Methacrylate peak determination and selection recommendations using ATR-FTIR to investigate polymerisation of dental methacrylate mixtures.
Methacrylate peak determination and selection recommendations using ATR-FTIR to investigate polymerisation of dental methacrylate mixtures.
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DOI：
10.1371/journal.pone.0252999
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发表时间：
2021
期刊：
影响因子：
3.7
通讯作者：
Young AM
中科院分区：
文献类型：
--
作者：
Delgado AHS;Young AM
使用ATR-FTIR系统研究聚合动力学在许多牙科研究中是常见的。然而，计算单体-聚合物转化率的峰选择方法可以变化，从而影响最终结果。因此，本研究的目的是通过实验来确认哪种方法不太容易出现系统误差。测试了三种商业修复材料-Vertise Flow（VF），Constic和Activa Bioactive Restorative Kids。首先，衰减全反射傅里叶变换（全反射红外光谱）（Spectrum One，Perkin-Elmer，UK）获得单体的光谱-磷酸二氢10-甲基丙烯酰氧基癸酯（10-MDP）、双酚-A二甲基丙烯酸缩水甘油酯（Bis-GMA）、甲基丙烯酸2-羟乙酯（HEMA）、二甲基丙烯酸三乙二醇酯（TEGDMA）和二甲基丙烯酸氨基甲酸酯（UDMA）以研究甲基丙烯酸酯峰高与浓度的比例。评估修复材料的2 mm盘（照射20秒，LED固化单元1100-1330 mW/cm 2）在光暴露后的光谱变化，以研究聚合动力学（n = 3），在光暴露之前、期间和之后连续采集光谱。使用1320/1336、1320/1350和1636/1648 cm-1作为反应/参比峰，计算峰差和转化度（DC %）。推理统计包括MANOVA和受试者内重复测量ANOVA设计（5%显著性水平）。证实了甲基丙烯酸酯峰高与浓度的比例关系，1320/1352 cm-1峰组合显示出最低的变异系数（8%）。聚合反应的差谱显示在1500-1800 cm-1区域附近的噪声干扰。在不同的材料中，DC %结果高度依赖于峰选择（p<0.001），1636 cm-1的变异性更高。仅当使用1320 cm-1峰时才检测到材料的显著差异（p<0.05）。在相同材料内，Constic和Activa的方法显著不同（p<0.05）。可以得出结论，1320 cm-1峰更适合评估甲基丙烯酸酯的聚合，因此推荐使用。
Investigation of polymerisation kinetics using ATR-FTIR systems is common in many dental studies. However, peak selection methods to calculate monomer-polymer conversion can vary, consequently affecting final results. Thus, the aim of this study is to experimentally confirm which method is less prone to systematic errors. Three commercial restorative materials were tested–Vertise Flow (VF), Constic and Activa Bioactive Restorative Kids. Firstly, Attenuated Total Reflectance Fourier Transform Infra-Red (ATR-FTIR) (Spectrum One, Perkin-Elmer, UK) spectra of monomers were acquired—10-methacryloyloxy decyl dihydrogen phosphate (10-MDP), bisphenol-A glycidyl dimethacrylate (Bis-GMA), 2-hydroxyethyl methacrylate (HEMA), triethyelene glycol dimethacrylate (TEGDMA) and urethane dimethacrylate (UDMA) to investigate proportionality of methacrylate peak heights versus concentration. Spectral changes upon light exposure of 2 mm discs of the restorative materials (irradiated for 20 s, LED curing unit 1100–1330 mW/cm2) were assessed to study polymerisation kinetics (n = 3), with continuous acquisition of spectra, before, during and after light exposure. Peak differences and degrees of conversion (DC %) were calculated using 1320/1336, 1320/1350 and 1636/1648 cm-1 as reaction/reference peaks. Inferential statistics included a MANOVA and within-subjects repeated measures ANOVA design (5% significance level). Proportionality of methacrylate peak height to concentration was confirmed, with the 1320/1352 cm-1 peak combination showing the lowest coefficient of variation (8%). Difference spectra of the polymerisation reaction showed noise interference around the 1500–1800 cm-1 region. Across the different materials, DC % results are highly dependent upon peak selection (p<0.001), with higher variability associated to the 1636 cm-1. Significant differences in the materials were only detected when the 1320 cm-1 peak was used (p<0.05). Within the same materials, methods were significantly different for Constic and Activa (p<0.05). It is possible to conclude that the 1320 cm-1 peak is more adequate to assess polymerisation of methacrylates and is therefore recommended.
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影响因子：
5
作者：
Aljabo, A.;Xia, W.;Young, A. M.
通讯作者：
Young, A. M.
影响因子：
13.1
作者：
Chalmers, JM;Everall, NJ
通讯作者：
Everall, NJ
影响因子：
4.2
作者：
Derenne, Allison;Verdonck, Magali;Goormaghtigh, Erik
通讯作者：
Goormaghtigh, Erik
DOI：
10.1007/s10856-014-5370-6
发表时间：
2015-01-01
影响因子：
3.7
作者：
Barbosa, Marilia Oliveira;de Carvalho, Rodrigo Varella;da Silva, Adriana Fernandes
通讯作者：
da Silva, Adriana Fernandes
影响因子：
2.2
作者：
Borges, B. C. D.;Souza-Junior, E. J.;Sinhoreti, M. A. C.
通讯作者：
Sinhoreti, M. A. C.