Bai Xiaomei, Liu Haiyan, Wei Dan, Yang Gengliang
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.
Talanta. 2014 Feb;119:479-84. doi: 10.1016/j.talanta.2013.11.050. Epub 2013 Nov 25.
A novel poly (trimethylol propane triacrylate-co-ethylene dimethacrylate) [poly (TMPTA-co-EDMA)] monolith was prepared by in situ free-radical polymerization in a 50 mm × 4.6mm i.d. stainless steel column and was investigated for high performance liquid chromatography (HPLC). The porous structure of monolith was optimized by changing the conditions of polymerization. The chemical group of the monolithic column was confirmed by a Fourier transform infrared spectroscopy (FT-IR) method and the morphology of column structure was characterized by scanning electron microscopy (SEM). The mechanical strength and permeability were also studied. Finally, a series of low-molecular-weight organic compounds were utilized to evaluate the retention behaviors of the monolithic column. The result demonstrated that the prepared column exhibited an RP-chromatographic behavior and good separation performance. The method reproducibility was obtained by evaluating the run-to-run and column-to-column with relative standard deviations (RSDs) less than 0.7% (n=6) and 2.9% (n=6), respectively, which indicated that prepared monolithic columns had good reproducibility and stability.
通过在50 mm×4.6mm内径的不锈钢柱中原位自由基聚合制备了一种新型聚（三羟甲基丙烷三丙烯酸酯 - 二甲基丙烯酸乙烯酯）[聚（TMPTA - co - EDMA）]整体柱，并对其进行了高效液相色谱（HPLC）研究。通过改变聚合条件优化了整体柱的多孔结构。采用傅里叶变换红外光谱（FT - IR）法确认了整体柱的化学基团，并用扫描电子显微镜（SEM）对柱结构的形态进行了表征。还研究了其机械强度和渗透率。最后，利用一系列低分子量有机化合物评估了整体柱的保留行为。结果表明，所制备的柱表现出反相色谱行为和良好的分离性能。通过评估批间和柱间重复性获得了方法重现性，相对标准偏差（RSD）分别小于0.7%（n = 6）和2.9%（n = 6），这表明所制备的整体柱具有良好的重现性和稳定性。
