. The acrylic resin disk was immersed in 5 mL of a liquid medium to which 100 μL of each culture solution of albicans was added, and cultured for 18 hours. After incubation, the acrylic resin discs were washed three times with 1% phosphate-buffered saline (PBS). The acrylic resin disk was immersed in 5 mL of PBS, and the bacteria were detached from the acrylic resin disk by sonication for 1 minute using a Transsonic T780 (ultrasonic cleaner; manufactured by Elma Schmidbauer GmbH). The exfoliated bacterial suspension was diluted, smeared on an agar medium, cultured, and the number of viable bacteria was measured. The results are shown in the graph of FIG.
図７のグラフから、３種の口腔細菌ともに、表面改質酸化亜鉛粉末の濃度に依存してアクリルレジンディスクへの付着菌数が減少したことがわかる。
このことから、表面改質酸化亜鉛粉末を配合した歯科用樹脂材料に、プラークの付着抑制効果があることが確認された。
From the graph in FIG. 7, it can be seen that the number of bacteria adhering to the acrylic resin disk decreased depending on the concentration of the surface-modified zinc oxide powder for all three types of oral bacteria.
From this, it was confirmed that the dental resin material containing the surface-modified zinc oxide powder has the effect of suppressing adhesion of plaque.
試験例５：表面改質酸化亜鉛粉末を配合した樹脂材料の口臭抑制試験
表面改質酸化亜鉛粉末を配合した歯科用樹脂材料が、歯周病患者の強い口臭の原因物質であるメチルメルカプタン量を減少させることができるか否かを確認する。
Test Example 5: Halitosis inhibition test of resin material containing surface-modified zinc oxide powder See if it can be reduced.
表面改質酸化亜鉛粉末ＡＤ－ＰＳＪを、０．５％、１．０％、及び１．５％の含有率で配合したアクリルレジンディスク（試験片）及び表面改質酸化亜鉛粉末を配合していないアクリルレジンディスク（ｃｏｎｔｒｏｌ）を、Ｐ．ｇｉｎｇｉｖａｌｉｓの菌液へ浸潰し２日間培養した。培養後、アクリルレジンディスクを滅菌蒸留水で３回洗浄し、スペリアチューブに入れ、パラフィルムで密閉した。回転培養機ローテーターＲＴ－３０ｍｉｎｉ（タイテック株式会社製）にて転倒撹拌を行い、２日後にアクリルレジンディスクを新しいスペリアチューブへ移し替えて密封し、再度転倒撹拌を行った。２４時間後にＯｒａｌＣｈｒｏｍａ ＣＨＭ－１（ＮＩＳＳＨＡエフアイエス株式会社製）を用いてスペリアチューブ内のメチルメルカプタン（ＣＨ３ＳＨ）量を測定した。結果を表１に示す。 Surface-modified zinc oxide powder AD-PSJ was blended with acrylic resin discs (test pieces) at 0.5%, 1.0%, and 1.5% contents, and surface-modified zinc oxide powder was blended. The acrylic resin disk (control) without the P.C. gingivalis and cultured for 2 days. After incubation, the acrylic resin discs were washed three times with sterile distilled water, placed in speria tubes, and sealed with parafilm. Inverted stirring was carried out using a rotary incubator Rotator RT-30mini (manufactured by Taitec Co., Ltd.). Two days later, the acrylic resin disk was transferred to a new superior tube, sealed, and inverted and stirred again. After 24 hours, the amount of methyl mercaptan (CH 3 SH) in the superior tube was measured using OralChroma CHM-1 (manufactured by Nissha FIS Co., Ltd.). Table 1 shows the results.
表１の結果から、表面改質酸化亜鉛粉末を含有する樹脂材料は、Ｐ．ｇｉｎｇｉｖａｌｉｓが生産するメチルメルカプタンを減少させることがわかる。また、表面改質酸化亜鉛粉末の含有率に依存してメチルメルカプタン量がより大きく減少することがわかる。
このことから、表面改質酸化亜鉛粉末を配合した樹脂材料によって、歯周病患者の強い口臭の原因物質であるメチルメルカプタン量を減少させることができることが確認された。
From the results in Table 1, the resin material containing the surface-modified zinc oxide powder was P.I. gingivalis to reduce the amount of methyl mercaptan produced. Also, it can be seen that the amount of methyl mercaptan decreases more depending on the content of the surface-modified zinc oxide powder.
From this, it was confirmed that the resin material containing the surface-modified zinc oxide powder can reduce the amount of methyl mercaptan, which is a causative agent of strong bad breath in patients with periodontal disease.
試験例６：表面改質酸化亜鉛粉末を配合したナイトガードによる口臭抑制試験
被験者（歯周病患者）に、表面改質酸化亜鉛粉末を配合した樹脂材料で作製したナイトガードを装着してもらい、口臭の原因物質である揮発性硫化物（硫化水素Ｈ２Ｓ、メチルメルカプタンＣＨ３ＳＨ、及びジメチルサルファイド（ＣＨ３）２Ｓ）の量が減少するか否かを確認する。
尚、「ナイトガード」とは、睡眠中に使用するマウスピースであり、歯周病患者が、就寝中に歯ぎしりや歯を食いしばったりする場合にクッションとなって歯を保護するために用いる。
Test Example 6: Halitosis Suppression Test Using a Night Guard Formulated with Surface-Modified Zinc Oxide Powder A test subject (patient with periodontal disease) was asked to wear a night guard made of a resin material containing surface-modified zinc oxide powder. Check whether the amount of volatile sulfides (hydrogen sulfide H 2 S, methyl mercaptan CH 3 SH, and dimethyl sulfide (CH 3 ) 2 S), which are causative substances of bad breath, is reduced.
A "night guard" is a mouthpiece that is used during sleep, and is used by a periodontal disease patient to act as a cushion to protect teeth when they grind or clench their teeth while sleeping.
被験者に、就寝前に歯磨きをしてもらい、歯磨き直後の呼気中の３種類の揮発性硫化物の濃度（単位：ｐｐｂ）を口臭測定装置オーラルクロマ（ＮＩＳＳＨＡエフアイエス社製）で測定した。
次に、被験者に、表面改質酸化亜鉛粉末を配合していない樹脂材料で作製したナイトガードを装着して就寝してもらった。翌朝起床時の呼気中の３種類の揮発性硫化物の濃度（ｐｐｂ）を同様に測定した。
次の日に、被験者に、就寝前に歯磨きをしてもらい、表面改質酸化亜鉛粉末ＡＤ－ＰＳＪを１質量％配合した樹脂材料で作製したナイトガードを装着して就寝してもらった。翌朝起床時の呼気中の３種類の揮発性硫化物の濃度（ｐｐｂ）を同様に測定した。結果を表２に示す。
The subjects were asked to brush their teeth before going to bed, and the concentrations (unit: ppb) of the three types of volatile sulfides in the breath immediately after brushing were measured using a halitosis measuring device Oral Chroma (manufactured by Nissha FIS).
Next, the subjects were asked to sleep while wearing a night guard made of a resin material containing no surface-modified zinc oxide powder. Concentrations (ppb) of the three types of volatile sulfides in exhaled air upon waking up the next morning were similarly measured.
On the next day, the subjects brushed their teeth before going to bed, and went to bed wearing a night guard made of a resin material containing 1% by mass of surface-modified zinc oxide powder AD-PSJ. Concentrations (ppb) of the three types of volatile sulfides in exhaled air upon waking up the next morning were similarly measured. Table 2 shows the results.
表２の結果から、表面改質酸化亜鉛粉末を配合したナイトガードを装着することにより、３種類の口臭成分の濃度がそれぞれ約半分になったことがわかる。具体的には、硫化水素が４４％、メチルメルカプタンが５３％、ジメチルサルファイドが６４％に減少した。
このことから、表面改質酸化亜鉛粉末を配合した樹脂材料で作製したナイトガードによって歯周病患者の口臭の原因物質である揮発性硫化物を低減できることが確認された。
From the results in Table 2, it can be seen that the concentration of each of the three types of halitosis components was approximately halved by wearing the night guard containing the surface-modified zinc oxide powder. Specifically, hydrogen sulfide was reduced to 44%, methyl mercaptan to 53%, and dimethyl sulfide to 64%.
From this, it was confirmed that a night guard made of a resin material containing surface-modified zinc oxide powder can reduce volatile sulfides, which are causative substances of bad breath in patients with periodontal disease.
上記試験結果から、本発明の歯科用樹脂材料は、表面改質酸化亜鉛粉末を配合しても、表面改質酸化亜鉛粉末を配合していない樹脂と同等の吸水性、機械的強度等の特性を保持し、口腔細菌、特に歯周病原因菌に対する高い抗菌性を有し、口腔細菌の樹脂材料表面への付着が低減でき、口臭の原因物質である揮発性硫化物を抑制することができることがわかる。
From the above test results, the dental resin material of the present invention, even when the surface-modified zinc oxide powder is blended, has properties such as water absorption and mechanical strength equivalent to resins not blended with the surface-modified zinc oxide powder. , has high antibacterial properties against oral bacteria, especially periodontal disease-causing bacteria, can reduce adhesion of oral bacteria to the resin material surface, and can suppress volatile sulfides, which are causative substances of bad breath. I understand.
本発明の歯科用樹脂材料は、歯科領域で用いられる口腔内に適用される各種材料、治療過程で用いる一時的な詰め物、合着用セメント等の接着剤、固定して用いる被せ物、義歯、義歯床等の材料として有用である。その他、ナイトガード、歯ブラシの毛、歯ブラシの柄等としても用いることができる。
また、本発明の歯科用樹脂材料は、歯科領域だけでなく、例えば、ボクシング等のスポーツで用いられるマウスピース等の口腔内で用いる物品の樹脂材料としても有用である。
The dental resin material of the present invention includes various materials applied to the oral cavity used in the dental field, temporary fillings used in the course of treatment, adhesives such as luting cement, fixed coverings, dentures, and dentures. It is useful as a material for floors and the like. In addition, it can also be used as night guards, toothbrush bristles, toothbrush handles, and the like.
Moreover, the dental resin material of the present invention is useful not only in the dental field but also as a resin material for articles used in the oral cavity, such as mouthpieces used in sports such as boxing.
Claims (13)
A night guard made of the dental resin material according to any one of claims 1 to 11.
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