Preparation and characterization of mixed-mode monolithic silica column for capillary electrochromatography.
A silica-based monolithic stationary phase with mixed-mode of reversed phase (RP) and weak anion-exchange (WAX) for capillary electrochromatography (CEC) has been prepared. The mixed-mode monolithic silica column was prepared using the sol-gel technique and followed by a post-modification with hexadecyltrimethoxysilane (HDTMS) and aminopropyltrimethoxysilane (APTMS). The amino groups on the surface of the stationary phase were used to generate a substantial anodic EOF as well as to provide electrostatic interaction sites for charged compounds at low pH. A cathodic EOF was observed at pH above 7.3 due to the full ionization of residual silanol groups and the suppression in the ionization of amino groups. A variety of analytes were used to evaluate the electrochromatographic characterization and column performance. The monolithic stationary phase exhibited RP chromatographic behavior toward neutral solutes. The model anionic solutes were separated by the mixed-mode mechanism, which comprised RP interaction, WAX, and electrophoresis. Symmetrical peaks can be obtained for basic solutes because positively charged amino groups can effectively minimize the adsorption of positively charged analytes to the stationary phase.
Ye
Fanggui
F
Key Laboratory for the Chemistry and Molecular Engineering of Medicinal Resources (Ministry of Education of China), School of Chemistry & Chemical Engineering of Guangxi Normal University, Yucai Road 15, Guilin 541004, Guangxi, China. fangguiye@163.com
Wang
Shun
S
Zhao
Shulin
S
D002021:Buffers; D053801:Capillary Electrochromatography / Q000295:instrumentation*; D006863:Hydrogen-Ion Concentration; D009930:Organic Chemicals / Q000302:isolation & purification; D012822:Silicon Dioxide / Q000737:chemistry*
D002021:Buffers; D009930:Organic Chemicals; D012822:Silicon Dioxide