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Analysis of residual monomers in dendritic methacrylate copolymers and composites by HPLC and headspace-GC/MS

机译:HPLC和顶空-GC / MS分析树枝状甲基丙烯酸酯共聚物和复合材料中的残留单体

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Objectives. The aim of this study was to analyze the residual monomer content of photopoly-merized dendritic methacrylate copolymers and particulate filler composites. Headspace-gas chromatography/mass spectrometry (HS-GC/MS) was compared with high performance liquid chromatography (HPLC). Methods. The resin mixtures consisted of a dendritic methacrylate monomer, methyl methacrylate and acetoacetoxyethyl methacrylate in varied proportions. In addition, one of the composites contained 1,4-butanediol dimethacrylate. Camphorquinone and 2-(N,N-dimethylamino)ethyl methacrylate were used as the light-activated initiator system. The content of residual methyl methacrylate and acetoacetoxyethyl methacrylate after 40 s pho-topolymerization were analyzed with HPLC and HS-GC/MS. Results. The content of residual methyl methacrylate decreased and residual acetoacetoxyethyl methacrylate increased with increasing concentration of acetoacetoxyethyl methacrylate in the resin mixture. The results with both methods had the same trend. Significance. The addition of acetoacetoxyethyl methacrylate enhanced the copolymerization of methyl methacrylate, but did not decrease the total residual monomer content. The HS-GC/MS method was found to be a feasible method in the analysis of low-boiling residuals in dental polymers.
机译:目标。这项研究的目的是分析光聚合的树枝状甲基丙烯酸共聚物和颗粒状填料复合材料的残留单体含量。将顶空-气相色谱/质谱(HS-GC / MS)与高效液相色谱(HPLC)进行了比较。方法。树脂混合物由不同比例的树枝状甲基丙烯酸酯单体,甲基丙烯酸甲酯和甲基丙烯酸乙酰乙酰氧基乙酯组成。另外,一种复合材料包含1,4-丁二醇二甲基丙烯酸酯。樟脑醌和甲基丙烯酸2-(N,N-二甲基氨基)乙酯用作光活化引发剂体系。用HPLC和HS-GC / MS分析40 s光聚合后的残留甲基丙烯酸甲酯和甲基乙酰乙酰氧基乙酯的含量。结果。随着树脂混合物中甲基丙烯酸乙酰乙酰氧基乙酯浓度的增加,甲基丙烯酸甲酯残留的含量降低,甲基丙烯酸乙酰乙酰氧基乙基酯的含量增加。两种方法的结果趋势相同。意义。甲基丙烯酸乙酰乙酰氧基乙酯的加入增强了甲基丙烯酸甲酯的共聚作用,但没有降低总残留单体含量。发现HS-GC / MS方法是分析牙科聚合物中低沸点残留物的可行方法。

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