Synthesis and characterization of new hybrid monolithic stationary phases for use in capillary liquid chromatography

• Grant number: 19/04567-1
• Support Opportunities: Regular Research Grants
• Start date: July 01, 2020
• End date: September 30, 2022
• Field of knowledge: Physical Sciences and Mathematics - Chemistry - Analytical Chemistry
• Principal Investigator: Carla Beatriz Grespan Bottoli
• Grantee: Carla Beatriz Grespan Bottoli
• Host Institution: Instituto de Química (IQ). Universidade Estadual de Campinas (UNICAMP). Campinas , SP, Brazil

Abstract

The use of hybrid monolithic stationary phases has been gaining ground in capillary separation techniques, since they combine the advantages of both organic and silica- based monoliths, such as a wide pH range, less shrinkage, greater mechanical stability and surface area. Currently, for the production of this type of column several strategies of synthesis have been developed suchas sol-gel, one-pot, click chemistry, among others.Among the various reagents that can be used in the synthesis of the hybrid monoliths, the oligomeric polyhedral silsesquioxanes (POSS) have been shown to have good mechanical and pH stability, as well as high thermal stability. In addition, ionic liquids appearhave been incorporated in the monolithic structure or used as a modifier on their surface, because they confer to the stationary phase a mixed mode of separation with hydrophobic interactions, À-À, ion exchange, electrostatics, dipole-dipole and hydrogen bonding.In this work, hybrid monolithic capillary columns have been/will be synthesized using POSS-MA (substituted methacrylate) and monomeric ionic liquids as precursors. Hybrid monolithic capillary columns using one-pot synthesis and thiol-ene and thiol-methacrylate reactions of the click chemistry type will also be synthesized for the separation of molecules with polarities and different chemical characteristics like drugs and proteins using Capillary Liquid Chromatography (CLC) in the reversed phase mode and hydrophilic interaction liquid chromatography (HILIC).The columns will be characterized by physical-chemical analysis (infrared, surface area and pore volume, elemental analysis, thermogravimetry and NMR), morphological analysis, via scanning electron microscopy and chromatographic analyses, via liquid chromatography and will subsequently be applied for protein analysis using CLC with mass spectrometric detection (CLC-MS). (AU)