牙科释氟材料缓释氟及再充氟性能的研究

发布时间：2018-01-07 05:44

本文关键词：牙科释氟材料缓释氟及再充氟性能的研究　出处：《第四军医大学》2013年硕士论文　论文类型：学位论文

【摘要】：具有释氟性和再充氟性能的牙齿充填修复材料能够提高充填物周围牙齿硬组织的抗脱矿、抗龋坏能力，预防或延缓充填物边缘继发龋的发生，延长修复体的寿命。测定、评价充填材料的释氟性和再充氟性是研究释氟性修复材料有效性的重要方面。研究目的：建立牙科材料释氟和再充氟性能的研究测试平台，评价自制的释氟性复合树脂及目前市售的释氟性修复材料的缓释氟性能和再充氟性能，探讨释氟性材料释氟及再充氟的特点、机制及其影响因素，为研制、改进新型释氟性材料释氟性能提供试验依据。材料与方法： 1.常用释氟充填材料缓释氟及再充氟性能的体外测定用8种充填材料（玻璃离子水门汀：Fuji IX、Fuji II LC、Fuji VII，复合体：Compoglass、Beautifil，复合树脂：Z350、Charisma及试验I型释氟性复合树脂）分别制备直径10mm、厚度1mm的试样。将每个试样浸入盛有5ml去离子水的聚乙烯小瓶中进行浸泡，每天更换浸泡液，至第28天。取出试样，吹干后浸入1.23％氟化泡沫中进行4min氟再充，流水冲洗后再浸泡于5ml去离子水中，浸泡7天，每天更换浸泡液。用氟离子选择电极测定每天的浸泡液中氟离子浓度。 2.释氟性充填材料的表面形貌观测及能谱分析每种材料选取4个时间点（未浸水、浸水24h、浸水28天和浸水28天+充氟后24h）的试样，常规干燥喷金后在扫描电镜下观测材料表面微观结构，并进行表面元素能谱分析。 3.氟化物涂膜抑制釉质脱矿的研究选用6种氟化物涂膜，分别为Duraphat（含5%氟化钠）及5种不同的成膜基质（渗透型丙烯酸树脂、珂巴树脂、聚合松香、聚乙烯醇缩丁醛、甲基丙烯酸乙酯共聚树脂）配制的氟化物涂膜。将新鲜拔除的牛切牙，制备成5mm×5mm×3mm大小的釉质块，随机分成6组涂布6中氟涂膜，每组15个。试样进行pH循环7d后测定并计算脱矿前后釉质表面荧光强度的变化率（△F%）和显微硬度的变化率（%SMHC）。 4.成膜基质对氟化物涂膜抑制釉质脱矿深度的影响釉质块分别涂布6种氟涂膜，经过pH循环7d后，纵向切开，暴露剖面重新包埋，用硬组织切片机制备厚100m的釉质切片，中性树胶封片后于偏光显微镜下测量脱矿深度。实验结果： 1.玻璃离子水门汀类充填材料表现出初期爆发性释氟特点，浸水后3天释氟性趋于平缓，其他材料初期爆发性释氟不明显。浸水28天后，3种玻璃离子水门汀的释放值较高，复合体和复合树脂的释氟值较低。对所有材料进行氟再充后24h，各材料的氟离子释放量均显著增加，其中释氟增加幅度最大的是FujiVII和Fuji II LC，其次是Fuji IX、Beautifil和试验I型释氟性复合树脂，Compoglass，Z350和Charisma的释氟增加幅度最低。氟再充后的2~3天各材料释氟值逐渐下降，在3~4天后基本恢复到之前的水平。 2.扫描电镜观察发现各种充填材料因材料类型不同，，表面形貌各有差异，浸水28天后，均有不同程度的溶蚀现象，其中以Beautifil的溶解后留下的孔洞最明显，溶蚀现象主要发生在填料边缘及填料与基质的结合处，而玻璃离子类材料和复合树脂的表面溶解现象较轻微。能谱分析的结果表明玻璃离子类材料氟离子主要聚集在未反应完全的玻璃颗粒中，复合体、Beautifil和试验I型释氟性复合树脂的氟离子主要聚集在填料中所含的玻璃粉中，复合树脂由于自身含氟量极低，而且表面致密，溶解度小，故氟离子的释放与再充均不明显。 3. pH循环能够有效地使釉质发生脱矿，在釉质表面应用氟化物涂膜，能够显著提高牙釉质的抗脱矿能力，以含渗透型丙烯酸树脂的氟涂膜组的荧光损失量和显微硬度值的下降率最小，提示其抗脱矿能力最好。 4.偏光显微镜下正常釉质呈负性双折射（透光），实验区域早期龋显示以表层下脱矿为主要特征的病理改变，呈负性双折射的表层和紧接下面呈正性双折射(不透光)的病损体部。脱矿深度检测发现，渗透型丙烯酸组的脱矿深度显著小于其他涂膜组。结论：（1）材料的缓释氟性能与材料的类型密切相关，玻璃离子类材料释氟性较强。（2）材料的再充氟性能除与材料的类型有关外，还可能与材料溶解后的孔隙度及致密度有关。（3）表面形貌观察和能谱分析发现，大多数材料的氟离子释放均主要来源于成分中玻璃颗粒的溶蚀。（4）氟化物涂膜具有明显的抑制釉质早期龋损脱矿的作用，含渗透型丙烯酸树脂的氟涂膜效果优于其他组。
[Abstract]:With fluoride releasing and fluorine filling performance of dental filling repair materials can improve the anti demineralization filling around dental hard tissue, anti caries ability, prevent or delay the occurrence of secondary caries filling edge, extend the restoration of life. By evaluation of filling materials fluoride releasing and refilling of fluoride is study on the effectiveness of fluoride release important repair materials.
The purpose of the study is:
The establishment of dental materials and then study the fluoride release test platform of fluorine filling performance, evaluation of self-made fluoride releasing composite resin and the current commercially available fluoride releasing restorative materials and properties of slow-release fluoride fluorine filling performance, explore the characteristics of fluoride releasing materials and then release fluoride fluorine filling, factors, mechanism and its influence for the development of the new, improved fluoride releasing materials to provide the experimental basis for the fluoride release performance.
Materials and methods:
In vitro determination of fluorine and recharge performance of 1. commonly used fluorine release materials
Using 8 kinds of filling materials (glass ionomer cement: Fuji IX, Fuji II LC, Fuji VII, Compoglass, Beautifil, complex: composite resin: Z350, Charisma and test of I fluoride releasing composite resin) were prepared by the diameter of 10mm, thickness of 1mm. Each sample was immersed in Sheng soaked polyethylene vials with 5ml deionized water, soaking liquid changed every day, and twenty-eighth days. The specimen is removed, dried after immersion of 1.23% fluoride foam in 4min fluoride charge again, rinse water after soaking in 5ml deionized water for 7 days, every day. The replacement of soaking liquid fluoride concentration soaking solution was measured daily by fluorine ion selective electrode.
Surface morphology observation and energy spectrum analysis of 2. fluorinated filling materials
Each material was selected for 4 time points (unsoaked, 24h, 28 days and 28 days + 24h). After conventional drying, the microstructure of the material surface was observed under scanning electron microscope, and the surface element energy spectrum was analyzed.
Study on the inhibition of enamel demineralization by 3. fluoride coating
Using 6 kinds of fluoride varnish respectively, Duraphat (containing 5% sodium fluoride) and 5 kinds of film matrix (osmotic acrylic resin, copal resin, polymerized rosin, polyvinyl butyral, ethyl methacrylate copolymer resin) fluoride varnish prepared. The freshly extracted bovine incisors, prepared enamel pieces of 5mm * 5mm * the size of 3mm, were randomly divided into 6 groups of 6 fluorine coating film, each group of 15 samples. PH after 7d were determined before and after demineralization of enamel surface changes in fluorescence intensity ratio (F%) and the microhardness variation rate (%SMHC).
Effect of 4. film matrix on the inhibition of enamel demineralization by fluoride coating
The enamel blocks are respectively coated 6 fluorine coating, through the pH cycle 7d, longitudinal incision, exposure profile re embedding, with hard tissue slicing mechanism by 100m slice thick enamel, neutral balata in polarizing microscope measurement of demineralization depth.
Experimental results:
1. glass ionomer filling materials exhibit initial explosive fluoride release characteristics, after 3 days of fluoride releasing slowly, other material initial explosive fluoride release was not obvious. After 28 days, 3 kinds of glass ionomer cement release value is high, complex and composite resin fluoride release value is low. All the materials were fluoride rechargeable 24h after the release of fluoride materials were increased significantly, of which the largest increase of fluoride release is FujiVII Fuji and II LC, followed by Fuji IX, Beautifil and test of I fluoride releasing composite resin, Compoglass, Z350 and Charisma increased. The lowest fluoride fluoride release and then charge after 2~3 each day the material release fluoride decreased in 3~4 days before the return to the basic level.
Observation of various filling materials due to material type SEM of 2. different surface morphologies are different, soaking for 28 days, had different degrees of dissolution, the void left by the dissolution of Beautifil after the most obvious corrosion phenomenon occurred mainly in the filler filler and matrix and edge joints, and the phenomenon of surface dissolution of glass ionomer materials and composite resin is slight. Spectrum analysis results show that the glass ionomer materials fluoride ions gathered in the unreacted glass particles completely in complex fluoride Beautifil and test I fluoride releasing composite resin contained in the main gathering in the packing of glass powder, because of its containing composite resin fluorine content is extremely low, and dense surface, the solubility of small, so the release of fluoride and charge are not obvious.
The 3. pH cycle can effectively make the enamel demineralization occurred in the application of fluoride varnish, enamel surface, can significantly improve the ability of anti demineralization of enamel, with the decrease of fluorine containing osmotic acrylic resin coating group fluorescence loss and the microhardness values were the lowest, suggesting that the anti demineralization ability best.
4. normal enamel under polarizing microscope showed negative birefringence (light), the experimental area of early caries showed pathological changes in subsurface demineralization as the main feature of the negatively birefringent surface and then following positive birefringence (opaque) of the body. The detection of demineralization depth, demineralization the depth of penetration of acrylic group was significantly less than that of other film group.
Conclusion:
(1) the performance of the sustained release fluorine of the material is closely related to the type of the material, and the fluorine property of the glass ion material is stronger.
(2) the recharge performance of the material is related to the type of material, and it may be related to the porosity and density after the dissolution of the material.
(3) the surface morphology observation and the energy spectrum analysis show that the release of fluorine ions in most materials is mainly due to the dissolution of glass particles in the composition.
(4) the fluoride coating can obviously inhibit the demineralization of early enamel, and the effect of fluorine coating with osmotic acrylic resin is better than that of other groups.

【学位授予单位】：第四军医大学
【学位级别】：硕士
【学位授予年份】：2013
【分类号】：R783.1

【引证文献】