Zhu Yang, Morisato Kei, Hasegawa George, Moitra Nirmalya, Kiyomura Tsutomu, Kurata Hiroki, Kanamori Kazuyoshi, Nakanishi Kazuki
Department of Chemistry, Graduate School of Science, Kyoto University, Kitashirakawa, Sakyo-ku, Kyoto, Japan.
GL Science, Iruma, Saitama, Japan.
J Sep Sci. 2015 Aug;38(16):2841-7. doi: 10.1002/jssc.201500444. Epub 2015 Jul 15.
The optimization of a porous structure to ensure good separation performances is always a significant issue in high-performance liquid chromatography column design. Recently we reported the homogeneous embedment of Ag nanoparticles in periodic mesoporous silica monolith and the application of such Ag nanoparticles embedded silica monolith for the high-performance liquid chromatography separation of polyaromatic hydrocarbons. However, the separation performance remains to be improved and the retention mechanism as compared with the Ag ion high-performance liquid chromatography technique still needs to be clarified. In this research, Ag nanoparticles were introduced into a macro/mesoporous silica monolith with optimized pore parameters for high-performance liquid chromatography separations. Baseline separation of benzene, naphthalene, anthracene, and pyrene was achieved with the theoretical plate number for analyte naphthalene as 36,000 m(-1). Its separation function was further extended to cis/trans isomers of aromatic compounds where cis/trans stilbenes were chosen as a benchmark. Good separation of cis/trans-stilbene with separation factor as 7 and theoretical plate number as 76,000 m(-1) for cis-stilbene was obtained. The trans isomer, however, is retained more strongly, which contradicts the long- established retention rule of Ag ion chromatography. Such behavior of Ag nanoparticles embedded in a silica column can be attributed to the differences in the molecular geometric configuration of cis/trans stilbenes.
在高效液相色谱柱设计中，优化多孔结构以确保良好的分离性能一直是一个重要问题。最近，我们报道了银纳米颗粒在周期性介孔二氧化硅整体柱中的均匀嵌入，以及这种嵌入银纳米颗粒的二氧化硅整体柱在多环芳烃高效液相色谱分离中的应用。然而，分离性能仍有待提高，与银离子高效液相色谱技术相比，其保留机制仍需阐明。在本研究中，将银纳米颗粒引入具有优化孔参数的大孔/介孔二氧化硅整体柱中，用于高效液相色谱分离。实现了苯、萘、蒽和芘的基线分离，分析物萘的理论塔板数为36,000 m⁻¹。其分离功能进一步扩展到芳香族化合物的顺/反异构体，其中选择顺/反式芪作为基准。获得了顺/反式芪的良好分离，分离因子为7，顺式芪的理论塔板数为76,000 m⁻¹。然而，反式异构体保留更强，这与银离子色谱长期确立的保留规则相矛盾。嵌入二氧化硅柱中的银纳米颗粒的这种行为可归因于顺/反式芪分子几何构型的差异。
