镁掺杂羟基磷灰石复合树脂的制备及抗菌性能研究

Preparation of magnesium doped hydroxyapatite composite resin and its antibacterial property

目的用镁杂掺羟基磷灰石作为无机填料,制备实验用光固化牙科复合树脂材料,研究填料掺镁羟基磷灰石的含量对光固化复合树脂抗菌性能的影响。方法采用化学沉淀法制备的羟基磷灰石粉体与镁粉按照4∶1的比例均匀混合,在200 MPa的压力下压制成型,经高温1200℃烧结,制备出掺镁羟基磷灰石。采用水解法以硅烷偶联剂(KH570)改性处理掺镁羟基磷灰石后作为无机填料;双酚A-甲基丙烯酸缩水甘油酯(Bis-GMA)为树脂单体,二甲基丙烯酸三甘油酯(TEGDMA)为稀释剂,按6∶4(质量比)比例混合组成树脂基质;樟脑醌(CQ)与叔胺(EMADMA)混合组成光引发体系;然后将树脂基质、无机填料、光引发体系混合均匀进行光固化,制备出实验用牙科修复复合树脂填充材料。利用扫描电镜(SEM)及能谱仪(EDS)观察填料粒子的分布及复合树脂表面的元素分布情况。采用覆膜法衡量材料的抗菌性能。结果填料在树脂基质中分布均匀,并随着填料含量的增加,复合树脂的抗菌性逐渐增强。结论填料掺镁羟基磷灰石中的纳米氧化镁赋予复合树脂材料较强抗菌性,在实验范围内,随着填料含量的增加,复合树脂的抗菌性增大,当填料含量达到40mass%,复合树脂的抗菌率高达99.13%。

Objective Light cured dental composite resin materials were prepared with magnesium doped hydroxyapatite as the inorganic filler. The effect of the content of magnesium doped hydroxyapatite on the antibacterial properties of the composite resin was studied. Methods The magnesium doped hydroxyapatite was prepared using chemical precipitation method by mixing homogeneously magnesium powder with hydroxyapatite powder in the ratio of 4 ∶ 1（ mass ratio）,sintered in high temperature of 1200℃ and pressed at 200 MPa pressure. Magnesium doped hydroxyapatite treated by silane coupling agent（ KH570）was taken as the inorganic filler. The bisphenol A-glycol methacrylate（ Bis-GMA） was used as the resin monomers,and the triethylene glycol dimethacrylate（ TEGDMA） was taken as diluents to be blended in the ratio 6∶ 4（ mass ratio） to form the resin matrixes; The photoinitiating system was composed by blending the camphor quinon（ CQ） with dimethylaminoethyl methacrylate（ DMAEMA）; The distribution of filler particles and the elements distribution of the surface of composite resin were observed by SEM and EDS. The antimicrobial properties of the material were measured by the method of the PE film coating.Results The filler was evenly distributed in the resin matrix,and the antimicrobial properties of compound resin is gradually enhanced with the increase of the filler content. Conclusions The nanometer magnesia in the magnesium doped hydroxyapatite filler gives the composite resin a strong antibacterial property. Antibacterial activity would be increased with the increase of filler content. When the content of magnesium doped hydroxyapatite is 40 mass%,the antibacterial rate is up to 99. 13%.