Almusa Arwa, Delgado António H S, Ashley Paul, Young Anne M
Division of Biomaterials and Tissue Engineering, UCL Eastman Dental Institute, London WC1X 8DA, UK.
Centro de Investigação Interdisciplinar Egas Moniz (CiiEM), Monte de Caparica, 2829-511 Almada, Portugal.
Polymers (Basel). 2021 Nov 10;13(22):3886. doi: 10.3390/polym13223886.
The of this study aim was to develop a rapid method to determine the chemical composition, solvent evaporation rates, and polymerization kinetics of dental adhesives. Single-component, acetone-containing adhesives One-Step (OS; Bisco, Anaheim, CA, USA), Optibond Universal (OU; Kerr, Brea, CA, USA), and G-Bond (GB; GC, Tokyo, Japan) were studied. Filler levels were determined gravimetrically. Monomers and solvents were quantified by comparing their pure Attenuated Total Reflectance-Fourier Transform Infra-Red (ATR-FTIR) spectra, summed in different ratios, with those of the adhesives. Spectral changes at 37 °C, throughout passive evaporation for 5 min, then polymerisation initiated by 20 s, and blue light emitting diode (LED) (600 mW/cm) exposure ( = 3) were determined. Evaporation and polymerisation extent versus time and final changes were calculated using acetone (1360 cm) and methacrylate (1320 cm) peaks. OS, OU, and GB filler contents were 0, 9.6, and 5.3%. FTIR suggested OS and OU were Bis-GMA based, GB was urethane dimethacrylate (UDMA) based, and that each had a different diluent and acidic monomers and possible UDMA/acetone interactions. Furthermore, initial acetone percentages were all 40-50%. After 5 min drying, they were 0% for OS and OU but 10% for GB. Whilst OS had no water, that in OU declined from 18 to 10% and in GB from 25 to 20% upon drying. Evaporation extents were 50% of final levels at 23, 25, and 113 s for OS, OU, and GB, respectively. Polymerisation extents were all 50 and 80% of final levels before 10 and at 20 s of light exposure, respectively. Final monomer polymerisation levels were 68, 69, and 88% for OS, OU, and GB, respectively. An appreciation of initial and final adhesive chemistry is important for understanding the properties. The rates of evaporation and polymerisation provide indications of relative required drying and light cure times. UDMA/acetone interactions might explain the considerably greater drying time of GB.
本研究旨在开发一种快速方法，以测定牙科粘合剂的化学成分、溶剂蒸发速率和聚合动力学。对单组分含丙酮粘合剂一步胶（OS；美国加利福尼亚州阿纳海姆市的Bisco公司）、通用Optibond粘合剂（OU；美国加利福尼亚州布雷亚市的 Kerr公司）和G-Bond粘合剂（GB；日本东京的GC公司）进行了研究。通过重量法测定填料含量。通过将不同比例混合的纯单体和溶剂的衰减全反射傅里叶变换红外光谱（ATR-FTIR）与粘合剂的光谱进行比较，对单体和溶剂进行定量分析。测定了37℃下5分钟被动蒸发过程中的光谱变化，然后引发聚合20秒，并进行蓝光发光二极管（LED）（600 mW/cm）照射（=3）。利用丙酮（1360 cm）和甲基丙烯酸酯（1320 cm）峰计算蒸发和聚合程度随时间的变化以及最终变化。OS、OU和GB的填料含量分别为0%、9.6%和5.3%。傅里叶变换红外光谱表明，OS和OU以双酚A甲基丙烯酸缩水甘油酯（Bis-GMA）为基础，GB以聚氨酯二甲基丙烯酸酯（UDMA）为基础，且每种粘合剂都有不同的稀释剂和酸性单体以及可能的UDMA/丙酮相互作用。此外，初始丙酮百分比均为40-50%。干燥5分钟后，OS和OU中的丙酮百分比为0%，而GB中的为10%。干燥时，OS中无水，OU中的水含量从18%降至10%，GB中的水含量从25%降至20%。OS、OU和GB的蒸发程度分别在23秒、25秒和113秒达到最终水平的50%。在光照10秒前和20秒时，聚合程度分别达到最终水平的50%和80%。OS、OU和GB的最终单体聚合水平分别为68%、69%和88%。了解粘合剂初始和最终的化学性质对于理解其性能很重要。蒸发速率和聚合速率表明了相对所需的干燥时间和光固化时间。UDMA/丙酮相互作用可能解释了GB干燥时间长得多的原因。
