Preparation, physical chemistry characterization and chromatographic of stationary phases Benzylamine

• Grant number: 16/07333-3
• Support Opportunities: Scholarships in Brazil - Scientific Initiation
• Start date: September 01, 2016
• End date: July 31, 2017
• Field of knowledge: Physical Sciences and Mathematics - Chemistry - Analytical Chemistry
• Principal Investigator: Márcia Cristina Breitkreitz
• Grantee: Ana Carolina Marcucci
• Host Institution: Instituto de Química (IQ). Universidade Estadual de Campinas (UNICAMP). Campinas , SP, Brazil

Abstract

The filling material of the chromatography column (called stationary phase, FE) is of paramount importance to the success of the separation of components of a mixture by liquid chromatography, since it provides physicochemical interactions with the analytes. Many materials have been developed for use as stationary phases in order to achieve proper selectivity for analytes with different physicochemical properties. The separation of polar and basic compounds using conventional FE is still problematic in liquid chromatography and for this reason, stationary phases based on the introduction of a phenyl group to the alkyl chain or polar groups embedded in the alkyl chain have arisen great interest. In this project, an innovative methodology will be developed for the preparation of a stationary phase phenyl type with embedded amide group, called FE benzylamide. This FE can be used both in the reverse phase mode or HILIC mode on the separation of polar and basic compounds. A new strategy for obtaining that FE will be proposed in order to acquire a homogeneous FE, because it has been described in the literature with heterogeneous character. This FE will be characterized physically and chemically by techniques such as infrared spectroscopy, nuclear magnetic resonance and elemental analysis to prove the presence of the benzylamide group. Test-mixtures established in the literature containing compounds of different polarities will be used to evaluate the chromatographic performance of the developed FE through the following parameters: number of plates (N), asymmetric peaks (As), retention of analytes and resolution between (Rs) pairs of solutes. The applicability of this FE will be evaluated using two mixtures of polar and basic drugs: one containing beta-blockers and other containing hydrophilic vitamins. (AU)