Improving the Understanding of the Properties and Retention Behavior of Chemically Bonded Stationary Phases Employing Spectroscopic and Chromatographic Characterization Techniques

• Applicant: Professor Dr. Klaus Albert (†)
• Subject Area: Analytical Chemistry
• Term: from 2007 to 2012
• Project identifier: Deutsche Forschungsgemeinschaft (DFG) - Project number 50049040

This project intends to capitalize on the mutually complementary expertise [synthesis of novel HPLC stationary phases (JP) and NMR characterization and development of HPLC/NMR coupling (KA)] of the principal investigators to provide new insights into chromatographic retention in order to better design new separation protocols as well as new stationary phases. Intellectual Merit: A variety of stationary phases will be characterized using solid-state NMR and suspended-state NMR techniques. The latter is a valuable tool for understanding chromatographic behavior because it can detect interactions between solutes and the stationary phase as well as the chromatographic support material. These capabilities will provide answers to how various types of molecules are retained in the separation process. Conventional stationary phases (those produced by organosilanization) and new hydride based stationary phases (fabricated by silanization/hydrosilation creating a new surface where hydrides replace silanol groups) will be studied. The hydride-based phases can retain both polar and nonpolar compounds and operate in mobile phases from 100% aqueous to completely organic. Understanding retention on these materials will be particularly valuable for solving challenging separation problems in proteomics, metabolomics, clinical analysis and environmental monitoring. The NMR characterizations will be supported by chromatographic evaluations using conventional LC, capillary LC, LC-MS and LC-NMR. The synthesis of the various hydride stationary phases will be done at San Jose State University where these materials were developed and the NMR investigations will take place at the University of Tubingen where the suspended state NMR method was first used. Each lab will conduct various HPLC evaluations with those studies utilizing NMR for detection taking place in Tubingen where considerable effort is ongoing in the further development of this method. This project will address questions about solute retention on stationary phases that have existed for many years and also investigate the most recently developed separation materials. Broader Impacts: The project is a collaborative effort that encompasses synthetic chemistry as well as development of analytical methodology. The background and expertise of the PIs encompass all of the major directions outlined in this proposal. The project will involve the training of undergraduate and graduate students in an international team oriented format. Interactions between the two groups will involve exchange of ideas as well as personnel as appropriate to fulfilling the goals of the project. The SJSU student body is a diverse group where there is no ethnic majority so that the manpower development aspects of the project will have a significant impact on underrepresented groups in science. A teaching postdoctoral position is included in the project personnel that involves 50% of the time being devoted to research and a 50% commitment to participation in instructional activities. The results of these investigations will also be submitted to peer reviewed journals in analytical chemistry and materials science and will be described in presentations at significant national and international professional meetings in these disciplines.

• DFG Programme: Research Grants
• International Connection: USA
• Participating Person: Professor Dr. Joseph Pesek