Bioactive glass composite for orthodontic adhesives - Formation and characterisation of apatites using MAS-NMR and SEM.

Abstract

OBJECTIVES: To study the dissolution and fluoroapatite (FAP) formation of a new bioactive glass (BAG)-resin adhesive in an acidic solution in reference to neutral solutions, using the magic angle spinning-nuclear magnetic resonance (MAS-NMR) and the scanning electron microscopy (SEM). METHODS: BAG composite disks (n = 90) were prepared from, novel fluoride-containing BAG-resin. Three sample groups (n = 30) of the disks were immersed in Tris buffer pH = 7.3 (TB), neutral artificial saliva pH = 7 (AS7) and acidic artificial saliva pH = 4 (AS4) at ten time points (from 6 h to 6 months). Half of the immersed disks at each time point were crushed into a powder and investigated by the solid state MAS-NMR. SEM studies were undertaken by embedding the other half of the immersed disk in a self-cure acrylic where the fracture surface was imaged. RESULTS: MAS-NMR results show that the BAG composite degraded significantly faster in AS4 compared to TB and AS7. At the end of the immersion period (6 months), around 80% of the glass particles in AS4 had reacted to form an apatite, evidenced by the sharp peak at 2.82 ppm in 31P signals compared to a broader peak in TB and AS7. It also shows evidence of fluorapatite (FAP) formation, indicated by 19F signal at -103 ppm, while signal around -108 ppm indicated the formation of calcium fluoride, from the excess Ca2+ and F- especially on longer immersion. SEM images confirm higher degradation rate of the BAG composite in AS4 and reveal the impact of time on the dissolution of more glass particles. The images also indicate apatite formation around the glass particles in TB and AS4, while it forms predominantly over the disk surface in AS7. SIGNIFICANCE: BAG composite demonstrate smart reactivity in response to pH change which has a potential clinical benefit against demineralization and promoting remineralisation to form more stable fluorapatites.