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Author: Nilüfer Solak Publisher: ISBN: Category : Chemistry, Analytic Languages : en Pages : 221
Book Description
"This dissertation focuses on coupling liquid chromatography (LC) and/or ion mobility (IM) spectrometry to mass spectrometry (MS) and their application to characterization of complex mixtures. Fatty acid ethyl esters (FAEEs) in meconium, polyethylene oxide (PEO) copolymers, the nonionic surfactant Polysorbate 85, and poly(butylene adipate) were characterized by LC-MS[superscript n] and/or IMMS[superscript n]. Coupling of a separation technique to mass spectrometry improves the sensitivity of MS, thus permitting the detection of species present in low concentration. FAEEs are metabolites of ethanol. They are formed by nonoxidative metabolization of ethanol. FAEEs accumulate in various tissues. Ethanol can easily penetrate the placenta and results in the formation and deposition of FAEEs in fetal tissues including meconium. Therefore, FAEEs may be used as biomarkers for heavy alcohol consumption during pregnancy. In the first chapter of this dissertation (chapter 4), FAEEs were extracted from meconium and analyzed by LC-MS to determne the amount of ethyl linoleate, ethyl oleate, and ethyl palmitate. Among the fifty samples run, two were from mothers who had admitted alcohol consumption during pregnancy and those samples were found to contain high amounts of ethyl linoleate and ethyl palmitate. In the follow chapter of this dissertation (chapter 5), tandem mass spectrometry analyses were performed on PEO oligomers to elucidate their fragmentation pathways. These mechanisms derived the structural elucidation of the PEO copolymers analyzed by LC-MS[superscript n] in subsequent studies, as itemized below. In chapter 6, different chain lengths of a PEO-poly(propylene oxide) (PPO) triblock and a PEO-PPO random copolymer was separated and identified by LC-MS[superscript n]. Separation of the oligomers were based on their propylene oxide (PO) content. Oligomers with higher PO content had longer retention times. A putative PEO-poly(dimethylsiloxane) block copolymer was also investigated; in this case, unexpected minor byproducts/starting materials which could not be observed by MS were detected and identified using the LC-MS[superscript n] technique. Chapter 7 focuses on the LC-MS[superscript n] characterization of a commercial surfactant, Polysorbate 85. It is composed of many species with different degrees of esterification. Some of those species have identical nominal masses which complicates their characterization by MS. Therefore, a separation technique is needed prior to MS analysis. Reverse phase LC separated the oligomers based on their hydrophilicity/hydrophobicity. In addition, LC-MS2 experiments unveiled the esterification degree of the oligomers. A novel technique, IMMS, was also employed for characterization of the constituents of Polysorbate 85. IMMS disperses ions according to their collision cross sections and charge states. Oligomers with a different number of ester moieties could be separated and identified. Finally, Chapter 8 reports how IMMS was used to disperse and characterize linear and cyclic poly(butylene adipate) oligomers. The separation of the oligomers was based on their charge states. IMMS improved the sensitivity of MS and permitted the detection of +3 and +4 charged ions which were undetectable in the single-stage mass spectrum."--Abstract.
Author: Nilüfer Solak Publisher: ISBN: Category : Chemistry, Analytic Languages : en Pages : 221
Book Description
"This dissertation focuses on coupling liquid chromatography (LC) and/or ion mobility (IM) spectrometry to mass spectrometry (MS) and their application to characterization of complex mixtures. Fatty acid ethyl esters (FAEEs) in meconium, polyethylene oxide (PEO) copolymers, the nonionic surfactant Polysorbate 85, and poly(butylene adipate) were characterized by LC-MS[superscript n] and/or IMMS[superscript n]. Coupling of a separation technique to mass spectrometry improves the sensitivity of MS, thus permitting the detection of species present in low concentration. FAEEs are metabolites of ethanol. They are formed by nonoxidative metabolization of ethanol. FAEEs accumulate in various tissues. Ethanol can easily penetrate the placenta and results in the formation and deposition of FAEEs in fetal tissues including meconium. Therefore, FAEEs may be used as biomarkers for heavy alcohol consumption during pregnancy. In the first chapter of this dissertation (chapter 4), FAEEs were extracted from meconium and analyzed by LC-MS to determne the amount of ethyl linoleate, ethyl oleate, and ethyl palmitate. Among the fifty samples run, two were from mothers who had admitted alcohol consumption during pregnancy and those samples were found to contain high amounts of ethyl linoleate and ethyl palmitate. In the follow chapter of this dissertation (chapter 5), tandem mass spectrometry analyses were performed on PEO oligomers to elucidate their fragmentation pathways. These mechanisms derived the structural elucidation of the PEO copolymers analyzed by LC-MS[superscript n] in subsequent studies, as itemized below. In chapter 6, different chain lengths of a PEO-poly(propylene oxide) (PPO) triblock and a PEO-PPO random copolymer was separated and identified by LC-MS[superscript n]. Separation of the oligomers were based on their propylene oxide (PO) content. Oligomers with higher PO content had longer retention times. A putative PEO-poly(dimethylsiloxane) block copolymer was also investigated; in this case, unexpected minor byproducts/starting materials which could not be observed by MS were detected and identified using the LC-MS[superscript n] technique. Chapter 7 focuses on the LC-MS[superscript n] characterization of a commercial surfactant, Polysorbate 85. It is composed of many species with different degrees of esterification. Some of those species have identical nominal masses which complicates their characterization by MS. Therefore, a separation technique is needed prior to MS analysis. Reverse phase LC separated the oligomers based on their hydrophilicity/hydrophobicity. In addition, LC-MS2 experiments unveiled the esterification degree of the oligomers. A novel technique, IMMS, was also employed for characterization of the constituents of Polysorbate 85. IMMS disperses ions according to their collision cross sections and charge states. Oligomers with a different number of ester moieties could be separated and identified. Finally, Chapter 8 reports how IMMS was used to disperse and characterize linear and cyclic poly(butylene adipate) oligomers. The separation of the oligomers was based on their charge states. IMMS improved the sensitivity of MS and permitted the detection of +3 and +4 charged ions which were undetectable in the single-stage mass spectrum."--Abstract.
Author: Danijela Smiljanic Publisher: ISBN: Category : Chemistry Languages : en Pages : 154
Book Description
This dissertation focuses on coupling separation techniques such as ion mobility (IM) and liquid chromatography (LC) to mass spectrometry and their application to characterization of complex mixtures. Non-covalent complexes between poly(ethylene imine) (PEI) and single stranded oligodeoxynucleotides (ODNs), as well as components from black raspberries, were characterized utilizing ion mobility mass spectrometry (IM-MS) and liquid chromatography mass spectrometry (LC-MS), respectively. Interfacing these separation methods to mass spectrometry allows for detection and identification of isobaric species and species present in low concentration. Non-covalent complexes between low molecular weight poly(ethylene imine) (PEI 400 and 800) and single-stranded oligodeoxynucleotides (ODNs) were investigated for five ODNs, including d(TTTTT), d(CCCCC), d(AAAAA), d(GGGGG) and d(GCGAT). In chapter 4 the compositions, as well as solution and gas-phase stabilities of the complexes (termed polyplexes) were examined by electrospray ionization mass spectrometry (ESI-MS) and tandem mass spectrometry (MS2). Independent of the mixing ratio of the reactants, the polyplex with 1:1 polymer-to-nucleotide stoichiometry, PN, is the dominant product. The gas-phase stabilities, assessed by MS2 and collisionally activated dissociation, follow the same order, providing evidence that the polyplex structures in aqueous solution and the more hydrophobic environment of the gas phase are very similar. Non-covalent complexes with different composition but the same molecular mass were corroborated by ion mobility mass spectrometry (IM-MS). In chapter 5 of this dissertation an investigation of the expanded non-covalent system, ternary complexes, of poly(ethylene imine), single-stranded oligodeoxynucleotides and glutamic acid entities, is discussed. The solution stabilities and gas-phase stabilities of the ternary complexes (termed terplexes) were examined by electrospray ionization mass spectrometry (ESI-MS) and tandem mass spectrometry (MS2). In addition, higher order ternary structures with multiple units of polymer and/or nucleotide present within the terplex were identified utilizing IM-MS. Finally, chapter 6 provides information on characterization of non-anthocyanin components from black raspberry fractions by interfacing liquid chromatography (LC) to mass spectrometry. The black raspberry extracts were provided from the lab of Dr. Joseph C. Scheerens at Ohio Agricultural Research and Development Center, Wooster, Ohio. Combination of LC-MS, ESI-MS and MS2 provided structural information for the corresponding components.
Author: Christopher Barner-Kowollik Publisher: John Wiley & Sons ISBN: 3527329242 Category : Science Languages : en Pages : 501
Book Description
Combining an up-to-date insight into mass-spectrometric polymer analysis beyond MALDI with application details of the instrumentation, this is a balanced and thorough presentation of the most important and widely used mass-spectrometric methods. Written by the world's most proficient experts in the field, the book focuses on the latest developments, covering such technologies and applications as ionization protocols, tandem and liquid chromatography mass spectrometry, gas-phase ion-separation techniques and automated data processing. Chapters on sample preparation, polymer degradation and the usage of mass-spectrometric tools on an industrial scale round off the book. As a result, both entrants to the field and experienced researchers are able to choose the appropriate methods and instrumentations -- and to assess their respective strengths and limitations -- for the characterization of polymer compounds.
Author: Ana Varela Coelho Publisher: BoD – Books on Demand ISBN: 9535111361 Category : Medical Languages : en Pages : 208
Book Description
Tandem Mass Spectrometry - Molecular Characterization presents a comprehensive coverage of theory, instrumentation and description of experimental strategies and MS/MS data interpretation for the structural characterization of relevant molecular compounds. The areas covered include the analysis of drugs, metabolites, carbohydrates and protein post-translational modifications. The book series in Tandem Mass Spectrometry serves multiple groups of audiences; professional (academic and industry), graduate students and general readers interested in the use of modern mass spectrometry in solving critical questions of chemical and biological sciences.
Author: Alexandre A. Shvartsburg Publisher: CRC Press ISBN: 9781420051070 Category : Science Languages : en Pages : 322
Book Description
Over the last decade, scientific and engineering interests have been shifting from conventional ion mobility spectrometry (IMS) to field asymmetric waveform ion mobility spectrometry (FAIMS). Differential Ion Mobility Spectrometry: Nonlinear Ion Transport and Fundamentals of FAIMS explores this new analytical technology that separates and characterizes ions by the difference between their mobility in gases at high and low electric fields. It also covers the novel topics of higher-order differential IMS and IMS with alignment of dipole direction. The book relates the fundamentals of FAIMS and other nonlinear IMS methods to the physics of gas-phase ion transport. It begins with the basics of ion diffusion and mobility in gases, covering the main attributes of conventional IMS that are relevant to all IMS approaches. Building on this foundation, the author reviews diverse high-field transport phenomena that underlie differential IMS. He discusses the conceptual implementation and first-principles optimization of FAIMS as a filtering technique, emphasizing the dependence of FAIMS performance metrics on instrumental parameters and properties of ion species. He also explores ion reactions in FAIMS caused by field heating and the effects of inhomogeneous electric field in curved FAIMS gaps. Written by an accomplished scientist in the field, this state-of-the-art book supplies the foundation to understand the new technology of nonlinear IMS methods.
Author: Nathanael Frederick Zinnel Publisher: ISBN: Category : Languages : en Pages :
Book Description
Mass spectrometry (MS) has been established as important analytical tool in the characterization of an array of analyte classes, including biological samples. However, without hyphenation with other techniques, the approach has limitations to the information that can be elucidated and the samples that can be analyzed. In an attempt to overcome these limitations, separation is performed prior to MS analysis to aid in alleviating sample complexity while dissociation is incorporated to increase the information content. Here, we employ ion mobility (IM), a gas-phase separation technique, to disperse product ions resulting from collision-induced dissociation (CID), denoted as MS-CID-IM-MS, for top-down analysis for a variety of applications, specifically, primary structure elucidation, disulfide bond identification, secondary structure characterization, and polymer characterization. First, the fundamental attributes of this approach and the resulting information elucidated are investigated. Using this approach CID product ions are dispersed in two-dimensions, specifically size-to-charge (IM) and mass-to-charge (MS), and the resulting 2-D data display greatly facilitates the top-down information contents; (i) charge state specific trand lines, (ii) increased dynamic range, (iii) separation of overlapping ion signals. The increase in peak capacity allows for detection of low abundant fragment ions providing an increase in the primary sequence coverage and the confidence of ion assignments as demonstrated by melittin and ubiquitin. Second, this general approach is applied to the top-down analysis for a variety of applications. MS-CID-IM-MS is used for the structural characterization of disulfide linked protein ions by monitoring the ATD of the ion pre- and post-collisional activation. Similarly, this approach can also be used to distinguish product ion type as well as, in some cases, specific secondary structural elements, viz. extended coils or helices providing rapid identification of the onset and termination of extended coil structure in peptides as demonstrated by insulin B-chain. Detect of low abundant ion signals associated with cross-ring cleavages allows this approach to be extended to determine regiochemistry of glucose derived polymers. As demonstrated, the MS-CID-IM-MS approach is highly versatile owing to the information content gained upon dispersion of ions in two-dimensions, providing an effective increase in experimental dynamic range as well as providing conformational information. The electronic version of this dissertation is accessible from http://hdl.handle.net/1969.1/152846
Author: Stormy Lee Ann Koeniger Publisher: ISBN: Category : Languages : en Pages : 436
Book Description
For characterization of proteomic mixtures, high-quality primary sequence information is necessary to positively identify the components with database search algorithms. To improve parallel sequencing capabilities with this technology, a new drift tube design has been developed. This design provides high-efficiency fragmentation and improves the transmission efficiency of the fragments to the time-of-flight mass spectrometer. Additionally, the new method of collisional activation utilizes a system of potential at the exit of the drift tube, allowing rapid modulation of the potentials to provide precursor and fragment ion information during the course of a single LC separation.
Author: Johannes Karl Fink Publisher: John Wiley & Sons ISBN: 1119593131 Category : Science Languages : en Pages : 294
Book Description
The text focuses on the basic issues and also the literature of the past decade. The book provides a broad overview of functional synthetic polymers. Special issues in the text are: Surface functionalization supramolecular polymers, shape memory polymers, foldable polymers, functionalized biopolymers, supercapacitors, photovoltaic issues, lithography, cleaning methods, such as recovery of gold ions olefin/paraffin, separation by polymeric membranes, ultrafiltration membranes, and other related topics.
Author: Nilüfer Solak
Author: Nilüfer Solak
Author: Danijela Smiljanic
Author: Christopher Barner-Kowollik
Author: Ana Varela Coelho
Author: Alexandre A. Shvartsburg
Author: Nathanael Frederick Zinnel
Author: Stormy Lee Ann Koeniger
Author: Johannes Karl Fink
Author: T.W. Carr
Author: J. Rafael Montenegro Burke