硅油中微量二甲基硅氧烷环体的定量分析研究

Study on the Quantitative Analysis of Trace Cyclicdimethylsiloxanes in Silicone Oil

性能优异的各种硅油是二甲基硅氧烷环体通过开环聚合而成,随着人们对二甲基硅氧烷环体毒性的进一步认识,非常有必要对硅油中二甲基硅氧烷环体残留量进行测定.本研究采用顶空-气相色谱法对硅油中4种常见二甲基硅氧烷环体(D3、D4、D5和D6)进行定量分析研究,通过优化不同溶剂、平衡温度、平衡时间、样品体积等因素,建立上述4种环体的同时定量方法.结果表明,各组分质量浓度在0.5~100μg/mL范围内具有良好的线性关系(r^2>0.999)、重现性(质量浓度在10μg/mL的RSD<2.5%),准确度(加标回收率在83.4%~99.9%之间),为硅油的质量控制提供参考.

Various silicone oil with excellent performance are produced by the polymerization of cyclicdimethylsiloxanes, and it is essential to determine the trace cyclicdimethylsiloxanes in silicone oil with the further understanding of their toxity. In this work, the quantitative analysis of four common cyclicdimethylsiloxanes （D3, D4, D5 and D6） in silicone oil is investigated by headspace-gas chromatography, and the simultaneous quantitation method is established by the optimization of different solvents, equilibrium temperature, equilibration time and sample volume. The results show that there is a good linear relationship in the concentration range of 0.5~100 μg/mL with r 2〉 0.999, RSD 〈6.34% at the concentration level of 10 μg/mL and spike recoveries between 83.43% and 99.87%, which provides a reference on the quality control of silicone oil.