Synthesis and Chromatographic Evaluation of Superficially Porous Particles for Ultrahigh Pressure Liquid Chromatography Public Deposited

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  • March 19, 2019
  • Treadway, James
    • Affiliation: College of Arts and Sciences, Department of Chemistry
  • Chromatographic separations play a vital role in the separation and analysis of biological samples. Superficially porous particle have emerged as a useful particle architecture for liquid chromatography. These particles have received significant attention recently for the chromatographic efficiency gains that they display. Ultrahigh pressure liquid chromatography employs small particles and high pressures to also yield highly efficient separations. Increasingly, the field of chromatography had employed a combination of these two methods for creating highly efficient columns. One portion of this work details the work with micron-sized superficially porous particles for the separation of intact proteins and other large molecules. Superficially porous particles specifically tailored for the separation of large molecules are not currently commercially available in the single micron size range. One aspect of this work describes the synthetic route that was utilized to create these particles in such a small overall particle size. Another aspect of this work details an evaluation of the separation capabilities of these particles when packed into capillary columns. These columns were utilized for the separation of small molecules, peptides and proteins. Another portion of this work concerns the utilization of commercially manufactured superficially porous particles. One chapter focuses on the creation of highly efficient capillary columns packed with commercial prototype superficially porous particles. The capillary columns created in that chapter exhibit isocratic efficiencies for the separation of small molecules rivaling those seen for capillary columns packed with fully porous particles. This is the first time that such efficient separations have been demonstrated using superficially porous particles packed into capillary columns. A final section of the dissertation focuses on the comparison between commercially available fully and superficially porous particles packed into capillary columns. These particles were bonded with either conventional or charged-surface reversed-phase bondings. The separation characteristics for these columns were evaluated in terms of separating small molecules, peptides, and proteins. It was seen that both the bonded phase and the particle morphology contributed to separation differences between the columns. This work provides insight into which particle and bonding type should be pursued for future investigations.
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Rights statement
  • In Copyright
  • Pielak, Gary J.
  • Erie, Dorothy
  • Ramsey, J. Michael
  • Jorgenson, James
  • Schoenfisch, Mark H.
  • Doctor of Philosophy
Degree granting institution
  • University of North Carolina at Chapel Hill Graduate School
Graduation year
  • 2015
Place of publication
  • Chapel Hill, NC
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