Preparation of monolithic capillary columns based on poly(methyloctylsiloxane) thermally immobilized onto silica and mixed oxides for use in capillary liquid chromatography

• Grant number: 12/23518-2
• Support type: Scholarships in Brazil - Post-Doctorate
• Effective date (Start): March 01, 2013
• Effective date (End): February 29, 2016
• Field of knowledge: Physical Sciences and Mathematics - Chemistry - Analytical Chemistry
• Principal researcher: Carla Beatriz Grespan Bottoli
• Grantee: Carla Grazieli Azevedo da Silva
• Home Institution: Instituto de Química (IQ). Universidade Estadual de Campinas (UNICAMP). Campinas , SP, Brazil
• Associated research grant: 06/57897-9 - Preparation, characterization and application of new stationary phases for high-performance liquid chromatography and electrochromatography, AP.TEM

Abstract

The aim of this project is to synthesize and apply new monolithic silica-based stationary phases (SP) and silica modified with zirconium and titanium with poly(methyloctylsiloxane) SP to be used in capillary liquid chromatography in the HILIC (hydrophilic-interaction chromatography) and reversed-phase (RP) modes. The preparation of monoliths will use the process sol-gel (SGP), and the reaction parameters of the preparation of monolithic stationary phases, as well as the evaluation of polymer immobilization (for time and temperature) will be studied by the application of central composite designs and responses surface with 11 experiments. The best experimental conditions will be used in the synthesis of new stationary phases, which will be characterized by physical-chemical and chromatographic techniques. The physical-chemical characterizations will be performed by utilization of optic and electronic microscopies, thermogravimetric analysis, Fourier transform infrared (FTIR) spectroscopy, solid-state 29Si and 13C CP-MAS NMR spectroscopy, elemental analysis, and the chromatographic characterization will use test mixtures described by the literature for capillary monolithic columns for HILIC and reversed modes. The chemical stability of new stationary phases will be evaluated in the separation of solutes with different polarities in drastic conditions of pH, acidic and basic media (pH 1.7 e pH 10) and high temperatures.

Scientific publications

(References retrieved automatically from Web of Science and SciELO through information on FAPESP grants and their corresponding numbers as mentioned in the publications by the authors)

DA SILVA, CARLA G. A.; GRESPAN BOTTOLI, CARLA BEATRIZ; COLLINS, CAROL H.. 3-Dimensional X-ray microtomography methodology for characterization of monolithic stationary phases and columns for capillary liquid chromatography - A tutorial. Analytica Chimica Acta, v. 991, p. 30-45, OCT 23 2017. (12/23518-2, 13/25933-0, 08/57805-2)