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MASS SPECTROMETRY METHODS FOR THE ANALYSIS OF POLYMERS AND BIOCONJUGATES

Sallam, Sahar
http://rave.ohiolink.edu/etdc/view?acc_num=akron1511882035662337

Abstract Details

2017, Doctor of Philosophy, University of Akron, Chemistry.
This dissertation focuses on the characterization of complex biomaterials by mass spectrometry (MS), tandem mass spectrometry (MS/MS) and ion mobility mass spectrometry (IM-MS). Chapter I provides a brief summary of the analytical problems addressed in this dissertation. Chapter II discusses the basic principles of mass spectrometry, including ionization techniques, mass analyzers, tandem mass spectrometry, and ion mobility. Chapter III describes the materials and instruments used to accomplish this work. Chapters IV, V, VI and VII are research project chapters, and each is briefly introduced below. Finally, Chapter VIII summarizes the conclusions drawn from this dissertation followed by an appendix and the copyright permissions obtained for this dissertation. The analysis of isomeric biodegradable polyesters is discussed in chapter IV. Matrix assisted laser desorption ionization (MALDI) and electrospray ionization (ESI) coupled with time-of-flight (ToF) mass analysis and tandem mass spectrometry (MS2) fragmentation were used to elucidate the composition, end groups, the chain sequence of poly(propylene maleate) (PPM) and poly(propylene fumarate) (PPF) copolymers. Additionally, ion mobility mass spectrometry (IM-MS) was used to differentiate the isomeric PPM and PPF copolyesters and to probe the extent and efficiency of PPM to PPF (i.e., all-cis to all-trans) isomerization. The analysis of the alanine-rich peptides AQK18 and GpAQK18 and their poly(ethylene glycol)-conjugated (PEGylated) forms AQK18-PEG and GpAQK18-PEG,is discussed in chapter V. In this work, ESI and MALDI interfaced with MS2 fragmentation and shape-sensitive separation via ion mobility mass spectrometry (IM-MS), were applied to elucidate the sequence and conformation of alanine-rich polypeptides and their conjugates. IM-MS data revealed the existence of two conformers for both the polypeptides and the conjugates. These were assigned to a fast-drifting random coil and a more slowly drifting helical structure. The collision cross-sections of the random coil and helical conformers of the polypeptides and their PEG conjugates were simulated for comparison with the experimental values to confirm the identity of the observed architectures and understand the stabilizing effects of the polymer chain. Chapter VI focuses on the structural characterization of a branched glycopolymer. Reversible addition-fragmentation chain transfer (RAFT) copolymerization of galactose acrylate and a polymerizable chain transfer agent branching unit was used to prepare this glycopolymer. Multistage mass spectrometry (MSn) and ion mobility were employed in this work to unveil useful information about the glycopolymer composition, possible end groups and architecture. Chapter VII discusses the analysis of a trehalose glycopolymer and its insulin conjugate. The goal of this study was to provide full characterization and detailed information about the chemical composition of the trehalose glycopolymer and its insulin conjugate and to determine the degree and the sites of conjugation by using multidimensional MS, including MALDI-MS, ESI-MS, and MS2.
Chrys Wesdemiotis, PhD (Advisor)
198 p.
Analytical Chemistry

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Citations

  • Sallam, S. (2017). MASS SPECTROMETRY METHODS FOR THE ANALYSIS OF POLYMERS AND BIOCONJUGATES [Doctoral dissertation, University of Akron]. OhioLINK Electronic Theses and Dissertations Center. http://rave.ohiolink.edu/etdc/view?acc_num=akron1511882035662337

    APA Style (7th edition)

  • Sallam, Sahar. MASS SPECTROMETRY METHODS FOR THE ANALYSIS OF POLYMERS AND BIOCONJUGATES. 2017. University of Akron, Doctoral dissertation. OhioLINK Electronic Theses and Dissertations Center, http://rave.ohiolink.edu/etdc/view?acc_num=akron1511882035662337.

    MLA Style (8th edition)

  • Sallam, Sahar. "MASS SPECTROMETRY METHODS FOR THE ANALYSIS OF POLYMERS AND BIOCONJUGATES." Doctoral dissertation, University of Akron, 2017. http://rave.ohiolink.edu/etdc/view?acc_num=akron1511882035662337

    Chicago Manual of Style (17th edition)

akron1511882035662337
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This open access ETD is published by University of Akron and OhioLINK.