Department of Chemistry and Center for Nanotechnology at CYCU, Chung Yuan Christian University, Chung-Li 320, Taiwan.
Talanta. 2010 Sep 15;82(4):1426-33. doi: 10.1016/j.talanta.2010.07.014. Epub 2010 Jul 13.
In this study, several organic polymer-based monoliths prepared by single step in situ copolymerization of styrene- and methacrylate ester-based monomers (styrene (S), divinylbenzene (DVB) and lauryl methacrylate (LMA)) were developed as stationary phases of capillary electrochromatography (CEC) for the analyses of synthetic antioxidants. These monoliths were characterized by examining the SEM image, IR spectrum, and measuring the pore size, surface area, conversion yield, and thermal decomposition temperature. The polymerization procedure was optimized by varying the reaction temperature, the reaction time, and the LMA-styrene ratio. The LMA-styrene ratio had the most significant influence on the peak symmetry of butylated hydroxyanisole (BHA) and 2, 6-di-tert-butyl-4-methyl phenol (BHT), the latter being greatly affected by excessive peak tailing in the poly(S-DVB) monolith. It showed that the interaction between the poly(S-DVB) monolith and the antioxidant (BHT or BHA) was significantly altered by the insertion of LMA. Compared with the best HPLC and CE methods previously reported, this proposed CEC method provides a comparable separation ability for the five antioxidants analyzed. This study demonstrates that the potentiality of poly(S-DVB-LMA) monolith as stationary phase, especially for CEC system, because of high thermal stability and good column reproducibility.
在这项研究中，通过一步原位共聚苯乙烯和甲基丙烯酸酯基单体（苯乙烯（S）、二乙烯基苯（DVB）和月桂基甲基丙烯酸酯（LMA））合成了几种基于有机聚合物的整体柱，作为毛细管电色谱（CEC）的固定相，用于合成抗氧化剂的分析。通过检查 SEM 图像、IR 光谱、测量孔径、表面积、转化率和热分解温度来对这些整体柱进行了表征。通过改变反应温度、反应时间和 LMA-苯乙烯比例优化了聚合过程。LMA-苯乙烯比例对丁基羟基茴香醚（BHA）和 2,6-二叔丁基-4-甲基苯酚（BHT）的峰对称性影响最大，后者在聚（S-DVB）整体柱中受到过度峰拖尾的极大影响。结果表明，LMA 的插入显著改变了聚（S-DVB）整体柱与抗氧化剂（BHT 或 BHA）之间的相互作用。与之前报道的最佳 HPLC 和 CE 方法相比，该提议的 CEC 方法对分析的五种抗氧化剂具有相当的分离能力。本研究表明，聚（S-DVB-LMA）整体柱作为固定相具有潜力，特别是对于 CEC 系统，因为它具有高热稳定性和良好的柱重现性。
