Patel Darshan C, Breitbach Zachary S, Yu JeongJae, Nguyen Kate A, Armstrong Daniel W
Department of Chemistry and Biochemistry, University of Texas at Arlington, 700 Planetarium Place, Arlington, TX 76019, United States.
Department of Chemistry and Biochemistry, University of Texas at Arlington, 700 Planetarium Place, Arlington, TX 76019, United States; Department of Chemistry, Kyungpook National University, Daegu, 702-701, Republic of Korea.
Anal Chim Acta. 2017 Apr 22;963:164-174. doi: 10.1016/j.aca.2017.02.005. Epub 2017 Feb 20.
Two new anion-exchange columns were prepared by bonding tert-butyl carbamoylated quinine to 2.7 μm superficially porous particle (SPP) silica to create chiral stationary phases for high-efficiency and ultrafast chromatography. Performance and retention parameters of these new columns are compared with an analogous 5 μm fully porous particle (FPP) based Chiralpak QNAX column and a 3-4 fold increase in efficiency was observed. Ultrafast separations ranging from 12 s down to sub-second are shown using 2.7 μm SPPs bonded via hydrosilation to the selector. Potential benefits of 2.7 μm SPP based columns for increased LC-MS compatibility were investigated. A van Deemter plot comparison showed 2.7 μm SPP based columns provided a lower reduced plate height and a higher optimal linear velocity compared to the 5 μm FPP based column. With geometry-independent kinetic plots, 2.7 μm SPP and 5 μm FPP based columns were assessed for their kinetic performance and the maximal number of plates each column can generate in a given analysis time. The 2.7 μm SPP based column showed remarkable performance improvements in speed and efficiency as indicated by the kinetic plots.
通过将叔丁基氨基甲酰化奎宁键合到2.7μm表面多孔颗粒(SPP)硅胶上,制备了两种新型阴离子交换柱,以创建用于高效和超快速色谱的手性固定相。将这些新柱的性能和保留参数与类似的基于5μm全多孔颗粒(FPP)的Chiralpak QNAX柱进行了比较,观察到效率提高了3至4倍。使用通过硅氢化键合到选择剂上的2.7μm SPP展示了从12秒到亚秒级的超快速分离。研究了基于2.7μm SPP的柱在提高LC-MS兼容性方面的潜在优势。范德姆特曲线比较表明,与基于5μm FPP的柱相比,基于2.7μm SPP的柱提供了更低的折合板高和更高的最佳线性速度。通过与几何形状无关的动力学曲线,评估了基于2.7μm SPP和5μm FPP的柱的动力学性能以及每根柱在给定分析时间内可产生的最大塔板数。动力学曲线表明,基于2.7μm SPP的柱在速度和效率方面表现出显著的性能提升。