Author ORCID Identifier

0000-0002-8315-6929

Date of Award

Fall 12-12-2022

Degree Type

Dissertation

Degree Name

Doctor of Philosophy (PhD)

Department

Chemistry

First Advisor

Dr. W. David Wilson

Abstract

The hyphenation of micellar electrokinetic chromatography and mass spectrometry (MEKC-MS) serves as a valuable tool for the enantioseparations of charged and neutral chiral analytes using polymeric micelles as pseudo-stationary phases. However, the technique still requires significant improvements. Two major challenges in MEKC-MS are: (i) lack of ruggedness and robustness of bare fused silica column and (ii) low-throughput enantioseparations using one single chiral selector. This work demonstrates the utilization of 2-acrylamido-2-methyl-1-propane-sulfonic acid (AMPS) based covalently bonded column in MEKC-MS for the simultaneous enantioseparations of three β-blockers (atenolol, metoprolol, and pindolol). Excellent reproducibility is achieved, and the method validation is performed by analyzing two commercial tablets of atenolol and metoprolol using pindolol as an internal standard. The developed AMPS bonded rugged column is further utilized for the enantioseparations of small chiral molecules using newly designed glycopeptide-based MoMs as chiral selectors. A library of glycopeptide MoMs was prepared by co-polymerizing sugar and dipeptide-based surfactants in 50/50 ratios. The syntheses of sugar and dipeptide-based surfactants are reported in the literature; however, their combination to prepare a glycopeptide micelle is the first to be reported here. Different separation parameters such as pH, BGE, and micelle concentrations were optimized and using optimum conditions (buffer1: 20 mM NH4OAC and 15 mM TEA, buffer 2: 20 mM NH4OAC), 16 chiral analytes achieved Rs≥0.5. The %success rate for baseline resolved compounds is also evaluated.

DOI

https://doi.org/10.57709/32726648

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