Institute of Pharmaceutical Sciences, Pharmaceutical (Bio-)Analysis, University of Tübingen, Tübingen, Germany.
Institute of Analytical Chemistry, University of Vienna, Vienna, Austria.
J Sep Sci. 2022 Sep;45(17):3286-3300. doi: 10.1002/jssc.202200268. Epub 2022 Jun 17.
The present work reports on a novel stable-bonded amino silica stationary phase obtained by crosslinking of surface aminopropyl moieties using triglycidyl isocyanurate. The obtained cross-linked amido-amino network silica material exhibited superior hydrolytic stability compared to classical 3-aminopropyl phases and showed, inter alia, excellent separation of nine therapeutically effective sulfonamides in hydrophilic interaction/weak anion exchange chromatography elution mode. Additionally, the separation of carbohydrates was investigated under classical hydrophilic interaction chromatography conditions as well proving the suitability of the novel phase for such applications. For the evaluation of the hydrolytic stability the prepared material, as well as two commercially available benchmark columns and a set of in-house synthesized amino-modified materials, were exposed to harsh aqueous mobile phase conditions for in total of 50 h at elevated temperature. In this context, the materials were examined by elemental analysis, ( C and Si cross-polarization/magic angle spinning) solid-state nuclear magnetic resonance, and a chromatographic test before and subsequent to the exposure to these stress conditions. Lastly, the new stationary phase was classified in comparison to a set of commercially available stationary phases by principal component analysis of resultant retention factors gained from chromatographic standard tests.
本工作报道了一种新型的稳定键合氨基硅胶固定相,它是通过使用三缩水甘油异氰尿酸酯交联表面氨丙基官能团得到的。所得到的交联酰胺-氨基网络硅胶材料与经典的 3-氨丙基相相比具有更高的水解稳定性,并且表现出,除其他外,在亲水相互作用/弱阴离子交换色谱洗脱模式下对九种治疗有效的磺胺类药物具有优异的分离性能。此外,还在经典的亲水相互作用色谱条件下研究了碳水化合物的分离,证明了该新型固定相适用于此类应用。为了评估水解稳定性,将制备的材料以及两种市售的基准柱和一组内部合成的氨基改性材料在高温下总共在苛刻的水性流动相条件下暴露 50 小时。在这种情况下,通过元素分析、(C 和 Si 交叉极化/魔角旋转)固态核磁共振和暴露于这些应力条件前后的色谱测试来检查材料。最后,通过对色谱标准测试获得的保留因子的主成分分析,将新型固定相与一组市售固定相进行了分类比较。