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模拟牙科粘结系统的衰减全反射傅里叶变换红外光谱以研究其组成和聚合动力学。

Modelling ATR-FTIR Spectra of Dental Bonding Systems to Investigate Composition and Polymerisation Kinetics.

作者信息

Delgado António Hs, Young Anne M

机构信息

Division of Biomaterials & Tissue Engineering, UCL Eastman Dental Institute, London NW3 2PF, UK.

Centro de Investigação Interdisciplinar Egas Moniz (CiiEM), Clinical Research Unit, Instituto Universitário Egas Moniz (IUEM), 2829-511 Caparica, Portugal.

出版信息

Materials (Basel). 2021 Feb 5;14(4):760. doi: 10.3390/ma14040760.

Abstract

Component ratios and kinetics are key to understanding and optimising novel formulations. This warrants investigation of valid methods. Attenuated Total Reflectance Fourier Transform Infra-Red (ATR)-FTIR spectra of separate primers/adhesives were modelled using summed spectra of solvents (water, ethanol), methacrylate monomers (HEMA (hydroxyethyl methacrylate), Bis-GMA (bisphenol A glycidyl methacrylate), and 10-MDP (10-methacryloyloxydecyl dihydrogen phosphate)), and fillers, multiplied by varying fractions. Filler loads were obtained following their separation from the adhesives, by analysing three repetitions ( = 3). Spectral changes during light exposure at 37 °C (20 s, LED 1100-1330 mW/cm) were used to determine polymerisation kinetics ( = 3). Independent samples T-test was used for statistical analysis (significance level of 5%). FTIR modelling suggested a primer solvent percentage of OBFL (Optibond FL) (30%) was half that of CFSE (Clearfil SE 2) (60%). OBFL included ethanol and water, while CFSE included only water. Monomer peaks were largely those of HEMA with lower levels of phosphate monomers. OBFL/CFSE adhesive model spectra suggested that both contained equal volumes of Bis-GMA/HEMA, with CFSE having 10-MDP. Filler levels and spectra from OBFL (48 wt.%) and CFSE (5 wt.%) were different. Both systems reached a 50% conversion rate within seconds of light exposure. The final conversion for OBFL (74 ± 1%) was lower compared to CFSE (79 ± 2%) ( < 0.05). ATR-FTIR is a useful method to investigate relative levels of main components in bonding systems and their polymerisation kinetics. Such information is valuable to understanding such behaviour.

摘要

成分比例和动力学是理解和优化新型配方的关键。这就需要对有效方法进行研究。使用溶剂(水、乙醇)、甲基丙烯酸酯单体(甲基丙烯酸羟乙酯(HEMA)、双酚A缩水甘油醚甲基丙烯酸酯(Bis - GMA)和10 - 甲基丙烯酰氧基癸基二氢磷酸酯(10 - MDP))以及填料的总和光谱,并乘以不同的分数,对单独的底漆/粘合剂的衰减全反射傅里叶变换红外(ATR)-FTIR光谱进行建模。通过分析三次重复实验(n = 3),在将填料与粘合剂分离后获得填料负载量。利用在37℃光照(20秒,LED 1100 - 1330 mW/cm)期间的光谱变化来确定聚合动力学(n = 3)。采用独立样本T检验进行统计分析(显著性水平为5%)。FTIR建模表明,Optibond FL(OBFL)底漆的溶剂百分比(30%)是Clearfil SE 2(CFSE)底漆(60%)的一半。OBFL包含乙醇和水,而CFSE仅包含水。单体峰主要是HEMA的峰,磷酸酯单体含量较低。OBFL/CFSE粘合剂模型光谱表明,两者都含有等量体积的Bis - GMA/HEMA,CFSE含有10 - MDP。OBFL(48 wt.%)和CFSE(5 wt.%)的填料含量和光谱不同。两个体系在光照后几秒钟内都达到了50%的转化率。与CFSE(79±2%)相比,OBFL的最终转化率(74±1%)较低(p < 0.05)。ATR - FTIR是研究粘结体系中主要成分的相对含量及其聚合动力学的有用方法。这些信息对于理解此类行为很有价值。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/d815/7915020/6cfca107ee6d/materials-14-00760-g001.jpg

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