College of Pharmacy, Hebei University, Hebei Province Key Laboratory of Pharmaceutical Quality Control, Baoding 071002, China.
College of Pharmacy, Hebei University, Hebei Province Key Laboratory of Pharmaceutical Quality Control, Baoding 071002, China.
J Chromatogr A. 2014 Jan 10;1324:128-34. doi: 10.1016/j.chroma.2013.11.029. Epub 2013 Nov 19.
A porous monolith was prepared by in situ free-radical polymerization using N-isopropylacrylamide (NIPAAm) and trimethylol propane triacrylate (TMPTA) as functional monomers, ethylene dimethacrylate (EDMA) as crosslinking agent. The chemical group of the monolith was assayed by a Fourier transform infrared spectroscopy (FT-IR) method and the morphology of optimized monolithic column was characterized by scanning electron microscopy (SEM). The mechanical strength and permeability have been studied in detail as well. The run-to-run and column-to-column reproducibility of the retention times were less than 0.9% and 3.0%, respectively. Furthermore, the influence of temperature and mobile phase composition on the separation of aromatic compounds was investigated. The results indicated that poly (trimethylol propane triacrylate-co-N-isopropylacrylamide-co-ethylenedimethacrylate) (TMPTA-co-NIPAAm-co-EDMA) monolithic column not only had high porosity and strong rigidity, but also was a promising tool for analyzing small molecule compounds with a short analysis time by controlling the column temperature.
采用原位自由基聚合，以 N-异丙基丙烯酰胺（NIPAAm）和三羟甲基丙烷三丙烯酸酯（TMPTA）为功能单体，以二甲基丙烯酸乙二醇酯（EDMA）为交联剂，制备了多孔整体柱。采用傅里叶变换红外光谱（FT-IR）法对整体柱的化学基团进行了测定，并用扫描电子显微镜（SEM）对优化后的整体柱的形态进行了表征。还详细研究了整体柱的机械强度和渗透性。保留时间的运行间和柱间重现性分别小于 0.9%和 3.0%。此外，还研究了温度和流动相组成对芳香族化合物分离的影响。结果表明，聚（三羟甲基丙烷三丙烯酸酯-co-N-异丙基丙烯酰胺-co-二甲基丙烯酸乙二醇酯）（TMPTA-co-NIPAAm-co-EDMA）整体柱不仅具有高孔隙率和强刚性，而且通过控制柱温，是一种分析小分子化合物的有前途的工具，分析时间短。
