Probing Base Metal Coordination Complexes Using Electrospray Ionization Quadrupole Time-of-Flight Mass Spectrometry

Probing Base Metal Coordination Complexes Using Electrospray Ionization Quadrupole Time-of-Flight Mass Spectrometry
Author: Jessica J. Martin
Publisher:
Total Pages:
Release: 2022
Genre:
ISBN:
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Presently, much research has been completed focusing on metal coordination complexes in the liquid phase but very little in terms of the gas phase. The purpose of this research is to further investigate these conditions and learn more about the reactions that can occur using Electrospray Ionization Quadrupole Time-of-Flight Mass Spectrometry (ESI QToF MS). This research focuses on Nickel (II) and Iron (III) Nitrate solutions in combination with five ligands: 2,2'-Bipyridine, 4,4'-Bipyridine, 2,2'-Bipyridine-4,4'-Dicarboxylic Acid, 1,10-Phenanthroline and the Baker Group's SNS Ligand. Observations of these complexes were restricted to the monocations. Those combinations that successfully coordinated in the gas phase were subjected to further analysis to determine their fragmentation pathways under specific conditions. To investigate their interactions, studies were conducted using three different mixing techniques. These techniques included a pre-mixed single-spray solution, a dual-spray injection method, and the TRESI (time-resolved electrospray ionization) method. By using all three methods, the compounds' ability to react in solution over time can be compared to real-time mixing in both the gas and liquid phases, via dual-spray and TRESI techniques respectively. Further experimentation took place on target complexes, created by each of the ten combinations of starting compounds, to further investigate the gas phase properties and fragmentation patterns that exist. It was observed that most experiments with the Nickel (II) Nitrate solution were successful with all three methods, while the Iron (III) Nitrate however created some problems. In general, single-spray analysis gave the best results compared to dual-spray, which was ineffective for some combinations, particularly the 2,2'-Bipyridine-4,4'-Dicarboxylic Acid and SNS ligands. It was found that both the 2,2'-Bipyridine and 4,4'-Bipyrdine combinations produced very similar results despite their respective bidentate and bridging coordination tendencies. The TRESI method provided limited information due to the delayed reaction times with some combinations. Overall, this work proved useful in its ability to compare metal coordination complex formation in solution and gas phases.

Using Electrospray Ionization Mass Spectrometry for Understanding Metal-ligand Interactions

Using Electrospray Ionization Mass Spectrometry for Understanding Metal-ligand Interactions
Author: Adetayo Musbau Mustapha
Publisher:
Total Pages: 0
Release: 2015
Genre: Electrospray ionization mass spectrometry
ISBN:
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Metal-ligand interactions are important in such diverse areas as environmental remediation, drug development, and biochemistry. Potentiometric and spectroscopic techniques, including UV-Visible, infrared, Raman, and NMR spectroscopies, are commonly used to investigate metal-ligand interactions. However, ESI-MS is a valuable technique for accurate determination of complex stoichiometric ratios, and for the study of the gas-phase chemistry of metal complexes with organic ligands. This dissertation presents two broad areas where ESI-MS has been used to study such complexes. In the first area, I investigated the analytical importance of transition metal interactions with phosphorothioate and phosphorodithioate pesticides. These pesticides are important subclasses of organophosphorus pesticides commonly used in agriculture to control pests in fruits and vegetables. Using ESI-MS, I examined how the interactions of three phosphorothioate pesticides (fenitrothion, parathion, and diazinon) and one phosphorodithioate pesticide (malathion) with silver and copper ions affects the mass spectral detection of the resulting complexes. My results show that each pesticide forms silver and copper complexes that significantly improve their detection using ESI-MS. I also found that these metal-pesticide complexes do not undergo the thiono-thiolo rearrangement reaction during collision-induced dissociation, unlike protonated phosphorothioate ions. In the second part of the dissertation I explore the use of ESI-MS for characterization of gas-phase complexes that arise from uranyl(VI), vanadium(V) and iron(III) interactions with 2,6-dihydroxyiminopiperidine (DHIP) and N1, N5-dihydroxypentanediimidamide (DHPD) in aqueous solutions. I also investigated uranyl(VI) interactions with N1, N5-dihydroxyethanediimidamide (DHED). Uranium is an important fuel for nuclear power generation, and there is much interest in the possibility of its extraction from seawater using amidoxime-functionalized sorbents. Vanadium and iron can compete with uranium for binding sites on these sorbents. My results show that DHIP binds uranyl(VI) more effectively that DHPD or DHED, forming ions having uranyl(VI):DHIP stoichiometric ratios of 1:1, 1:2, and 2:3. Vanadium(V) forms 1:1 and 1:2 vanadium(V):DHIP complexes, while iron(III) forms only a 1:2 iron(III):DHIP complex. With DHPD, vanadium(V) forms only a 1:2 vanadium(V):DHPD complex, while iron(III) forms both 1:2 and 1:3 complexes with DHPD. I also observed that gas-phase uranyl(VI)-DHIP complexes are less likely to form in the presence of either vanadium(V) or iron(III).

Index Medicus

Index Medicus
Author:
Publisher:
Total Pages: 1812
Release: 2004
Genre: Medicine
ISBN:
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Mass Spectrometry of Inorganic and Organometallic Compounds

Mass Spectrometry of Inorganic and Organometallic Compounds
Author: William Henderson
Publisher: John Wiley & Sons
Total Pages: 272
Release: 2005-07-15
Genre: Science
ISBN: 047001430X
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This is the first modern book to treat inorganic and organometallic mass spectrometry simultaneously. It is textbook and handbook in one; as a textbook it introduces the techniques and gives hints on how to apply the various techniques, as a handbook it lists all available ionization techniques for just about any given compound. The book also includes non-mathematical explanations of how modern MS instruments work Mass Spectrometry of Inorganic and Organometallic Compounds will inspire the synthetic inorganic and organometallic chemist with the confidence to apply some of the new techniques to their characterization problems.

Ambient Ionization Mass Spectrometry

Ambient Ionization Mass Spectrometry
Author: Marek Domin
Publisher: Royal Society of Chemistry
Total Pages: 528
Release: 2014-11-25
Genre: Science
ISBN: 1849739269
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Ambient ionization has emerged as one of the hottest and fastest growing topics in mass spectrometry enabling sample analysis with minimal sample preparation. Introducing the subject and explaining the basic concepts and terminology, this book will provide a comprehensive, unique treatise devoted to the subject. Written by acknowledged experts, there are full descriptions on how new ionization techniques work, with an overview of their strengths, weaknesses and applications. This title will bring the reader right up to date, with both applications and theory, and will be suitable as a tutorial text for those starting in the field from a variety of disciplines.

Cumulated Index Medicus

Cumulated Index Medicus
Author:
Publisher:
Total Pages: 1844
Release: 2000
Genre: Medicine
ISBN:
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Metallointercalators

Metallointercalators
Author: Janice Aldrich-Wright
Publisher: Springer
Total Pages: 449
Release: 2011-04-06
Genre: Science
ISBN: 3211990798
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A comprehensive treatment of the characterisation techniques used in investigating inorganic and organic molecules that interact with biomolecules is presented to the reader in a clear fashion. The work consists of two parts: (i) synthetic aspects of metallointercalators along with targeting and improving transport and (ii) the various techniques that are used for probing their interactions, such as; DNA-NMR, PGSE-NMR, DNA ESI-MS, Linear and Circular Dichroism, Fluorescence Spectroscopy, Confocal Microscopy, Viscosity, TGA and dialysis, Microarrays, biological analysis. Chapters are devoted to the synthesis and the techniques used to study the interactions of inorganic complexes with biomolecules. Considerably detailed examples are used to help illustrate the application of these techniques. This book is a useful resource for an array of inorganic and organic advanced undergraduate and graduate courses and for researchers in drug discovery.

Electrospray and MALDI Mass Spectrometry

Electrospray and MALDI Mass Spectrometry
Author: Richard B. Cole
Publisher: John Wiley & Sons
Total Pages: 900
Release: 2011-09-26
Genre: Science
ISBN: 1118211553
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Discover how advances in mass spectrometry are fueling new discoveries across a broad range of research areas Electrospray and MALDI Mass Spectrometry brings both veteran practitioners and beginning scientists up to date with the most recent trends and findings in electrospray ionization and matrix-assisted laser desorption/ionization (MALDI) mass spectrometry. In particular, this Second Edition highlights how advances in electrospray and MALDI mass spectrometry are supporting important discoveries in new and emerging fields such as proteomics and metabolomics as well as in traditional areas of chemistry and physics research. Electrospray AND MALDI Mass Spectrometry, SECOND EDITION is divided into five parts: Part A, Fundamentals of ES, explains the fundamental phenomena underlying the electrospray process, including selectivity in ionization and inherent electrochemistry, and concludes with a chapter offering a comparative inventory of source hardware Part B, Fundamentals of MALDI, confronts ionization mechanisms, instrument development, and matrix selection, and includes a final chapter that explores the special application of MALDI to obtain two-dimensional images of spatial distributions of compounds on surfaces Part C, ES and MALDI Coupling to Mass Spectrometry Instrumentation, examines the coupling of these ionization techniques to various mass analyzers, including quadrupole ion trap, time-of-flight, Fourier transform ion cyclotron resonance, and ion mobility mass spectrometers Part D, Practical Aspects of ES and MALDI, investigates analytical issues including quantification, charge-state distributions, noncovalent interactions in solution that are preserved as gas-phase ions, and various means of ion excitation in preparation for tandem mass spectrometry, and offers a guide to the interpretation of even-electron mass spectra Part E, Biological Applications of ES and MALDI, examines the role of mass spectrometry in such areas as peptide and protein characterization, carbohydrate analysis, lipid analysis, and drug discovery Written by a team of leading experts, the book not only provides a critical review of the literature, but also presents key concepts in tutorial fashion to help readers take full advantage of the latest technological breakthroughs and applications. As a result, Electrospray and MALDI Mass Spectrometry will help researchers fully leverage the power of electrospray and MALDI mass spectrometry. The judicious compartmentalization of chapters, and the pedagogic presentation style throughout, render the book highly suitable for use as a text for graduate-level courses in advanced mass spectrometry.