采用高效液相色谱法（HPLC）和顶空-气相色谱/质谱联用仪（headspace-GC/MS）分析树枝状甲基丙烯酸酯共聚物及复合材料中的残留单体。

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

作者信息

Viljanen Eeva K, Langer Sarka, Skrifvars Mikael, Vallittu Pekka K

机构信息

Department of Prosthetic Dentistry and Biomaterials Science, University of Turku, Institute of Dentistry, Lemminkäisenkatu 2, FI-20520 Turku, Finland.

出版信息

Dent Mater. 2006 Sep;22(9):845-51. doi: 10.1016/j.dental.2005.11.012. Epub 2005 Dec 27.

DOI:10.1016/j.dental.2005.11.012

PMID:16380160

Abstract

OBJECTIVES

The aim of this study was to analyze the residual monomer content of photopolymerized 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 photopolymerization 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.

摘要

目的

本研究旨在分析光聚合树枝状甲基丙烯酸酯共聚物和颗粒填料复合材料中的残留单体含量。将顶空气相色谱/质谱联用仪（HS-GC/MS）与高效液相色谱（HPLC）进行比较。

方法

树脂混合物由树枝状甲基丙烯酸酯单体、甲基丙烯酸甲酯和乙酰乙酸乙酯甲基丙烯酸酯按不同比例组成。此外，其中一种复合材料含有1,4-丁二醇二甲基丙烯酸酯。樟脑醌和2-（N，N-二甲基氨基）乙基甲基丙烯酸酯用作光活化引发体系。用HPLC和HS-GC/MS分析光聚合40秒后残留甲基丙烯酸甲酯和乙酰乙酸乙酯甲基丙烯酸酯的含量。