Issues and opportunities in accelerator mass spectrometry for stable isotopes.

Science.gov (United States)

Matteson, Sam

2008-01-01

Accelerator mass spectrometry (AMS) has developed in the last 30 years many notable applications to the spectrometry of radioisotopes, particularly in radiocarbon dating. The instrumentation science of trace element AMS (TEAMS) that analyzes stable isotopes, also called Accelerator SIMS or MegaSIMS, while unique in many features, has also shared in many of these significant advances and has pushed TEAMS sensitivity to concentration levels surpassing many competing mass spectroscopic technologies. This review examines recent instrumentation developments, the capabilities of the new instrumentation and discernable trends for future development. Copyright 2008 Wiley Periodicals, Inc.

Boundaries of mass resolution in native mass spectrometry.

Science.gov (United States)

Lössl, Philip; Snijder, Joost; Heck, Albert J R

2014-06-01

Over the last two decades, native mass spectrometry (MS) has emerged as a valuable tool to study intact proteins and noncovalent protein complexes. Studied experimental systems range from small-molecule (drug)-protein interactions, to nanomachineries such as the proteasome and ribosome, to even virus assembly. In native MS, ions attain high m/z values, requiring special mass analyzers for their detection. Depending on the particular mass analyzer used, instrumental mass resolution does often decrease at higher m/z but can still be above a couple of thousand at m/z 5000. However, the mass resolving power obtained on charge states of protein complexes in this m/z region is experimentally found to remain well below the inherent instrument resolution of the mass analyzers employed. Here, we inquire into reasons for this discrepancy and ask how native MS would benefit from higher instrumental mass resolution. To answer this question, we discuss advantages and shortcomings of mass analyzers used to study intact biomolecules and biomolecular complexes in their native state, and we review which other factors determine mass resolving power in native MS analyses. Recent examples from the literature are given to illustrate the current status and limitations.

Tandem mass spectrometry at low kinetic energy

International Nuclear Information System (INIS)

Cooks, R.G.; Hand, O.W.

1987-01-01

Recent progress in mass spectrometry, as applied to molecular analysis, is reviewed with emphasis on tandem mass spectrometry. Tandem instruments use multiple analyzers (sector magnets, quadrupole mass filters and time-of-flight devices) to select particular molecules in ionic form, react them in the gas-phase and then record the mass, momenta or kinetic energies of their products. The capabilities of tandem mass spectrometry for identification of individual molecules or particular classes of compounds in complex mixtures are illustrated. Several different types of experiments can be run using a tandem mass spectrometer; all share the feature of sifting the molecular mixture being analyzed on the basis of chemical properties expressed in terms of ionic mass, kinetic energy or charge state. Applications of mass spectrometry to biological problems often depend upon desorption methods of ionization in which samples are bombarded with particle beams. Evaporation of preformed charged species from the condensed phase into the vacuum is a particularly effective method of ionization. It is suggested that the use of accelerator mass spectrometers be extended to include problems of molecular analysis. In such experiments, low energy tandem mass spectrometry conducted in the eV or keV range of energies, would be followed by further characterization of the production ion beam using high selective MeV collision processes

A new instrument of VUV laser desorption/ionization mass spectrometry imaging with micrometer spatial resolution and low level of molecular fragmentation.

Science.gov (United States)

Wang, Jia; Liu, Feng; Mo, Yuxiang; Wang, Zhaoying; Zhang, Sichun; Zhang, Xinrong

2017-11-01

Mass spectrometry imaging (MSI) has important applications in material research, biology, and medicine. The MSI method based on UV laser desorption/ionization (UVLDI) can obtain images of intact samples, but has a high level of molecular fragmentation. In this work, we report a new MSI instrument that uses a VUV laser (125.3 nm) as a desorption/ionization source to exploit its advantages of high single photon energy and small focus size. The new instrument was tested by the mass spectra of Nile red and FGB (Fibrinogen beta chain) samples and mass spectrometric images of a fly brain section. For the tested samples, the VUVDI method offers lower levels of molecular fragmentations and higher sensitivities than those of the UVLDI method and second ion mass spectrometry imaging method using a Bi 3 + beam. The ablation crater produced by the focused VUV laser on a quartz plate has an area of 10 μm 2 . The VUV laser is prepared based on the four-wave mixing method using three collimated laser beams and a heated Hg cell.

A new instrument of VUV laser desorption/ionization mass spectrometry imaging with micrometer spatial resolution and low level of molecular fragmentation

Science.gov (United States)

Wang, Jia; Liu, Feng; Mo, Yuxiang; Wang, Zhaoying; Zhang, Sichun; Zhang, Xinrong

2017-11-01

Mass spectrometry imaging (MSI) has important applications in material research, biology, and medicine. The MSI method based on UV laser desorption/ionization (UVLDI) can obtain images of intact samples, but has a high level of molecular fragmentation. In this work, we report a new MSI instrument that uses a VUV laser (125.3 nm) as a desorption/ionization source to exploit its advantages of high single photon energy and small focus size. The new instrument was tested by the mass spectra of Nile red and FGB (Fibrinogen beta chain) samples and mass spectrometric images of a fly brain section. For the tested samples, the VUVDI method offers lower levels of molecular fragmentations and higher sensitivities than those of the UVLDI method and second ion mass spectrometry imaging method using a Bi3+ beam. The ablation crater produced by the focused VUV laser on a quartz plate has an area of 10 μm2. The VUV laser is prepared based on the four-wave mixing method using three collimated laser beams and a heated Hg cell.

Steroid Profiling by Gas Chromatography–Mass Spectrometry and High Performance Liquid Chromatography–Mass Spectrometry for Adrenal Diseases

Science.gov (United States)

McDonald, Jeffrey G.; Matthew, Susan

2012-01-01

The ability to measure steroid hormone concentrations in blood and urine specimens is central to the diagnosis and proper treatment of adrenal diseases. The traditional approach has been to assay each steroid hormone, precursor, or metabolite using individual aliquots of serum, each with a separate immunoassay. For complex diseases, such as congenital adrenal hyperplasia and adrenocortical cancer, in which the assay of several steroids is essential for management, this approach is time consuming and costly, in addition to using large amounts of serum. Gas chromatography/mass spectrometry profiling of steroid metabolites in urine has been employed for many years but only in a small number of specialized laboratories and suffers from slow throughput. The advent of commercial high-performance liquid chromatography instruments coupled to tandem mass spectrometers offers the potential for medium- to high-throughput profiling of serum steroids using small quantities of sample. Here, we review the physical principles of mass spectrometry, the instrumentation used for these techniques, the terminology used in this field and applications to steroid analysis. PMID:22170384

Simultaneous mass detection for direct inlet mass spectrometry

International Nuclear Information System (INIS)

Gordon, R.L.

1979-05-01

The evolution of analytical techniques for application in trace analysis has led to interest in practical methods for real-time monitoring. Direct inlet mass spectrometry (DIMS) has been the subject of considerable activity in recent years. A DIMS instrument is described which consists of an inlet system designed to permit particles entrained in the inlet air stream to strike a hot, oxidized rhenium filament which serves as a surface ionization source. A mass analyzer and detection system then permits identification of the elemental composition of particulates which strike the filament

Four decades of joy in mass spectrometry

NARCIS (Netherlands)

Nibbering, N.M.M.

2006-01-01

Tremendous developments in mass spectrometry have taken place in the last 40 years. This holds for both the science and the instrumental revolutions in this field. In chemistry the research was heavily focused on organic molecules that upon electron ionization fragmented via complex mechanistic

imzML: Imaging Mass Spectrometry Markup Language: A common data format for mass spectrometry imaging.

Science.gov (United States)

Römpp, Andreas; Schramm, Thorsten; Hester, Alfons; Klinkert, Ivo; Both, Jean-Pierre; Heeren, Ron M A; Stöckli, Markus; Spengler, Bernhard

2011-01-01

Imaging mass spectrometry is the method of scanning a sample of interest and generating an "image" of the intensity distribution of a specific analyte. The data sets consist of a large number of mass spectra which are usually acquired with identical settings. Existing data formats are not sufficient to describe an MS imaging experiment completely. The data format imzML was developed to allow the flexible and efficient exchange of MS imaging data between different instruments and data analysis software.For this purpose, the MS imaging data is divided in two separate files. The mass spectral data is stored in a binary file to ensure efficient storage. All metadata (e.g., instrumental parameters, sample details) are stored in an XML file which is based on the standard data format mzML developed by HUPO-PSI. The original mzML controlled vocabulary was extended to include specific parameters of imaging mass spectrometry (such as x/y position and spatial resolution). The two files (XML and binary) are connected by offset values in the XML file and are unambiguously linked by a universally unique identifier. The resulting datasets are comparable in size to the raw data and the separate metadata file allows flexible handling of large datasets.Several imaging MS software tools already support imzML. This allows choosing from a (growing) number of processing tools. One is no longer limited to proprietary software, but is able to use the processing software which is best suited for a specific question or application. On the other hand, measurements from different instruments can be compared within one software application using identical settings for data processing. All necessary information for evaluating and implementing imzML can be found at http://www.imzML.org .

Radionuclide determination in environmental samples by inductively coupled plasma mass spectrometry

International Nuclear Information System (INIS)

Lariviere, Dominic; Taylor, Vivien F.; Evans, R. Douglas; Cornett, R. Jack

2006-01-01

The determination of naturally occurring and anthropogenic radionuclides in the environment by inductively coupled plasma mass spectrometry has gained recognition over the last fifteen years, relative to radiometric techniques, as the result of improvement in instrumental performance, sample introduction equipment, and sample preparation. With the increase in instrumental sensitivity, it is now possible to measure ultratrace levels (fg range) of many radioisotopes, including those with half-lives between 1 and 1000 years, without requiring very complex sample pre-concentration schemes. However, the identification and quantification of radioisotopes in environmental matrices is still hampered by a variety of analytical issues such as spectral (both atomic and molecular ions) and non-spectral (matrix effect) interferences and instrumental limitations (e.g., abundance sensitivity). The scope of this review is to highlight recent analytical progress and issues associated with the determination of radionuclides by inductively coupled plasma mass spectrometry. The impact of interferences, instrumental limitations (e.g., degree of ionization, abundance sensitivity, detection limits) and low sample-to-plasma transfer efficiency on the measurement of radionuclides by inductively coupled plasma mass spectrometry will be described. Solutions that overcome these issues will be discussed, highlighting their pros and cons and assessing their impact on the measurement of environmental radioactivity. Among the solutions proposed, mass and chemical resolution through the use of sector-field instruments and chemical reactions/collisions in a pressurized cell, respectively, will be described. Other methods, such as unique sample introduction equipment (e.g., laser ablation, electrothermal vaporisation, high efficiency nebulization) and instrumental modifications/optimizations (e.g., instrumental vacuum, radiofrequency power, guard electrode) that improve sensitivity and performance

Accelerator-based ultrasensitive mass spectrometry

International Nuclear Information System (INIS)

Gove, H.E.

1985-01-01

This chapter describes a new mass spectrometry technique involving charged particle accelerators normally used for basic research in nuclear science. Topics considered include the limitations of conventional mass spectrometry, the limitations of the direct measurement of radioactive decay, mass spectrometry using a tandem electrostatic accelerator, mass spectrometry using a cyclotron, how accelerator mass spectrometry circumvents the limitations of conventional mass spectrometry, measurements of stable isotopes, nuclear physics and astrophysics applications, modifications to existing accelerators, descriptions of dedicated systems, and future applications

Cluster secondary ion mass spectrometry microscope mode mass spectrometry imaging.

Science.gov (United States)

Kiss, András; Smith, Donald F; Jungmann, Julia H; Heeren, Ron M A

2013-12-30

Microscope mode imaging for secondary ion mass spectrometry is a technique with the promise of simultaneous high spatial resolution and high-speed imaging of biomolecules from complex surfaces. Technological developments such as new position-sensitive detectors, in combination with polyatomic primary ion sources, are required to exploit the full potential of microscope mode mass spectrometry imaging, i.e. to efficiently push the limits of ultra-high spatial resolution, sample throughput and sensitivity. In this work, a C60 primary source was combined with a commercial mass microscope for microscope mode secondary ion mass spectrometry imaging. The detector setup is a pixelated detector from the Medipix/Timepix family with high-voltage post-acceleration capabilities. The system's mass spectral and imaging performance is tested with various benchmark samples and thin tissue sections. The high secondary ion yield (with respect to 'traditional' monatomic primary ion sources) of the C60 primary ion source and the increased sensitivity of the high voltage detector setup improve microscope mode secondary ion mass spectrometry imaging. The analysis time and the signal-to-noise ratio are improved compared with other microscope mode imaging systems, all at high spatial resolution. We have demonstrated the unique capabilities of a C60 ion microscope with a Timepix detector for high spatial resolution microscope mode secondary ion mass spectrometry imaging. Copyright © 2013 John Wiley & Sons, Ltd.

Membrane introduction proton-transfer-reaction mass spectrometry

International Nuclear Information System (INIS)

Alexander, M.; Boscaini, E.; Maerk, T.; Lindinger, W.

2002-01-01

Proton-transfer-reaction mass spectrometry (PTR-MS) is a rapidly expanding field with multiple applications in ion physics, atmospheric chemistry, food chemistry, volatile organic compounds monitoring and biology. Initial studies that combine PTR-MS and membrane introduction mass spectrometry (MIMS) were researched and outlined. First using PTR-MS, certain fundamental physical properties of a poly-dimethylsiloxane (PDMS) membrane including solubilities and diffusion coefficients were measured. Second, it was shown how the chemical selectivity of the (PDMS) can be used to extend the capabilities of the PTR-MS instrument by eliminating certain isobaric interferences and excluding water from volatile organic compounds (VOCs). Experiments with mixtures of several VOCs (toluene, benzene, acetone, propanal, methanol) are presented. (nevyjel)

Direct analysis of samples by mass spectrometry: From elements to bio-molecules using laser ablation inductively couple plasma mass spectrometry and laser desorption/ionization mass spectrometry

Energy Technology Data Exchange (ETDEWEB)

Perdian, David C. [Iowa State Univ., Ames, IA (United States)

2009-01-01

Mass spectrometric methods that are able to analyze solid samples or biological materials with little or no sample preparation are invaluable to science as well as society. Fundamental research that has discovered experimental and instrumental parameters that inhibit fractionation effects that occur during the quantification of elemental species in solid samples by laser ablation inductively coupled plasma mass spectrometry is described. Research that determines the effectiveness of novel laser desorption/ionization mass spectrometric methods for the molecular analysis of biological tissues at atmospheric pressure and at high spatial resolution is also described. A spatial resolution is achieved that is able to analyze samples at the single cell level.

The Use of Gas Chromatography and Mass Spectrometry to Introduce General Chemistry Students to Percent Mass and Atomic Mass Calculations

Science.gov (United States)

Pfennig, Brian W.; Schaefer, Amy K.

2011-01-01

A general chemistry laboratory experiment is described that introduces students to instrumental analysis using gas chromatography-mass spectrometry (GC-MS), while simultaneously reinforcing the concepts of mass percent and the calculation of atomic mass. Working in small groups, students use the GC to separate and quantify the percent composition…

Extending the frontiers of mass spectrometric instrumentation and methods

Energy Technology Data Exchange (ETDEWEB)

Schieffer, Gregg Martin [Iowa State Univ., Ames, IA (United States)

2010-01-01

The focus of this dissertation is two-fold: developing novel analysis methods using mass spectrometry and the implementation and characterization of a novel ion mobility mass spectrometry instrumentation. The novel mass spectrometry combines ion trap for ion/ion reactions coupled to an ion mobility cell. The long term goal of this instrumentation is to use ion/ion reactions to probe the structure of gas phase biomolecule ions. The three ion source - ion trap - ion mobility - qTOF mass spectrometer (IT - IM - TOF MS) instrument is described. The analysis of the degradation products in coal (Chapter 2) and the imaging plant metabolites (Appendix III) fall under the methods development category. These projects use existing commercial instrumentation (JEOL AccuTOF MS and Thermo Finnigan LCQ IT, respectively) for the mass analysis of the degraded coal products and the plant metabolites, respectively. The coal degradation paper discusses the use of the DART ion source for fast and easy sample analysis. The sample preparation consisted of a simple 50 fold dilution of the soluble coal products in water and placing the liquid in front of the heated gas stream. This is the first time the DART ion source has been used for analysis of coal. Steven Raders under the guidance of John Verkade came up with the coal degradation projects. Raders performed the coal degradation reactions, worked up the products, and sent them to me. Gregg Schieffer developed the method and wrote the paper demonstrating the use of the DART ion source for the fast and easy sample analysis. The plant metabolite imaging project extends the use of colloidal graphite as a sample coating for atmospheric pressure LDI. DC Perdian and I closely worked together to make this project work. Perdian focused on building the LDI setup whereas Schieffer focused on the MSn analysis of the metabolites. Both Perdian and I took the data featured in the paper. Perdian was the primary writer of the paper and used it as a

Clinical review: improving the measurement of serum thyroglobulin with mass spectrometry.

Science.gov (United States)

Hoofnagle, Andrew N; Roth, Mara Y

2013-04-01

Serum thyroglobulin (Tg) measurements are central to the management of patients treated for differentiated thyroid carcinoma. For decades, Tg measurements have relied on methods that are subject to interference by commonly found substances in human serum and plasma, such as Tg autoantibodies. As a result, many patients need additional imaging studies to rule out cancer persistence or recurrence that could be avoided with more sensitive and specific testing methods. The aims of this review are to: 1) briefly review the interferences common to Tg immunoassays; 2) introduce readers to liquid chromatography-tandem mass spectrometry as a method for quantifying proteins in human serum/plasma; and 3) discuss the potential benefits and limitations of the method in the quantification of serum Tg. Mass spectrometric methods have traditionally lacked the sensitivity, robustness, and throughput to be useful clinical assays. These methods failed to meet the necessary clinical benchmarks due to the nature of the mass spectrometry workflow and instrumentation. Over the past few years, there have been major advances in reagents, automation, and instrumentation for the quantification of proteins using mass spectrometry. More recently, methods using mass spectrometry to detect and quantify Tg have been developed and are of sufficient quality to be used in the management of patients. Novel serum Tg assays that use mass spectrometry may avoid the issue of autoantibody interference and other problems with currently available immunoassays for Tg. Prospective studies are needed to fully understand the potential benefits of novel Tg assays to patients and care providers.

Atmospheric pressure ionization-tandem mass spectrometry of the phenicol drug family.

Science.gov (United States)

Alechaga, Élida; Moyano, Encarnación; Galceran, M Teresa

2013-11-01

In this work, the mass spectrometry behaviour of the veterinary drug family of phenicols, including chloramphenicol (CAP) and its related compounds thiamphenicol (TAP), florfenicol (FF) and FF amine (FFA), was studied. Several atmospheric pressure ionization sources, electrospray (ESI), atmospheric pressure chemical ionization and atmospheric pressure photoionization were compared. In all atmospheric pressure ionization sources, CAP, TAP and FF were ionized in both positive and negative modes; while for the metabolite FFA, only positive ionization was possible. In general, in positive mode, [M + H](+) dominated the mass spectrum for FFA, while the other compounds, CAP, TAP and FF, with lower proton affinity showed intense adducts with species present in the mobile phase. In negative mode, ESI and atmospheric pressure photoionization showed the deprotonated molecule [M-H](-), while atmospheric pressure chemical ionization provided the radical molecular ion by electron capture. All these ions were characterized by tandem mass spectrometry using the combined information obtained by multistage mass spectrometry and high-resolution mass spectrometry in a quadrupole-Orbitrap instrument. In general, the fragmentation occurred via cyclization and losses or fragmentation of the N-(alkyl)acetamide group, and common fragmentation pathways were established for this family of compounds. A new chemical structure for the product ion at m/z 257 for CAP, on the basis of the MS(3) and MS(4) spectra is proposed. Thermally assisted ESI and selected reaction monitoring are proposed for the determination of these compounds by ultra high-performance liquid chromatography coupled to tandem mass spectrometry, achieving instrumental detection limits down to 0.1 pg. Copyright © 2013 John Wiley & Sons, Ltd.

Technical and economical aspects of mass spectrometry in food and agricultural industries

International Nuclear Information System (INIS)

Cornu, Ayme

1975-01-01

Mass spectrometry proved to be very useful for solving analytical problems in food and agricultural industries. Its essential properties are: high resolution mass spectrometry allows to find the molecular structure of an isolated compound, even with a very small sample; associated with on line gas chromatographic separation, it gives the possibility to identify a great number of components in a small complex extract; isotope determinations by mass spectrometry give an essential contribution to follow kinetic mechanisms of formation of natural molecules in plant-growing, photosynthesis, fertilization, ..., leading to identification of the origin of foods and beverages. The economical aspect of mass spectrometry is characterized by the cost of investment in instrumentation and the necessary high level of competence of the technicians [fr

Native Mass Spectrometry in Fragment-Based Drug Discovery

Directory of Open Access Journals (Sweden)

Liliana Pedro

2016-07-01

Full Text Available The advent of native mass spectrometry (MS in 1990 led to the development of new mass spectrometry instrumentation and methodologies for the analysis of noncovalent protein–ligand complexes. Native MS has matured to become a fast, simple, highly sensitive and automatable technique with well-established utility for fragment-based drug discovery (FBDD. Native MS has the capability to directly detect weak ligand binding to proteins, to determine stoichiometry, relative or absolute binding affinities and specificities. Native MS can be used to delineate ligand-binding sites, to elucidate mechanisms of cooperativity and to study the thermodynamics of binding. This review highlights key attributes of native MS for FBDD campaigns.

Native Mass Spectrometry in Fragment-Based Drug Discovery.

Science.gov (United States)

Pedro, Liliana; Quinn, Ronald J

2016-07-28

The advent of native mass spectrometry (MS) in 1990 led to the development of new mass spectrometry instrumentation and methodologies for the analysis of noncovalent protein-ligand complexes. Native MS has matured to become a fast, simple, highly sensitive and automatable technique with well-established utility for fragment-based drug discovery (FBDD). Native MS has the capability to directly detect weak ligand binding to proteins, to determine stoichiometry, relative or absolute binding affinities and specificities. Native MS can be used to delineate ligand-binding sites, to elucidate mechanisms of cooperativity and to study the thermodynamics of binding. This review highlights key attributes of native MS for FBDD campaigns.

Space Applications of Mass Spectrometry. Chapter 31

Science.gov (United States)

Hoffman, John H.; Griffin, Timothy P.; Limero, Thomas; Arkin, C. Richard

2010-01-01

Mass spectrometers have been involved in essentially all aspects of space exploration. This chapter outlines some of these many uses. Mass spectrometers have not only helped to expand our knowledge and understanding of the world and solar system around us, they have helped to put man safely in space and expand our frontier. Mass spectrometry continues to prove to be a very reliable, robust, and flexible analytical instrument, ensuring that its use will continue to help aid our investigation of the universe and this small planet that we call home.

Application of Laser Mass Spectrometry to Art and Archaeology

Science.gov (United States)

Gulian, Lase Lisa E.; Callahan, Michael P.; Muliadi, Sarah; Owens, Shawn; McGovern, Patrick E.; Schmidt, Catherine M.; Trentelman, Karen A.; deVries, Mattanjah S.

2011-01-01

REMPI laser mass spectrometry is a combination of resonance enhanced multiphoton ionization spectroscopy and time of flight mass spectrometry, This technique enables the collection of mass specific optical spectra as well as of optically selected mass spectra. Analytes are jet-cooled by entrainment in a molecular beam, and this low temperature gas phase analysis has the benefit of excellent vibronic resolution. Utilizing this method, mass spectrometric analysis of historically relevant samples can be simplified and improved; Optical selection of targets eliminates the need for chromatography while knowledge of a target's gas phase spectroscopy allows for facile differentiation of molecules that are in the aqueous phase considered spectroscopically indistinguishable. These two factors allow smaller sample sizes than commercial MS instruments, which in turn will require less damage to objects of antiquity. We have explored methods to optimize REMPI laser mass spectrometry as an analytical tool to archaeology using theobromine and caffeine as molecular markers in Mesoamerican pottery, and are expanding this approach to the field of art to examine laccaic acid in shellacs.

Mass spectrometry. [review of techniques

Science.gov (United States)

Burlingame, A. L.; Kimble, B. J.; Derrick, P. J.

1976-01-01

Advances in mass spectrometry (MS) and its applications over the past decade are reviewed in depth, with annotated literature references. New instrumentation and techniques surveyed include: modulated-beam MS, chromatographic MS on-line computer techniques, digital computer-compatible quadrupole MS, selected ion monitoring (mass fragmentography), and computer-aided management of MS data and interpretation. Areas of application surveyed include: organic MS and electron impact MS, field ionization kinetics, appearance potentials, translational energy release, studies of metastable species, photoionization, calculations of molecular orbitals, chemical kinetics, field desorption MS, high pressure MS, ion cyclotron resonance, biochemistry, medical/clinical chemistry, pharmacology, and environmental chemistry and pollution studies.

Lipidomic mass spectrometry and its application in neuroscience

Institute of Scientific and Technical Information of China (English)

Mabel; Enriquez-Algeciras; Sanjoy; K; Bhattacharya

2013-01-01

Central and peripheral nervous systems are lipid rich tissues. Lipids, in the context of lipid-protein complexes, surround neurons and provide electrical insulation for transmission of signals allowing neurons to remain embedded within a conducting environment. Lipids play a key role in vesicle formation and fusion in synapses. They provide means of rapid signaling, cell motility and migration for astrocytes and other cell types that surround and play supporting roles neurons. Unlike many other signaling molecules, lipids are capable of multiple signaling events based on the different fragments generated from a single precursor during each event. Lipidomics, until recently suffered from two major disadvantages:(1) level of expertise required an overwhelming amount of chemical detail to correctly identify a vast number of different lipids which could be close in their chemical reactivity; and(2) high amount of purified compounds needed by analytical techniques to determine their structures. Advances in mass spectrometry have enabled overcoming these two limitations. Mass spectrometry offers a great degree of simplicity in identification and quantification of lipids directly extracted from complex biological mixtures. Mass spectrometers can be regarded to as mass analyzers. There are those that separate and analyze the product ion fragments in space(spatial) and those which separate product ions in time in the same space(temporal). Databases and standardized instrument parameters have further aided the capabilities of the spatial instruments while recent advances in bioinformatics have made the identification and quantification possible using temporal instruments.

microMS: A Python Platform for Image-Guided Mass Spectrometry Profiling

Science.gov (United States)

Comi, Troy J.; Neumann, Elizabeth K.; Do, Thanh D.; Sweedler, Jonathan V.

2017-09-01

Image-guided mass spectrometry (MS) profiling provides a facile framework for analyzing samples ranging from single cells to tissue sections. The fundamental workflow utilizes a whole-slide microscopy image to select targets of interest, determine their spatial locations, and subsequently perform MS analysis at those locations. Improving upon prior reported methodology, a software package was developed for working with microscopy images. microMS, for microscopy-guided mass spectrometry, allows the user to select and profile diverse samples using a variety of target patterns and mass analyzers. Written in Python, the program provides an intuitive graphical user interface to simplify image-guided MS for novice users. The class hierarchy of instrument interactions permits integration of new MS systems while retaining the feature-rich image analysis framework. microMS is a versatile platform for performing targeted profiling experiments using a series of mass spectrometers. The flexibility in mass analyzers greatly simplifies serial analyses of the same targets by different instruments. The current capabilities of microMS are presented, and its application for off-line analysis of single cells on three distinct instruments is demonstrated. The software has been made freely available for research purposes. [Figure not available: see fulltext.

Proceedings of twelfth ISMAS symposium cum workshop on mass spectrometry

International Nuclear Information System (INIS)

Alamelu, D.; Jaison, P.G.; Aggarwal, S.K.

2007-03-01

Mass Spectrometry is an important analytical tool and has encompassed almost all branches of science and technology including Agricultural, biology, Chemistry, Earth sciences, environment, Forensic Science, Medical Sciences, Hydrology, Nuclear Technology, Oceanography, Physics etc. Recent advancements in the instrumentation of Mass Spectrometry have further strengthened its role for various applications. It is indeed a matter of great pleasure to present this special Issue of ISMAS Bulletin which is brought out on the occasion of the 12th ISMAS Symposium cum Workshop on Mass spectrometry (12th ISMAS-WS 2007) being held at Cidade-de-Goa, Dona Paula, Goa from March 25 to 30, 2007 in association with National Institute of Oceanography, Goa. This Symposium cum Workshop is co-sponsored by Scientific Departments of Government of India. Papers relevant to INIS are indexed separately

The allure of mass spectrometry: From an earlyday chemist's perspective.

Science.gov (United States)

Tőkés, László

2017-07-01

This reminiscing review article is an account of the author's fascination and involvements with mass spectrometry from the perspective of an organic chemist with an interest in natural product chemistry. It covers a period from 1961 through the mid 1990s as mass spectrometry evolved form a novelty technique to become a most widely used analytical technique. Following a brief synopsis of my pathway to mass spectrometry, my research efforts in this field are presented with a focus mainly on evolving principles and technologies which I had personal involvements with. To provide historical perspectives, discussions of these developments are accompanied by brief outlines of the relevant state-of-the-art, shedding light on the technical and conceptual challenges encountered during those early days in mass spectrometry. Examples are presented of my involvements with basic and applied research in mass spectrometry during graduate studies at Stanford University and close to three decade tenure in pharmaceutical research at Syntex Research. My basic research interests focused mainly on principles of electron ionization induced fragmentation mechanisms, with an emphasis on steroids and other model compounds. Extensive deuterium labeling evidence was used to determine the fragmentation mechanisms of the diagnostically significant ions in the spectra of numerous model compounds, uncovering examples of wide-ranging hydrogen transfers, skeletal rearrangements, methyl and phenyl migrations, stereoselective fragmentations and low and high energy fragmentation processes. Depiction of the industrial research phase of my career includes comments on the pivotal role mass spectrometry played on advancing modern pharmaceutical research. Examples are presented of involvements with instrumental developments and a few select cases of applied research, including studies of bile mechanisms in vertebrates, identification of bisphenol-A leaching from sterilized polycarbonate containers, high

Operational Experience of an Open-Access, Subscription-Based Mass Spectrometry and Proteomics Facility

Science.gov (United States)

Williamson, Nicholas A.

2018-03-01

This paper discusses the successful adoption of a subscription-based, open-access model of service delivery for a mass spectrometry and proteomics facility. In 2009, the Mass Spectrometry and Proteomics Facility at the University of Melbourne (Australia) moved away from the standard fee for service model of service provision. Instead, the facility adopted a subscription- or membership-based, open-access model of service delivery. For a low fixed yearly cost, users could directly operate the instrumentation but, more importantly, there were no limits on usage other than the necessity to share available instrument time with all other users. All necessary training from platform staff and many of the base reagents were also provided as part of the membership cost. These changes proved to be very successful in terms of financial outcomes for the facility, instrument access and usage, and overall research output. This article describes the systems put in place as well as the overall successes and challenges associated with the operation of a mass spectrometry/proteomics core in this manner. [Figure not available: see fulltext.

Imaging mass spectrometry statistical analysis.

Science.gov (United States)

Jones, Emrys A; Deininger, Sören-Oliver; Hogendoorn, Pancras C W; Deelder, André M; McDonnell, Liam A

2012-08-30

Imaging mass spectrometry is increasingly used to identify new candidate biomarkers. This clinical application of imaging mass spectrometry is highly multidisciplinary: expertise in mass spectrometry is necessary to acquire high quality data, histology is required to accurately label the origin of each pixel's mass spectrum, disease biology is necessary to understand the potential meaning of the imaging mass spectrometry results, and statistics to assess the confidence of any findings. Imaging mass spectrometry data analysis is further complicated because of the unique nature of the data (within the mass spectrometry field); several of the assumptions implicit in the analysis of LC-MS/profiling datasets are not applicable to imaging. The very large size of imaging datasets and the reporting of many data analysis routines, combined with inadequate training and accessible reviews, have exacerbated this problem. In this paper we provide an accessible review of the nature of imaging data and the different strategies by which the data may be analyzed. Particular attention is paid to the assumptions of the data analysis routines to ensure that the reader is apprised of their correct usage in imaging mass spectrometry research. Copyright © 2012 Elsevier B.V. All rights reserved.

Mass spectrometry in clinical chemistry

International Nuclear Information System (INIS)

Pettersen, J.E.

1977-01-01

A brief description is given of the functional elements of a mass spectrometer and of some currently employed mass spectrometric techniques, such as combined gas chromatography-mass spectrometry, mass chromatography, and selected ion monitoring. Various areas of application of mass spectrometry in clinical chemistry are discussed, such as inborn errors of metabolism and other metabolic disorders, intoxications, quantitative determinations of drugs, hormones, gases, and trace elements, and the use of isotope dilution mass spectrometry as a definitive method for the establishment of true values for concentrations of various compounds in reference sera. It is concluded that mass spectrometry is of great value in clinical chemistry. (Auth.)

Origin of the chemical noise in ambient mass spectrometry

International Nuclear Information System (INIS)

Yang Shuiping; Zhu Zhiqiang; Huang Longzhu; Zhang Xinglei; Zhu Tenggao; Chen Huanwen

2012-01-01

The instrumental background of ambient mass spectrometry, (API-MS) is analyzed and the possible potential origins of the background noise is identified. According to the mass spectra obtained using the API-MS instruments by different manufacturers, the characteristic fragment ions all indicated that the background noise are resulted from the phthalates such as diethyl phthalate (DEP), dibutyl phthalate (DBP), benzyl butyl phthalate (BBP), bis (2-ethylhexyl) phthalate (DEHP), and silicones such as decamethylcyclopentasiloxane (D5) and dodecamethylcyclohexasiloxane (D6). These chemicals are probably released from the polymeric materials used in the ionization sources, such as O-type sealing ring etc. In addition, the instrumental background has to be considered especially during the analysis of phthalate and peptide compounds. (authors)

Atomic mass spectrometry

International Nuclear Information System (INIS)

Sanz-Medel, A.

1997-01-01

The elemental inorganic analysis seems to be dominated today by techniques based on atomic spectrometry. After an evaluation of advantages and limitations of using mass analysers (ion detectors) versus conventional photomultipliers (photon detector) a brief review of the more popular techniques of the emerging Atomic Mass spectrometry is carried out. Their huge potential for inorganic trace analysis is such that in the future we could well witness how this end of the century and millennium marked the fall of the photons empire in Analytical Atomic Spectrometry. (Author)

Mass Spectrometry on Future Mars Landers

Science.gov (United States)

Brinckerhoff, W. B.; Mahaffy, P. R.

2011-01-01

Mass spectrometry investigations on the 2011 Mars Science Laboratory (MSL) and the 2018 ExoMars missions will address core science objectives related to the potential habitability of their landing site environments and more generally the near-surface organic inventory of Mars. The analysis of complex solid samples by mass spectrometry is a well-known approach that can provide a broad and sensitive survey of organic and inorganic compounds as well as supportive data for mineralogical analysis. The science value of such compositional information is maximized when one appreciates the particular opportunities and limitations of in situ analysis with resource-constrained instrumentation in the context of a complete science payload and applied to materials found in a particular environment. The Sample Analysis at Mars (SAM) investigation on MSL and the Mars Organic Molecule Analyzer (MOMA) investigation on ExoMars will thus benefit from and inform broad-based analog field site work linked to the Mars environments where such analysis will occur.

Mass spectrometry and tandem mass spectrometry of citrus limonoids.

Science.gov (United States)

Tian, Qingguo; Schwartz, Steven J

2003-10-15

Methods for atmospheric pressure chemical ionization tandem mass spectrometry (APCI-MS/MS) of citrus limonoid aglycones and electrospray ionization tandem mass spectrometry (ESI-MS/MS) of limonoid glucosides are reported. The fragmentation patterns of four citrus limonoid aglycones (limonin, nomilin, obacunone, and deacetylnomilin) and six limonoid glucosides, that is, limonin 17-beta-D-glucopyranoside (LG), nomilin 17-beta-D-glucopyranoside (NG), nomilinic acid 17-beta-D-glucopyranoside (NAG), deacetyl nomilinic acid 17-beta-D-glucopyranoside (DNAG), obacunone 17-beta-D-glucopyranoside (OG), and obacunoic acid 17-beta-D-glucopyranoside (OAG) were investigated using a quadruple mass spectrometer in low-energy collisionally activated dissociation (CAD). The four limonoid aglycones and four limonoid glucosides (LG, OG, NAG, and DNAG) were purified from citrus seeds; the other two limonoid glucosides (NG and OAG) were tentatively identified in the crude extract of grapefruit seeds by ESI mass spectrometry in both positive and negative ion analysis. Ammonium hydroxide or acetic acid was added to the mobile phase to facilitate ionization. During positive ion APCI analysis of limonoid aglycones, protonated molecular ion, [M + H]+, or adduct ion, [M + NH3 + H]-, was formed as base peaks when ammonium hydroxide was added to the mobile phase. Molecular anions or adduct ions with acetic acid ([M + HOAc - H] and [M + HOAc]-) or a deprotonated molecular ion were produced during negative ion APCI analysis of limonoid aglycones, depending on the mobile-phase modifier used. Positive ion ESI-MS of limonoid glucosides produced adduct ions of [M + H + NH3]+, [M + Na]+, and [M + K]+ when ammonium hydroxide was added to the mobile phase. After collisionally activated dissociation (CAD) of the limonoid aglycone molecular ions in negative ion APCI analysis, fragment ions indicated structural information of the precursor ions, showing the presence of methyl, carboxyl, and oxygenated ring

Traveling-wave ion mobility mass spectrometry of protein complexes

DEFF Research Database (Denmark)

Salbo, Rune; Bush, Matthew F; Naver, Helle

2012-01-01

The collision cross-section (Ω) of a protein or protein complex ion can be measured using traveling-wave (T-wave) ion mobility (IM) mass spectrometry (MS) via calibration with compounds of known Ω. The T-wave Ω-values depend strongly on instrument parameters and calibrant selection. Optimization ...

Eleventh ISMAS workshop on mass spectrometry

International Nuclear Information System (INIS)

Aggarwal, S.K.; Jaison, P.G.

2004-10-01

This volume deals with the latest developments in this field, exposing the innumerable applications of mass spectrometry. The topics covered include basic fundamentals of mass spectrometry, qualitative and quantitative aspects and data interpretation, maintenance of mass spectrometers, selection of a mass spectrometer, its applications in various branches of science as well as recent advances in mass spectrometry. Emphasis is also laid on the practical aspects of mass spectrometry. Papers relevant to INIS are indexed separately

The combined measurement of uranium by alpha spectrometry and secondary ion mass spectrometry (SIMS)

International Nuclear Information System (INIS)

Harvan, D.

2009-01-01

The aim of thesis was to found the dependence between radiometric method - alpha spectrometry and surface sensitive method - Secondary Ion Mass Spectrometry (SIMS). Uranium or naturally occurring uranium isotopes were studied. Samples (high polished stainless steel discs) with uranium isotopes were prepared by electrodeposition. Samples were measured by alpha spectrometry after electrodeposition and treatment. It gives surface activities. Weights, as well as surface's weights of uranium isotopes were calculated from their activities, After alpha spectrometry samples were analyzed by TOF-SIMS IV instrument in International Laser Centre in Bratislava. By the SIMS analysis intensities of uranium-238 were obtained. The interpretation of SIMS intensities vs. surface activity, or surface's weights of uranium isotopes indicates the possibility to use SIMS in quantitative analysis of surface contamination by uranium isotopes, especially 238 U. (author)

Radiocarbon positive-ion mass spectrometry

Energy Technology Data Exchange (ETDEWEB)

Freeman, Stewart P.H.T.; Shanks, Richard P. [Scottish Universities Environmental Research Centre (SUERC), Scottish Enterprise Technology Park, East Kilbride G75 0QF (United Kingdom); Donzel, Xavier; Gaubert, Gabriel [Pantechnik S.A., 13 Rue de la Résistance, 14400 Bayeux (France)

2015-10-15

Proof-of-principle of a new mass spectrometric technique for radiocarbon measurement is demonstrated. Interfering nitrogen and hydrocarbon molecules are largely eliminated in a charge-exchange cell operating on non-metallic gas. The positive-to-negative ion conversion is the reverse of that conventionally used in accelerator mass spectrometry (AMS) and is compatible with plasma ion sources that may be significantly more efficient and capable of greater output than are AMS sputter ion sources. The Nanogan electron cyclotron resonance (ECR) ion source employed exhibited no sample memory and the >50 kyrs age range of AMS was reproduced. A bespoke prototype new instrument is now required to optimise the plasma and cell physics and to realise hypothetical performance gains over AMS.

Radiocarbon positive-ion mass spectrometry

International Nuclear Information System (INIS)

Freeman, Stewart P.H.T.; Shanks, Richard P.; Donzel, Xavier; Gaubert, Gabriel

2015-01-01

Proof-of-principle of a new mass spectrometric technique for radiocarbon measurement is demonstrated. Interfering nitrogen and hydrocarbon molecules are largely eliminated in a charge-exchange cell operating on non-metallic gas. The positive-to-negative ion conversion is the reverse of that conventionally used in accelerator mass spectrometry (AMS) and is compatible with plasma ion sources that may be significantly more efficient and capable of greater output than are AMS sputter ion sources. The Nanogan electron cyclotron resonance (ECR) ion source employed exhibited no sample memory and the >50 kyrs age range of AMS was reproduced. A bespoke prototype new instrument is now required to optimise the plasma and cell physics and to realise hypothetical performance gains over AMS.

Ninth ISMAS workshop on mass spectrometry

International Nuclear Information System (INIS)

Aggarwal, S.K.

2000-12-01

Mass spectrometry has wide-ranging applications in such diverse areas as nuclear industry, agriculture, drugs, environment, petroleum and lentils. There is an urgent need to absorb and assimilate state-of-the-art technological developments in the field. Emerging trends in atomic mass spectrometry, advances in organic mass spectrometry, qualitative and quantitative analyses by mass spectrometry and mass spectrometry in oceanography are some of the areas that need to be expeditiously examined and are covered in this volume. Papers relevant to INIS are indexed separately

Fourier Transform Mass Spectrometry

Science.gov (United States)

Scigelova, Michaela; Hornshaw, Martin; Giannakopulos, Anastassios; Makarov, Alexander

2011-01-01

This article provides an introduction to Fourier transform-based mass spectrometry. The key performance characteristics of Fourier transform-based mass spectrometry, mass accuracy and resolution, are presented in the view of how they impact the interpretation of measurements in proteomic applications. The theory and principles of operation of two types of mass analyzer, Fourier transform ion cyclotron resonance and Orbitrap, are described. Major benefits as well as limitations of Fourier transform-based mass spectrometry technology are discussed in the context of practical sample analysis, and illustrated with examples included as figures in this text and in the accompanying slide set. Comparisons highlighting the performance differences between the two mass analyzers are made where deemed useful in assisting the user with choosing the most appropriate technology for an application. Recent developments of these high-performing mass spectrometers are mentioned to provide a future outlook. PMID:21742802

ISMAS international discussion meet on elemental mass spectrometry in health and environmental sciences

International Nuclear Information System (INIS)

Aggarwal, S.K.; Jaison, P.G.; Telmore, V.M.

2011-04-01

Mass spectrometry is an indispensable analytical tool associated with almost all branches of science including biology, chemistry, earth sciences, nuclear science, physics, etc. The technique holds tremendous potential owing to its high sensitivity, selectivity and its ability to measure small changes in the isotopic abundances of different elements. Innovations in mass spectrometry instrumentation are further widening the scope by making it possible to handle very large bio-molecules and polymers. New techniques for mass analysis, novel designs for ionization and developments in electronic accessories have contributed to elevate mass spectrometry to a position of prime importance in research. Development in mass spectrometry has revolutionized the study of micro-nutrient metabolism, of biologically active compounds and for drug discovery in pharmaceutical research. Elemental mass spectrometry is making major contributions to food toxicology, food forensics, and study of metabolism of nutrient minerals including Fe, Zn, Ca, Cu and Se. The area of speciation analysis using hyphenated techniques as well as electro-spray ionization have undergone a phenomenal evolution and development in the recent past. Impressive progress in mass spectrometry towards lower detection limits, higher resolution and molecule-specific detection at trace levels in complex matrices allows new frontiers to be crossed. Papers relevant to INIS are indexed separately

Liulin-type spectrometry-dosimetry instruments

International Nuclear Information System (INIS)

Dachev, T.; Dimitrov, P.; Tomov, B.; Matviichuk, Y.; Spurny, F.; Ploc, O.; Brabcova, K.; Jadrnickova, I.

2011-01-01

The main purpose of Liulin-type spectrometry-dosimetry instruments (LSDIs) is cosmic radiation monitoring at the workplaces. An LSDI functionally is a low mass, low power consumption or battery-operated dosemeter. LSDIs were calibrated in a wide range of radiation fields, including radiation sources, proton and heavy-ion accelerators and CERN-EC high-energy reference field. Since 2000, LSDIs have been used in the scientific programmes of four manned space flights on the American Laboratory and ESA Columbus modules and on the Russian segment of the International Space Station, one Moon spacecraft and three spacecraft around the Earth, one rocket, two balloons and many aircraft flights. In addition to relative low price, LSDIs have proved their ability to qualify the radiation field on the ground and on the above-mentioned carriers. (authors)

Glycomics using mass spectrometry

OpenAIRE

Wuhrer, Manfred

2013-01-01

Mass spectrometry plays an increasingly important role in structural glycomics. This review provides an overview on currently used mass spectrometric approaches such as the characterization of glycans, the analysis of glycopeptides obtained by proteolytic cleavage of proteins and the analysis of glycosphingolipids. The given examples are demonstrating the application of mass spectrometry to study glycosylation changes associated with congenital disorders of glycosylation, lysosomal storage di...

Mass Spectrometry Imaging of Biological Tissue: An Approach for Multicenter Studies

Energy Technology Data Exchange (ETDEWEB)

Rompp, Andreas; Both, Jean-Pierre; Brunelle, Alain; Heeren, Ronald M.; Laprevote, Olivier; Prideaux, Brendan; Seyer, Alexandre; Spengler, Bernhard; Stoeckli, Markus; Smith, Donald F.

2015-03-01

Mass spectrometry imaging has become a popular tool for probing the chemical complexity of biological surfaces. This led to the development of a wide range of instrumentation and preparation protocols. It is thus desirable to evaluate and compare the data output from different methodologies and mass spectrometers. Here, we present an approach for the comparison of mass spectrometry imaging data from different laboratories (often referred to as multicenter studies). This is exemplified by the analysis of mouse brain sections in five laboratories in Europe and the USA. The instrumentation includes matrix-assisted laser desorption/ionization (MALDI)-time-of-flight (TOF), MALDI-QTOF, MALDIFourier transform ion cyclotron resonance (FTICR), atmospheric-pressure (AP)-MALDI-Orbitrap, and cluster TOF-secondary ion mass spectrometry (SIMS). Experimental parameters such as measurement speed, imaging bin width, and mass spectrometric parameters are discussed. All datasets were converted to the standard data format imzML and displayed in a common open-source software with identical parameters for visualization, which facilitates direct comparison of MS images. The imzML conversion also allowed exchange of fully functional MS imaging datasets between the different laboratories. The experiments ranged from overview measurements of the full mouse brain to detailed analysis of smaller features (depending on spatial resolution settings), but common histological features such as the corpus callosum were visible in all measurements. High spatial resolution measurements of AP-MALDI-Orbitrap and TOF-SIMS showed comparable structures in the low-micrometer range. We discuss general considerations for planning and performing multicenter studies in mass spectrometry imaging. This includes details on the selection, distribution, and preparation of tissue samples as well as on data handling. Such multicenter studies in combination with ongoing activities for reporting guidelines, a common

Mass Spectrometry-Based Biomarker Discovery.

Science.gov (United States)

Zhou, Weidong; Petricoin, Emanuel F; Longo, Caterina

2017-01-01

The discovery of candidate biomarkers within the entire proteome is one of the most important and challenging goals in proteomic research. Mass spectrometry-based proteomics is a modern and promising technology for semiquantitative and qualitative assessment of proteins, enabling protein sequencing and identification with exquisite accuracy and sensitivity. For mass spectrometry analysis, protein extractions from tissues or body fluids and subsequent protein fractionation represent an important and unavoidable step in the workflow for biomarker discovery. Following extraction of proteins, the protein mixture must be digested, reduced, alkylated, and cleaned up prior to mass spectrometry. The aim of our chapter is to provide comprehensible and practical lab procedures for sample digestion, protein fractionation, and subsequent mass spectrometry analysis.

Optical spectroscopy versus mass spectrometry: The race for fieldable isotopic analysis

International Nuclear Information System (INIS)

Barshick, C.M.; Young, J.P.; Shaw, R.W.

1995-01-01

Several techniques have been developed to provide on-site isotopic analyses, including decay-counting and mass spectrometry, as well as methods that rely on the accessibility of optical transitions for isotopic selectivity (e.g., laser-induced fluorescence and optogalvanic spectroscopy). The authors have been investigating both mass spectrometry and optogalvanic spectroscopy for several years. Although others have considered these techniques for isotopic analysis, the authors have focussed on the use of a dc glow discharge for atomization and ionization, and a demountable discharge cell for rapid sample exchange. The authors' goal is a fieldable instrument that provides useful uranium isotope ratio information

Ultra-sensitive radionuclide spectrometry. Radiometrics and mass spectrometry synergy

International Nuclear Information System (INIS)

Povinec, P.P.

2005-01-01

Recent developments in radiometrics and mass spectrometry techniques for ultra-sensitive analysis of radionuclides in the marine environment are reviewed. In the radiometrics sector the dominant development has been the utilization of large HPGe detectors in underground laboratories with anti-cosmic or anti-Compton shielding for the analysis of short and medium-lived radionuclides in the environment. In the mass spectrometry sector, applications of inductively coupled plasma mass spectrometry (ICP-MS) and accelerator mass spectrometry (AMS) for the analysis of long-lived radionuclides in the environment are the most important recent achievements. The recent developments do not only considerably decrease the detection limits for several radionuclides (up to several orders of magnitude), but they also enable to decrease sample volumes so that sampling, e.g., of the water column can be much easier and more effective. A comparison of radiometrics and mass spectrometry results for the analysis of radionuclides in the marine environment shows a reasonable agreement - within quoted uncertainties, for wide range of activities and different sample matrices analyzed. (author)

Thermal ionisation mass spectrometry: recent developments and future prospects

International Nuclear Information System (INIS)

Aggarwal, S.K.

1996-01-01

This paper presents the current state of art of thermal ionization mass spectrometry (TIMS) instrumentation and highlights some of the recent applications of TIMS in geological, biological and nuclear sciences with special emphasis on some of the recent work undertaken in the area of nuclear science and technology. A few examples from the published literature are also discussed here

Proceedings of the second Alfred O. Nier symposium on inorganic mass spectrometry

International Nuclear Information System (INIS)

Green, L.W.

1996-01-01

The proceedings are organized under the following headings: thermal ionization mass spectrometry, applications and instrumentation; inductively coupled plasma and glow discharge mass spectrometry; gases; laser resonance ionization; general. Topics of nuclear significance include: determination of trace iron in zirconium; characterization of uranium in surface waters; subpicogram quantities of technetium; measurement of isotope ratios; determination of hydrogen and deuterium in zirconium and its alloys; Kr and Xe isotopic measurements; Kr-85 detection; SIMS study of zirconium corrosion; isotopes at CEA (Commissariat a l'Energie Atomique). All the papers have been abstracted separately for INIS

Selective-Reagent-Ionization Mass Spectrometry: New Prospects for Atmospheric Research

Science.gov (United States)

Sulzer, Philipp; Jordan, Alfons; Hartungen, Eugen; Hanel, Gernot; Jürschik, Simone; Herbig, Jens; Märk, Lukas; Märk, Tilmann D.

2014-05-01

Proton-Transfer-Reaction Mass Spectrometry (PTR-MS), which was introduced to the scientific community in the 1990's, has quickly evolved into a well-established technology for atmospheric research and environmental chemistry [1]. Advantages of PTR-MS are i) high sensitivities of several hundred cps/ppbv, ii) detection limits at or below the pptv level, iii) direct injection sampling (i.e. no sample preparation), iv) response times in the 100 ms regime and v) online quantification. However, one drawback is a somehow limited selectivity, as in case of quadrupole mass filter based instruments only information about nominal m/z are available. In Time-Of-Flight (TOF) mass analyzer based instruments selectivity is drastically increased by a high mass resolution of up to 8000 m/Δm, but e.g. isomers still cannot be separated. In 2009 we introduced an advanced version of PTR-MS, which permits switching the reagent ions from H3O+ to NO+ and O2+, respectively [2]. This novel type of instrumentation was called Selective-Reagent-Ionization Mass Spectrometry (SRI-MS) and has been successfully used to separate isomers, e.g. the biogenic compounds isoprene and 2-methyl-3-buten-2-ol as shown by Karl et al. [3]. Switching the reagent ions dramatically increases selectivity and thus applicability of SRI-MS in atmospheric research. Here we report on the latest results utilizing an even more advanced embodiment of SRI-MS enabling the use of the additional reagent ions Kr+ and Xe+ [4]. With this technology important atmospheric compounds, such as CO2, CO, CH4, O2, etc. can be quantified and selectivity is increased even further. We present comparison data between diesel and gasoline car exhaust gases and quantitative data on indoor air for these compounds, which are not detectable with classical PTR-MS. Additionally, we show very recent examples of isomers which cannot be separated with PTR-MS but can clearly be distinguished with SRI-MS. Finally, we give an overview of ongoing SRI

Instrumental development and data processing

International Nuclear Information System (INIS)

Franzen, J.

1978-01-01

A review of recent developments in mass spectrometry instrumentation is presented under the following headings: introduction (scope of mass spectrometry compared with neighbouring fields); ion sources and ionization techniques; spectrometers (instrumental developments); measuring procedures; coupling techniques; data systems; conclusions (that mass spectrometry should have a broader basis and that there would be mutual profit from a better penetration of mass spectrometry into fields of routine application). (U.K.)

Mass Spectrometry Parameters Optimization for the 46 Multiclass Pesticides Determination in Strawberries with Gas Chromatography Ion-Trap Tandem Mass Spectrometry

Science.gov (United States)

Fernandes, Virgínia C.; Vera, Jose L.; Domingues, Valentina F.; Silva, Luís M. S.; Mateus, Nuno; Delerue-Matos, Cristina

2012-12-01

Multiclass analysis method was optimized in order to analyze pesticides traces by gas chromatography with ion-trap and tandem mass spectrometry (GC-MS/MS). The influence of some analytical parameters on pesticide signal response was explored. Five ion trap mass spectrometry (IT-MS) operating parameters, including isolation time (IT), excitation voltage (EV), excitation time (ET), maximum excitation energy or " q" value (q), and isolation mass window (IMW) were numerically tested in order to maximize the instrument analytical signal response. For this, multiple linear regression was used in data analysis to evaluate the influence of the five parameters on the analytical response in the ion trap mass spectrometer and to predict its response. The assessment of the five parameters based on the regression equations substantially increased the sensitivity of IT-MS/MS in the MS/MS mode. The results obtained show that for most of the pesticides, these parameters have a strong influence on both signal response and detection limit. Using the optimized method, a multiclass pesticide analysis was performed for 46 pesticides in a strawberry matrix. Levels higher than the limit established for strawberries by the European Union were found in some samples.

Proceedings of the twenty ninth ISMAS international symposium on mass spectrometry

International Nuclear Information System (INIS)

Aggarwal, Suresh K.; Pranaw Kumar; Jaison, P.G.; Sarkar, Arnab; Telmore, Vijay M.

2015-02-01

Mass spectrometry is a truly multi-disciplinary science and has emerged as an indispensable analytical tool due to its high sensitivity, specificity and universality. It is playing a key role in variety of scientific disciplines of chemistry, physics, biology, archaeology, material science etc. Progress in the field of mass spectrometry in the last two decades has led to the advent of new ion sources, improvements in existing mass analyzers and introduction of hybrid mass analyzers. As the technique continues to advance, many new applications have emerged particularly in health sciences and for forensic applications. The current world scenario demands determination at single atom and single molecule with high specificity. The vendors in the international mass spectrometric instrumentation market are guided by these requirements as well as the inputs from mass spectrometrists around the world engaged in new developments. Papers relevant to INIS are indexed separately

A REVIEW ON MASS SPECTROMETRY DETECTORS

OpenAIRE

Khatri Neetu; Gupta Ankit; Taneja Ruchi; Bilandi Ajay; Beniwal Prashant

2012-01-01

Mass spectrometry is an analytical technique for "weighing" molecules. Obviously, this is not done with a conventional scale or balance. Instead, mass spectrometry is based upon the principle of the motion of a charged particle that is called an ion, in an electric or magnetic field. The mass to charge ratio (m/z) of the ion affects particles motion. Since the charge of an electron is known, the mass to charge ratio (m/z) is a measurement of mass of an ion. Mass spectrometry research focuses ...

Mass Spectrometry for Large Undergraduate Laboratory Sections

Science.gov (United States)

Illies, A.; Shevlin, P. B.; Childers, G.; Peschke, M.; Tsai, J.

1995-08-01

min. Under these conditions each analysis takes the student about 10 min and two students are scheduled per 20 min block. Since the instrument is under computer control, students operate the computer during the run. As the peaks appear on the mass chromatogram, their mass spectra are obtained and the student decides which corresponds to product and evaluates product purity and the structure of impurities. There is ample time to display all spectra, conduct library searches, and print data. This relatively simple laboratory exercise has the advantage of allowing each student to carry out an analysis on his or her own product. The fact that a brominated product is obtained introduces a discussion of isotopic patterns in mass spectrometry. The experiment is scheduled to coincide with the lecture discussion of spectroscopic structure determination and after SN2 reactions have been covered. One of our mass spectrometer satellite data stations is interfaced with a "3-gun" projector in a large lecture hall allowing the display of actual mass spectra from our instrument to lecture sections. AcknowlegementThis work was partially supported by a grant, DUE9350846, from the National Science Foundation Division of Undergraduate Education Instrumentation and Laboratory Improvement Program. Literature Cited Brush, R. C.; Rice, G. W. J. Chem. Educ. 1994, 71, A293-A294. Asleson, G. L.; Doig, M. T.; Heldrich, F. J. J. Chem. Educ. 1993, 70, A290. Novak, M.; Heinrich, J. J. Chem. Educ. 1993, 70, A150. (b) Novak, M.; Heinrich, J.; Martin, K. A. J. Chem. Educ. 1993, 70, A103-104. Harman, C. S.; Myers, D. P.; Rittle, K. J. J. Chem. Educ. 1991, 68, 438-42. Mabbott, G. A. J. Chem. Educ. 1990, 67, 441-5. Hill, D. W.; McSharry, B. T.; Trzupek. J. Chem. Educ. 1988, 65, 907-10. Williamson, K. L. Macroscale and Microscale Organic Experiments, 2nd ed.; D. C. Heath: Lexington, MA, 1994; pp 247-51.

Mass and emission spectrometry in the Analytical Chemistry Division of Oak Ridge National Laboratory

Energy Technology Data Exchange (ETDEWEB)

Smith, D.H. (ed.)

1978-11-01

The capabilities of the Mass and Emission Spectrometry Section of the Analytical Chemistry Division of Oak Ridge National Laboratory are described. Many different areas of mass spectrometric expertise are represented in the section: gas analysis, high abundance sensitivity measurements, high- and low-resolution organic analyses, spark source trace constituent analysis, and ion microprobe analysis of surfaces. These capabilities are complemented by emission spectrometry. The instruments are described along with a few applications, some of which are unique.

Mass and emission spectrometry in the Analytical Chemistry Division of Oak Ridge National Laboratory

International Nuclear Information System (INIS)

Smith, D.H.

1978-11-01

The capabilities of the Mass and Emission Spectrometry Section of the Analytical Chemistry Division of Oak Ridge National Laboratory are described. Many different areas of mass spectrometric expertise are represented in the section: gas analysis, high abundance sensitivity measurements, high- and low-resolution organic analyses, spark source trace constituent analysis, and ion microprobe analysis of surfaces. These capabilities are complemented by emission spectrometry. The instruments are described along with a few applications, some of which are unique

Current use of high-resolution mass spectrometry in drug screening relevant to clinical and forensic toxicology and doping control.

Science.gov (United States)

Ojanperä, Ilkka; Kolmonen, Marjo; Pelander, Anna

2012-05-01

Clinical and forensic toxicology and doping control deal with hundreds or thousands of drugs that may cause poisoning or are abused, are illicit, or are prohibited in sports. Rapid and reliable screening for all these compounds of different chemical and pharmaceutical nature, preferably in a single analytical method, is a substantial effort for analytical toxicologists. Combined chromatography-mass spectrometry techniques with standardised reference libraries have been most commonly used for the purpose. In the last ten years, the focus has shifted from gas chromatography-mass spectrometry to liquid chromatography-mass spectrometry, because of progress in instrument technology and partly because of the polarity and low volatility of many new relevant substances. High-resolution mass spectrometry (HRMS), which enables accurate mass measurement at high resolving power, has recently evolved to the stage that is rapidly causing a shift from unit-resolution, quadrupole-dominated instrumentation. The main HRMS techniques today are time-of-flight mass spectrometry and Orbitrap Fourier-transform mass spectrometry. Both techniques enable a range of different drug-screening strategies that essentially rely on measuring a compound's or a fragment's mass with sufficiently high accuracy that its elemental composition can be determined directly. Accurate mass and isotopic pattern acts as a filter for confirming the identity of a compound or even identification of an unknown. High mass resolution is essential for improving confidence in accurate mass results in the analysis of complex biological samples. This review discusses recent applications of HRMS in analytical toxicology.

Preface Miniaturization and Mass Spectrometry

NARCIS (Netherlands)

Unknown, [Unknown; le Gac, Severine; le Gac, S.; van den Berg, Albert; van den Berg, A.

2009-01-01

Miniaturization and Mass Spectrometry illustrates this trend and focuses on one particular analysis technique, mass spectrometry whose popularity has "dramatically" increased in the last two decades with the explosion of the field of biological analysis and the development of two "soft" ionization

Characterization of the phosphoproteome and sialoproteome in brain tissues by mass spectrometry

DEFF Research Database (Denmark)

Ibáñez-Vea, María; Kempf, Stefan J.; Larsen, Martin R.

2017-01-01

Mass spectrometry is an essential tool for the characterization of proteins within neuroscience. The development of faster instruments enables neuroscientists to investigate a large proportion of the proteome in the brain in only short analysis time. Yet, a detailed functional investigation of th...

Advances in 193 nm excimer lasers for mass spectrometry applications

Science.gov (United States)

Delmdahl, Ralph; Esser, Hans-Gerd; Bonati, Guido

2016-03-01

Ongoing progress in mass analysis applications such as laser ablation inductively coupled mass spectrometry of solid samples and ultraviolet photoionization mediated sequencing of peptides and proteins is to a large extent driven by ultrashort wavelength excimer lasers at 193 nm. This paper will introduce the latest improvements achieved in the development of compact high repetition rate excimer lasers and elaborate on the impact on mass spectrometry instrumentation. Various performance and lifetime measurements obtained in a long-term endurance test over the course of 18 months will be shown and discussed in view of the laser source requirements of different mass spectrometry tasks. These sampling type applications are served by excimer lasers delivering pulsed 193 nm output of several mJ as well as fast repetition rates which are already approaching one Kilohertz. In order to open up the pathway from the laboratory to broader market industrial use, sufficient component lifetimes and long-term stable performance behavior have to be ensured. The obtained long-term results which will be presented are based on diverse 193 nm excimer laser tube improvements aiming at e.g. optimizing the gas flow dynamics and have extended the operational life the laser tube for the first time over several billion pulses even under high duty-cycle conditions.

Challenges ahead for mass spectrometry and proteomics applications in epigenetics.

Science.gov (United States)

Kessler, Benedikt M

2010-02-01

Inheritance of biological information to future generations depends on the replication of DNA and the Mendelian principle of distribution of genes. In addition, external and environmental factors can influence traits that can be propagated to offspring, but the molecular details of this are only beginning to be understood. The discoveries of DNA methylation and post-translational modifications on chromatin and histones provided entry points for regulating gene expression, an area now defined as epigenetics and epigenomics. Mass spectrometry turned out to be instrumental in uncovering molecular details involved in these processes. The central role of histone post-translational modifications in epigenetics related biological processes has revitalized mass spectrometry based investigations. In this special report, current approaches and future challenges that lay ahead due to the enormous complexity are discussed.

Radiocarbon mass spectrometry for drug development

International Nuclear Information System (INIS)

Ulrich, Schulze-Konig Tim

2011-01-01

Full text: Radiocarbon has a huge potential as a tracer for metabolism studies in humans. By using Accelerator Mass Spectrometry (AMS) for its detection, a unique sensitivity is reached reducing required radiation doses to a negligible level. Until recently, a widespread use of AMS in biomedical research was impeded by the high complexity of the instrument, time-consuming sample preparation, and a limited availability of measurement capacity. Over the last few years, tremendous progress has been achieved in the reduction of size and complexity of AMS instruments. It allowed designing a compact AMS system, dubbed BioMICADAS to address the needs of biomedical users. For more than two years, this system is in successful operation at a commercial service provider for the pharmaceutical industry. A further drastic simplification of radiocarbon mass spectrometers seems possible and could establish a regular usage of this technology in drug development. However, to reach this goal a better integration of AMS into the workflow of bioanalytical laboratories will be necessary. For this purpose, CO 2 accepting ion sources may be a key, since they enable an almost automated sample preparation. The status of radiocarbon AMS in biomedical research and its perspective will be discussed

Tandem Mass Spectrometry on a Miniaturized Laser Desorption Time-of-Flight Mass Spectrometer

Science.gov (United States)

Li, Xiang; Cornish, Timothy; Getty, Stephanie A.; Brinckerhoff, William B.

2016-01-01

Tandem mass spectrometry (MSMS) is a powerful and widely-used technique for identifying the molecular structure of organic constituents of a complex sample. Application of MSMS to the study of unknown planetary samples on a remote space mission would contribute to our understanding of the origin, evolution, and distribution of extraterrestrial organics in our solar system. Here we report on the realization of MSMS on a miniaturized laser desorption time-of-flight mass spectrometer (LD-TOF-MS), which is one of the most promising instrument types for future planetary missions. This achievement relies on two critical components: a curved-field reflectron and a pulsed-pin ion gate. These enable use of the complementary post-source decay (PSD) and laser-assisted collision induced dissociation (L-CID) MSMS methods on diverse measurement targets with only modest investment in instrument resources such as volume and weight. MSMS spectra of selected molecular targets in various organic standards exhibit excellent agreement when compared with results from a commercial, laboratory-scale TOF instrument, demonstrating the potential of this powerful technique in space and planetary environments.

Measuring Thermodynamic Properties of Metals and Alloys With Knudsen Effusion Mass Spectrometry

Science.gov (United States)

Copland, Evan H.; Jacobson, Nathan S.

2010-01-01

This report reviews Knudsen effusion mass spectrometry (KEMS) as it relates to thermodynamic measurements of metals and alloys. First, general aspects are reviewed, with emphasis on the Knudsen-cell vapor source and molecular beam formation, and mass spectrometry issues germane to this type of instrument are discussed briefly. The relationship between the vapor pressure inside the effusion cell and the measured ion intensity is the key to KEMS and is derived in detail. Then common methods used to determine thermodynamic quantities with KEMS are discussed. Enthalpies of vaporization, the fundamental measurement, are determined from the variation of relative partial pressure with temperature using the second-law method or by calculating a free energy of formation and subtracting the entropy contribution using the third-law method. For single-cell KEMS instruments, measurements can be used to determine the partial Gibbs free energy if the sensitivity factor remains constant over multiple experiments. The ion-current ratio method and dimer-monomer method are also viable in some systems. For a multiple-cell KEMS instrument, activities are obtained by direct comparison with a suitable component reference state or a secondary standard. Internal checks for correct instrument operation and general procedural guidelines also are discussed. Finally, general comments are made about future directions in measuring alloy thermodynamics with KEMS.

Symposium on accelerator mass spectrometry

Energy Technology Data Exchange (ETDEWEB)

None

1981-01-01

The area of accelerator mass spectrometry has expanded considerably over the past few years and established itself as an independent and interdisciplinary research field. Three years have passed since the first meeting was held at Rochester. A Symposium on Accelerator Mass Spectrometry was held at Argonne on May 11-13, 1981. In attendance were 96 scientists of whom 26 were from outside the United States. The present proceedings document the program and excitement of the field. Papers are arranged according to the original program. A few papers not presented at the meeting have been added to complete the information on the status of accelerator mass spectrometry. Individual papers were prepared separately for the data base.

Symposium on accelerator mass spectrometry

International Nuclear Information System (INIS)

1981-01-01

The area of accelerator mass spectrometry has expanded considerably over the past few years and established itself as an independent and interdisciplinary research field. Three years have passed since the first meeting was held at Rochester. A Symposium on Accelerator Mass Spectrometry was held at Argonne on May 11-13, 1981. In attendance were 96 scientists of whom 26 were from outside the United States. The present proceedings document the program and excitement of the field. Papers are arranged according to the original program. A few papers not presented at the meeting have been added to complete the information on the status of accelerator mass spectrometry. Individual papers were prepared separately for the data base

Theory and technique of spark source mass spectrometry; Theorie et technique de la spectrometrie de masse a etincelles

Energy Technology Data Exchange (ETDEWEB)

Stefani, R [Commissariat a l' Energie Atomique, Grenoble (France). Centre d' Etudes Nucleaires

1968-07-01

Trace analysis in solids by spark source mass spectrometry involves complicated phenomena: element ionization in spark and blacking of sensitive emulsion by focused ion beam. However the principal risk of selectivity lies in analyser system, which realizes double focusing only for a part of the ions. Therefore, each analyst has to known ionic optics of his apparatus, for ensuring the transmission of mean energetic ions, which are representative of sample composition. By a careful photometry of mass spectrum, good reproducibility can be obtained. Thereafter accuracy depends on the knowledge of sensitivity coefficients proper to this apparatus. (author) [French] L'analyse de traces dans les solides par spectrometrie de masse a etincelles met en jeu des phenomenes complexes qui sont l'ionisation des elements dans l'etincelle, et le noircissement de l'emulsion sensible par les faisceaux ioniques focalises. Cependant, le risque majeur de selectivite provient de l'ensemble analyseur, qui realise la double focalisation sur une fraction seulement du faisceau d'ions. L'analyste doit donc connaitre en detail l'optique ionique de son appareil, pour assurer le passage de la bande d'energie moyenne des ions, qui seule caracterise quantitativement la composition chimique de l'echantillon. Une exploitation photometrique soignee du spectrogramme donne alors des resultats reproductibles, dont la justesse ne depend plus que des coefficients de sensibilite propres a ce type d'instrument. (auteur)

Fourier Transform Mass Spectrometry.

Science.gov (United States)

Gross, Michael L.; Rempel, Don L.

1984-01-01

Discusses the nature of Fourier transform mass spectrometry and its unique combination of high mass resolution, high upper mass limit, and multichannel advantage. Examines its operation, capabilities and limitations, applications (ion storage, ion manipulation, ion chemistry), and future applications and developments. (JN)

Analysis of sulfates on low molecular weight heparin using mass spectrometry: structural characterization of enoxaparin.

Science.gov (United States)

Gupta, Rohitesh; Ponnusamy, Moorthy P

2018-05-21

Structural characterization of Low Molecular Weight Heparin (LMWH) is critical to meet biosimilarity standards. In this context, the review focuses on structural analysis of labile sulfates attached to the side-groups of LMWH using mass spectrometry. A comprehensive review of this topic will help readers to identify key strategies for tackling the problem related to sulfate loss. At the same time, various mass spectrometry techniques are presented to facilitate compositional analysis of LMWH, mainly Enoxaparin. Areas covered: This review summarizes findings on mass spectrometry application for LMWH, including modulation of sulfates, using enzymology and sample preparation approaches. Furthermore, popular open-source software packages for automated spectral data interpretation are also discussed. Successful use of LC/MS can decipher structural composition for LMWH and help evaluate their sameness or biosimilarity with the innovator molecule. Overall, the literature has been searched using PubMed by typing various search queries such as "enoxaparin", "mass spectrometry", "low molecular weight heparin", "structural characterization", etc. Expert commentary: This section highlights clinically relevant areas that need improvement to achieve satisfactory commercialization of LMWHs. It also primarily emphasizes the advancements in instrumentation related to mass spectrometry, and discusses building automated software for data interpretation and analysis.

Role of Mass Spectrometry in Clinical Endocrinology.

Science.gov (United States)

Ketha, Siva S; Singh, Ravinder J; Ketha, Hemamalini

2017-09-01

The advent of mass spectrometry into the clinical laboratory has led to an improvement in clinical management of several endocrine diseases. Liquid chromatography tandem mass spectrometry found some of its first clinical applications in the diagnosis of inborn errors of metabolism, in quantitative steroid analysis, and in drug analysis laboratories. Mass spectrometry assays offer analytical sensitivity and specificity that is superior to immunoassays for many analytes. This article highlights several areas of clinical endocrinology that have witnessed the use of liquid chromatography tandem mass spectrometry to improve clinical outcomes. Copyright © 2017 Elsevier Inc. All rights reserved.

Mass spectrometry

DEFF Research Database (Denmark)

Nyvang Hartmeyer, Gitte; Jensen, Anne Kvistholm; Böcher, Sidsel

2010-01-01

Matrix-assisted laser desorption ionization time-of-flight mass spectrometry (MALDI-TOF MS) is currently being introduced for the rapid and accurate identification of bacteria. We describe 2 MALDI-TOF MS identification cases - 1 directly on spinal fluid and 1 on grown bacteria. Rapidly obtained...

Protein Analysis by Mass Spectrometry

Directory of Open Access Journals (Sweden)

Cindic, M.

2008-04-01

Full Text Available Soft ionization techniques, electrospray (ESI and matrix-assisted laser desorption/ionization (MALDI make the analysis of biomolecules by mass spectrometry (MS possible. MS is used for determination of the molecular weight of peptides and protein, sequence analysis, characterization of protein-ligand interactions etc. The detection limit, resolution and mass accuracy depend on instrument used (Table 1. Impurities (buffers, salts, detergents can reduce the ion intensities or even totally suppress them, so a separation method (chromatography, 2D-gel electrophoresis must be used for purification of the sample.Molecular mass of intact protein can be determined by ESI or MALDI MS. Multiply charged ions are produced by ESI MS, while singly charged ions are predominant in MALDI spectra (Fig. 2.Sequence analysis of proteins by MS can be performed using peptide mass fingerprint. In this method, proteins are separated by 2-D gel electrophoresis and digested with specific protease (Table 2 or digested and then separated by two-dimensional chromatography (Fig. 1. The obtained peptide mixtures are analyzed by MS or MALDI-TOF technique. The masses determined by MS are compared with calculated masses from database entries. Different algorithms have been developed for protein identification. Example of posttranslational modifications (N- and O-glycosylation and protein sequence complex analysis after dual digestion (endoproteinase digestion followed by endoglycosidase digestion is shown in Fig. 3.It is known that detection of peptides by MS is influenced by intrinsic properties like amino acid composition, the basicity of the C-terminal amino acid, hydrophobicity, etc. Arginine-containing peptides dominate in MS spectra of tryptic digest, so the chemical derivatization of lysine terminal residue by O-methilisourea or 2-methoxy-4,5-1H-imidazole was suggested (Fig. 4.The peptide mass fingerprint method can be improved further by peptide fragmentation using tandem

qcML : an exchange format for quality control metrics from mass spectrometry experiments

NARCIS (Netherlands)

Walzer, Mathias; Pernas, Lucia Espona; Nasso, Sara; Bittremieux, Wout; Nahnsen, Sven; Kelchtermans, Pieter; Pichler, Peter; van den Toorn, Henk W P|info:eu-repo/dai/nl/31093205X; Staes, An; Vandenbussche, Jonathan; Mazanek, Michael; Taus, Thomas; Scheltema, Richard A; Kelstrup, Christian D; Gatto, Laurent; van Breukelen, Bas|info:eu-repo/dai/nl/244219087; Aiche, Stephan; Valkenborg, Dirk; Laukens, Kris; Lilley, Kathryn S; Olsen, Jesper V; Heck, Albert J R|info:eu-repo/dai/nl/105189332; Mechtler, Karl; Aebersold, Ruedi; Gevaert, Kris; Vizcaíno, Juan Antonio; Hermjakob, Henning; Kohlbacher, Oliver; Martens, Lennart

Quality control is increasingly recognized as a crucial aspect of mass spectrometry based proteomics. Several recent papers discuss relevant parameters for quality control and present applications to extract these from the instrumental raw data. What has been missing, however, is a standard data

Mass spectrometry with accelerators.

Science.gov (United States)

Litherland, A E; Zhao, X-L; Kieser, W E

2011-01-01

As one in a series of articles on Canadian contributions to mass spectrometry, this review begins with an outline of the history of accelerator mass spectrometry (AMS), noting roles played by researchers at three Canadian AMS laboratories. After a description of the unique features of AMS, three examples, (14)C, (10)Be, and (129)I are given to illustrate the methods. The capabilities of mass spectrometry have been extended by the addition of atomic isobar selection, molecular isobar attenuation, further ion acceleration, followed by ion detection and ion identification at essentially zero dark current or ion flux. This has been accomplished by exploiting the techniques and accelerators of atomic and nuclear physics. In 1939, the first principles of AMS were established using a cyclotron. In 1977 the selection of isobars in the ion source was established when it was shown that the (14)N(-) ion was very unstable, or extremely difficult to create, making a tandem electrostatic accelerator highly suitable for assisting the mass spectrometric measurement of the rare long-lived radioactive isotope (14)C in the environment. This observation, together with the large attenuation of the molecular isobars (13)CH(-) and (12)CH 2(-) during tandem acceleration and the observed very low background contamination from the ion source, was found to facilitate the mass spectrometry of (14)C to at least a level of (14)C/C ~ 6 × 10(-16), the equivalent of a radiocarbon age of 60,000 years. Tandem Accelerator Mass Spectrometry, or AMS, has now made possible the accurate radiocarbon dating of milligram-sized carbon samples by ion counting as well as dating and tracing with many other long-lived radioactive isotopes such as (10)Be, (26)Al, (36)Cl, and (129)I. The difficulty of obtaining large anion currents with low electron affinities and the difficulties of isobar separation, especially for the heavier mass ions, has prompted the use of molecular anions and the search for alternative

Recent advances of liquid chromatography-(tandem) mass spectrometry in clinical and forensic toxicology.

Science.gov (United States)

Peters, Frank T

2011-01-01

Liquid chromatography (LC) coupled to mass spectrometry (MS) or tandem mass spectrometry (MS/MS) has become increasingly important in clinical and forensic toxicology as well as doping control and is now a robust and reliable technique for routine analysis in these fields. In recent years, methods for LC-MS(/MS)-based systematic toxicological analysis using triple quadrupole or ion trap instruments have been considerably improved and a new screening approach based on high-resolution MS analysis using benchtop time-of-flight MS instruments has been developed. Moreover, many applications for so-called multi-target screening and/or quantification of drugs, poisons, and or their metabolites in various biomatrices have been published. The present paper will provide an overview and discuss these recent developments focusing on the literature published after 2006. Copyright © 2010 The Canadian Society of Clinical Chemists. Published by Elsevier Inc. All rights reserved.

Chromatography–mass spectrometry in aerospace industry

International Nuclear Information System (INIS)

Buryak, Alexey K; Serduk, T M

2013-01-01

The applications of chromatography–mass spectrometry in aerospace industry are considered. The primary attention is devoted to the development of physicochemical grounds of the use of various chromatography–mass spectrometry procedures to solve topical problems of this industry. Various methods for investigation of the composition of rocket fuels, surfaces of structural materials and environmental media affected by aerospace activities are compared. The application of chromatography–mass spectrometry for the development and evaluation of processes for decontaminations of equipment, industrial wastes and soils from rocket fuel components is substantiated. The bibliography includes 135 references.

Negative chemical ionization mass spectrometry

International Nuclear Information System (INIS)

Smit, A.L.C.

1979-01-01

This thesis describes some aspects of Negative Chemical Ionization (NCI) mass spectrometry. The reasons for the growing interest in NCI are: (i) to extend the basic knowledge of negative ions and their reactions in the gas phase; (ii) to investigate whether or not this knowledge of negative ions can be used successfully to elucidate the structure of molecules by mass spectrometry. (Auth.)

Investigating quantitation of phosphorylation using MALDI-TOF mass spectrometry.

Science.gov (United States)

Parker, Laurie; Engel-Hall, Aaron; Drew, Kevin; Steinhardt, George; Helseth, Donald L; Jabon, David; McMurry, Timothy; Angulo, David S; Kron, Stephen J

2008-04-01

Despite advances in methods and instrumentation for analysis of phosphopeptides using mass spectrometry, it is still difficult to quantify the extent of phosphorylation of a substrate because of physiochemical differences between unphosphorylated and phosphorylated peptides. Here we report experiments to investigate those differences using MALDI-TOF mass spectrometry for a set of synthetic peptides by creating calibration curves of known input ratios of peptides/phosphopeptides and analyzing their resulting signal intensity ratios. These calibration curves reveal subtleties in sequence-dependent differences for relative desorption/ionization efficiencies that cannot be seen from single-point calibrations. We found that the behaviors were reproducible with a variability of 5-10% for observed phosphopeptide signal. Although these data allow us to begin addressing the issues related to modeling these properties and predicting relative signal strengths for other peptide sequences, it is clear that this behavior is highly complex and needs to be further explored. John Wiley & Sons, Ltd

Mass spectrometry-assisted protease substrate screening

DEFF Research Database (Denmark)

Schlüter, Hartmut; Rykl, Jana; Thiemann, Joachim

2007-01-01

-phase chromatography they are analyzed by tandem mass spectrometry and the substrates identified by database searching. The proof of principle in this study is demonstrated by incubating immobilized human plasma proteins with thrombin and by identifying by tandem mass spectrometry the fibrinopeptides, released...

Thermal ionisation mass spectrometry (TIMS): what, how and why?

International Nuclear Information System (INIS)

Aggarwal, S.K.

2002-01-01

Thermal ionisation mass spectrometry (TIMS) is one of the oldest mass spectrometric techniques, which has been used for determining the isotopic composition and concentration of different elements using isotope dilution. In spite of the introduction of many other inorganic mass spectrometric techniques like spark source mass spectrometry (SSMS), glow discharge mass spectrometry (GDMS), inductively coupled plasma-mass spectrometry (ICP-MS), secondary ion mass spectrometry (SIMS), the TIMS technique plays the role of a definitive analytical methodology and still occupies a unique position in terms of its capabilities with respect to precision and accuracy as well as sensitivity

Surface analysis by imaging mass spectrometry

Czech Academy of Sciences Publication Activity Database

Vidová, Veronika; Volný, Michael; Lemr, Karel; Havlíček, Vladimír

2009-01-01

Roč. 74, 7-8 (2009), s. 1101-1116 ISSN 0010-0765 Institutional research plan: CEZ:AV0Z50200510 Keywords : secondary ion mass spectrometry * matrix assisted laser desorption ionization * mass spectrometry Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 0.856, year: 2009

Introduction to mass spectrometry-based proteomics

DEFF Research Database (Denmark)

Matthiesen, R.; Bunkenborg, J.

2013-01-01

Mass spectrometry has been widely applied to study biomolecules and one rapidly developing field is the global analysis of proteins, proteomics. Understanding and handling mass spectrometry data is a multifaceted task that requires many decisions to be made to get the most comprehensive informati...

Burnup determination of mass spectrometry for nuclear fuels

International Nuclear Information System (INIS)

Zhang Chunhua.

1987-01-01

The various methods currently being used in burnup determination of nuclear fuels are studied and reviewed. The mass spectrometry method of destructive testing is discussed emphatically. The burnup determination of mass spectrometry includes heavy isotopic abundance ratio method and isotope dilution mass spectrometry used as burnup indicator for the fission products. The former is applied to high burnup level, but the later to various burnup level. According to experiences, some problems which should be noticed in burnup determination of mass spectrometry are presented

Silver nanostructures in laser desorption/ionization mass spectrometry and mass spectrometry imaging.

Science.gov (United States)

Sekuła, Justyna; Nizioł, Joanna; Rode, Wojciech; Ruman, Tomasz

2015-09-21

Silver nanoparticles have been successfully applied as a matrix replacement for the laser desorption/ionization time-of-flight mass spectrometry (LDI-ToF-MS). Nanoparticles, producing spectra with highly reduced chemical background in the low m/z region, are perfectly suited for low-molecular weight compound analysis and imaging. Silver nanoparticles (AgNPs) can efficiently absorb ultraviolet laser radiation, transfer energy to the analyte and promote analyte desorption, but also constitute a source of silver ions suitable for analyte cationisation. This review provides an overview of the literature on silver nanomaterials as non-conventional desorption and ionization promoters in LDI-MS and mass spectrometry imaging.

U/Th dating by SHRIMP RG ion-microprobe mass spectrometry using single ion-exchange beads

Science.gov (United States)

Bischoff, J.L.; Wooden, J.; Murphy, F.; Williams, Ross W.

2005-01-01

We present a new analytical method for U-series isotopes using the SHRIMP RG (Sensitive High mass Resolution Ion MicroProbe) mass spectrometer that utilizes the preconcentration of the U-series isotopes from a sample onto a single ion-exchange bead. Ion-microprobe mass spectrometry is capable of producing Th ionization efficiencies in excess of 2%. Analytical precision is typically better than alpha spectroscopy, but not as good as thermal ionization mass spectroscopy (TIMS) and inductively coupled plasma multicollector mass spectrometry (ICP-MS). Like TIMS and ICP-MS the method allows analysis of small samples sizes, but also adds the advantage of rapidity of analysis. A major advantage of ion-microprobe analysis is that U and Th isotopes are analyzed in the same bead, simplifying the process of chemical separation. Analytical time on the instrument is ???60 min per sample, and a single instrument-loading can accommodate 15-20 samples to be analyzed in a 24-h day. An additional advantage is that the method allows multiple reanalyses of the same bead and that samples can be archived for reanalysis at a later time. Because the ion beam excavates a pit only a few ??m deep, the mount can later be repolished and reanalyzed numerous times. The method described of preconcentrating a low concentration sample onto a small conductive substrate to allow ion-microprobe mass spectrometry is potentially applicable to many other systems. Copyright ?? 2005 Elsevier Ltd.

Laser Time-of-Flight Mass Spectrometry for Future In Situ Planetary Missions

Science.gov (United States)

Getty, S. A.; Brinckerhoff, W. B.; Cornish, T.; Ecelberger, S. A.; Li, X.; Floyd, M. A. Merrill; Chanover, N.; Uckert, K.; Voelz, D.; Xiao, X.;

The optimization of some of the conditions for analysis by spark-source mass spectrometry

International Nuclear Information System (INIS)

Pearton, D.C.P.; Sobiecki, A.

1980-01-01

The need for improved precision in spark-source mass spectrometry is highlighted. Several parameters, such as photoplate-development technique, instrumental stability and focus, and sparking conditions, were optimized. Measurements made under these optimum conditions attained precisions of more than 12 per cent

Imaging mass spectrometry in drug development and toxicology.

Science.gov (United States)

Karlsson, Oskar; Hanrieder, Jörg

2017-06-01

During the last decades, imaging mass spectrometry has gained significant relevance in biomedical research. Recent advances in imaging mass spectrometry have paved the way for in situ studies on drug development, metabolism and toxicology. In contrast to whole-body autoradiography that images the localization of radiolabeled compounds, imaging mass spectrometry provides the possibility to simultaneously determine the discrete tissue distribution of the parent compound and its metabolites. In addition, imaging mass spectrometry features high molecular specificity and allows comprehensive, multiplexed detection and localization of hundreds of proteins, peptides and lipids directly in tissues. Toxicologists traditionally screen for adverse findings by histopathological examination. However, studies of the molecular and cellular processes underpinning toxicological and pathologic findings induced by candidate drugs or toxins are important to reach a mechanistic understanding and an effective risk assessment strategy. One of IMS strengths is the ability to directly overlay the molecular information from the mass spectrometric analysis with the tissue section and allow correlative comparisons of molecular and histologic information. Imaging mass spectrometry could therefore be a powerful tool for omics profiling of pharmacological/toxicological effects of drug candidates and toxicants in discrete tissue regions. The aim of the present review is to provide an overview of imaging mass spectrometry, with particular focus on MALDI imaging mass spectrometry, and its use in drug development and toxicology in general.

Alpha spectrometry and secondary ion mass spectrometry of thorium

International Nuclear Information System (INIS)

Strisovska, Jana; Kuruc, Jozef; Galanda, Dusan; Matel, Lubomir; Velic, Dusan; Aranyosiova, Monika

2009-01-01

A sample of thorium content on steel discs was prepared by electrodeposition with a view to determining the natural thorium isotope. Thorium was determined by alpha spectrometry and by secondary ion mass spectrometry and the results of the two methods were compared

High-sensitivity mass spectrometry with a tandem accelerator

International Nuclear Information System (INIS)

Henning, W.

1984-01-01

The characteristic features of accelerator mass spectrometry are discussed. A short overview is given of the current status of mass spectrometry with high-energy (MeV/nucleon) heavy-ion accelerators. Emphasis is placed on studies with tandem accelerators and on future mass spectrometry of heavier isotopes with the new generation of higher-voltage tandems

Inorganic mass spectrometry of solid samples

International Nuclear Information System (INIS)

Adams, F.; Vertes, A.

1990-01-01

In this review some recent developments in the field of inorganic mass spectrometry of solids are described with special emphasis on the actual state of understanding of the ionization processes. It concentrates on the common characteristics of methods such as spark source-, laser-, secondary ion-, inductively coupled plasma- and glow discharge mass spectrometry. (orig.)

Chromatography and mass spectrometry of chemical warfare agents, toxins and related compounds: state of the art and future prospects

NARCIS (Netherlands)

Kientz, C.E.

1998-01-01

Methods for the identification of chemical warfare agents, toxins, bioregulators and related products are frequently reported in literature. These methods are often based on instrumental analysis using chromatography (gas and liquid) and mass spectrometry. Here, these instrumental techniques are

Electrospray ionization tandem mass spectrometry of ammonium cationized polyethers.

Science.gov (United States)

Nasioudis, Andreas; Heeren, Ron M A; van Doormalen, Irene; de Wijs-Rot, Nicolette; van den Brink, Oscar F

2011-05-01

Quaternary ammonium salts (Quats) and amines are known to facilitate the MS analysis of high molar mass polyethers by forming low charge state adduct ions. The formation, stability, and behavior upon collision-induced dissociation (CID) of adduct ions of polyethers with a variety of Quats and amines were studied by electrospray ionization quadrupole time-of-flight, quadrupole ion trap, and linear ion trap tandem mass spectrometry (MS/MS). The linear ion trap instrument was part of an Orbitrap hybrid mass spectrometer that allowed accurate mass MS/MS measurements. The Quats and amines studied were of different degree of substitution, structure, and size. The stability of the adduct ions was related to the structure of the cation, especially the amine's degree of substitution. CID of singly/doubly charged primary and tertiary ammonium cationized polymers resulted in the neutral loss of the amine followed by fragmentation of the protonated product ions. The latter reveals information about the monomer unit, polymer sequence, and endgroup structure. In addition, the detection of product ions retaining the ammonium ion was observed. The predominant process in the CID of singly charged quaternary ammonium cationized polymers was cation detachment, whereas their doubly charged adduct ions provided the same information as the primary and tertiary ammonium cationized adduct ions. This study shows the potential of specific amines as tools for the structural elucidation of high molar mass polyethers. © American Society for Mass Spectrometry, 2011

Characterization of polyesters by matrix-assisted laser desorption/ionization and Fourier transform mass spectrometry.

Science.gov (United States)

Mize, Todd H; Simonsick, William J; Amster, I Jonathan

2003-01-01

Two homopolyesters, poly(neopentyl glycol-alt-isophthalic acid) and poly(hexanediol-alt-azelaic acid), and two copolyesters, poly(dipropoxylated bisphenol-A-alt-(isophthalic acid-co-adipic acid)) and poly(neopentyl glycol-alt-(adipic acid-co-isophthalic acid)) were analyzed by internal source matrix assisted laser desorption/ionization Fourier transform mass spectrometry (MALDI-FTMS). The high resolution and high mass accuracy provided by FTMS greatly facilitate the characterization of the polyester and copolyester samples. Isobaric resolution allows the ion abundances of overlapping isotopic envelopes to be assessed. Repeat units were confirmed and end functionality assigned. Single shot mass spectra of the entire polymeric distribution demonstrate that the dynamic range of this internal MALDI source instrument and the analyzer cell exceeds performance of those previously reported for higher field instruments. Corrections of space charge mass shift effects are demonstrated for the analytes using an external calibrant and (subsequent to confirmation of structure) via internal calibration which removes ambiguity due to space charge differences in calibrant and analyte spectra. Capillary gel permeation chromatography was used to prepare low polydispersity samples from a high polydispersity polyester, improving the measurement of molecular weight distribution two-fold while retaining the benefits of high resolution mass spectrometry for elucidation of oligomer identity.

Matrix-assisted laser desorption fourier transform mass spectrometry for biological compounds

Energy Technology Data Exchange (ETDEWEB)

Hettich, R.; Buchanan, M.

1990-01-01

The recent development of matrix-assisted UV laser desorption (LD) mass spectrometry has made possible the ionization and detection of extremely large molecules (with molecular weights exceeding 100,000 Daltons). This technique has generated enormous interest in the biological community for the direct examination of large peptides and oligonucleotides. Although this matrix-assisted ionization method has been developed and used almost exclusively with time-of-flight (TOF) mass spectrometers, research is currently in progress to demonstrate this technique with trapped ion mass spectrometers, such as Fourier transform ion cyclotron resonance mass spectrometry (FTMS). The potential capabilities of FTMS for wide mass range, high resolution measurement, and ion trapping experiments suggest that this instrumental technique should be useful for the detailed structural characterization of large ions generated by the matrix-assisted technique. We have recently demonstrated that matrix-assisted ultraviolet laser desorption can be successfully used with FTMS for the ionization of small peptides. The objective of this report is to summarize the application and current limitations of matrix-assisted laser desorption FTMS for the characterization of peptides and oligonucleotides at the isomeric level. 4 refs., 3 figs., 2 tabs.

Accelerator mass spectrometry-enabled studies: current status and future prospects.

Science.gov (United States)

Arjomand, Ali

2010-03-01

Accelerator mass spectrometry is a detection platform with exceptional sensitivity compared with other bioanalytical platforms. Accelerator mass spectrometry (AMS) is widely used in archeology for radiocarbon dating applications. Early exploration of the biological and pharmaceutical applications of AMS began in the early 1990s. AMS has since demonstrated unique problem-solving ability in nutrition science, toxicology and pharmacology. AMS has also enabled the development of new applications, such as Phase 0 microdosing. Recent development of AMS-enabled applications has transformed this novelty research instrument to a valuable tool within the pharmaceutical industry. Although there is now greater awareness of AMS technology, recognition and appreciation of the range of AMS-enabled applications is still lacking, including study-design strategies. This review aims to provide further insight into the wide range of AMS-enabled applications. Examples of studies conducted over the past two decades will be presented, as well as prospects for the future of AMS.

Accelerator mass spectrometry of Strontium-90 for homeland security, environmental monitoring, and human health

Energy Technology Data Exchange (ETDEWEB)

Tumey, S J; Brown, T A; Hamilton, T F; Hillegonds, D J

2008-03-03

Strontium-90 is one of the most hazardous materials managed by agencies charged with protecting the public from radiation. Traditional radiometric methods have been limited by low sample throughput and slow turnaround times. Mass spectrometry offers the advantage of shorter analysis times and the ability to measure samples immediately after processing, however conventional mass spectrometric techniques are susceptible to molecular isobaric interferences that limit their overall sensitivity. In contrast, accelerator mass spectrometry is insensitive to molecular interferences and we have therefore begun developing a method for determination of {sup 90}Sr by accelerator mass spectrometry. Despite a pervasive interference from {sup 90}Zr, our initial development has yielded an instrumental background of {approx} 10{sup 8} atoms (75 mBq) per sample. Further refinement of our system (e.g., redesign of our detector, use of alternative target materials) is expected to push the background below 10{sup 6} atoms, close to the theoretical limit for AMS. Once we have refined our system and developed suitable sample preparation protocols, we will utilize our capability in applications to homeland security, environmental monitoring, and human health.

Mass spectrometry in nuclear science and technology

International Nuclear Information System (INIS)

Komori, Takuji

1985-01-01

Mass spectrometry has been widely used and playing a very important role in the field of nuclear science and technology. A major reason for this is that not only the types of element but also its isotopes have to be identified and measured in this field. Thus, some applications of this analytical method are reviewed and discussed in this article. Its application to analytical chemistry is described in the second section following an introductory section, which includes subsections for isotropic dilution mass spectrometry, resonance ionization mass spectrometry and isotopic correlation technique. The isotopic ratio measurement for hydrogen, uranium and plutonium as well as nuclear material control and safeguards are also reviewed in this section. In the third section, mass spectrometry is discussed in relation to nuclear reactors, with subsections on natural uranium reactor and neutron flux observation. Some techniques for measuring the burnup fraction, including the heavy isotopic ratio method and fission product monitoring, are also described. In the fourth section, application of mass spectrometry to measurement of nuclear constants, such as ratio of effective cross-sectional area for 235 U, half-life and fission yield is reviewed. (Nogami, K.)

Transition of Iodine Analysis to Accelerator Mass Spectrometry

International Nuclear Information System (INIS)

Watrous, Matthew George; Adamic, Mary Louise; Olson, John Eric; Baeck, D. L.; Fox, R. V.; Hahn, P. A.; Jenson, D. D.; Lister, T. E.

2015-01-01

The goal of the project, New Paradigms for Isotope Ratio Mass Spectrometry: Raising the Scientific Profile and Improved Performance for Accelerator Mass Spectrometry (AMS) and Thermal Ionization Mass Spectrometry (TIMS), is to ensure that the ongoing isotope ratio determination capability within the U.S. Department of Energy complex is the world's best for application to nonproliferation. This report spells out the progress of Task 4, Transition of TIMS to AMS for Iodine Analysis, of the larger project. The subtasks under Task 4 and the accomplishments throughout the three year project life cycle are presented in this report. Progress was made in optimization of chemical extraction, determination of a detection limit for 127Iodine, production of standard materials for AMS analysis quality assurance, facilitation of knowledge exchange with respect to analyzing iodine on an AMS, cross comparison with a world-leading AMS laboratory, supercritical fluid extraction of iodine for AMS analysis and electrodeposition of seawater as a direct method of preparation for iodine analysis by AMS--all with the goal of minimizing the time required to stand up an AMS capability for iodine analysis of exposed air filters at INL. An effective extraction method has been developed and demonstrated for iodine analysis of exposed air filters. Innovative techniques to accomplish the cathode preparation for AMS analysis were developed and demonstrated and published. The known gap of a lack of available materials for reference standards in the analysis of iodine by AMS was filled by the preparation of homogenous materials that were calibrated against NIST materials. A minimum limit on the amount of abundant isotope in a sample was determined for AMS analysis. The knowledge exchange occurred with fantastic success. Scientists engaged the international AMS community at conferences, as well as in their laboratories for collaborative work. The supercritical fluid extraction work has positive

Transition of Iodine Analysis to Accelerator Mass Spectrometry

Energy Technology Data Exchange (ETDEWEB)

Watrous, Matthew George [Idaho National Lab. (INL), Idaho Falls, ID (United States); Adamic, Mary Louise [Idaho National Lab. (INL), Idaho Falls, ID (United States); Olson, John Eric [Idaho National Lab. (INL), Idaho Falls, ID (United States); Baeck, D. L. [Idaho National Lab. (INL), Idaho Falls, ID (United States); Fox, R. V. [Idaho National Lab. (INL), Idaho Falls, ID (United States); Hahn, P. A. [Idaho National Lab. (INL), Idaho Falls, ID (United States); Jenson, D. D. [Idaho National Lab. (INL), Idaho Falls, ID (United States); Lister, T. E. [Idaho National Lab. (INL), Idaho Falls, ID (United States)

2015-09-01

The goal of the project, New Paradigms for Isotope Ratio Mass Spectrometry: Raising the Scientific Profile and Improved Performance for Accelerator Mass Spectrometry (AMS) and Thermal Ionization Mass Spectrometry (TIMS), is to ensure that the ongoing isotope ratio determination capability within the U.S. Department of Energy complex is the world’s best for application to nonproliferation. This report spells out the progress of Task 4, Transition of TIMS to AMS for Iodine Analysis, of the larger project. The subtasks under Task 4 and the accomplishments throughout the three year project life cycle are presented in this report. Progress was made in optimization of chemical extraction, determination of a detection limit for 127Iodine, production of standard materials for AMS analysis quality assurance, facilitation of knowledge exchange with respect to analyzing iodine on an AMS, cross comparison with a world-leading AMS laboratory, supercritical fluid extraction of iodine for AMS analysis and electrodeposition of seawater as a direct method of preparation for iodine analysis by AMS--all with the goal of minimizing the time required to stand up an AMS capability for iodine analysis of exposed air filters at INL. An effective extraction method has been developed and demonstrated for iodine analysis of exposed air filters. Innovative techniques to accomplish the cathode preparation for AMS analysis were developed and demonstrated and published. The known gap of a lack of available materials for reference standards in the analysis of iodine by AMS was filled by the preparation of homogenous materials that were calibrated against NIST materials. A minimum limit on the amount of abundant isotope in a sample was determined for AMS analysis. The knowledge exchange occurred with fantastic success. Scientists engaged the international AMS community at conferences, as well as in their laboratories for collaborative work. The supercritical fluid extraction work has positive

Resonant laser mass spectrometry for environmental and industrial chemical trace analysis

International Nuclear Information System (INIS)

Boesl, Ulrich; Rink, Joerg; Distelrath, Volker; Pueffel, Peter

2001-01-01

A promising new method for pollutant trace analysis is resonant laser mass spectrometry. It combines selectivity, sensitivity, and speed of measurement. In this paper, two examples of application are presented: exhaust analysis of combustion engines and analysis of polycylcic aromatic compounds in soil samples. The sensitivity of small, mobile instruments is discussed as well as alternative laser-based techniques in the case formation of cations by nanosecond lasers is improbable

Examining the Heterogeneous Genome Content of Multipartite Viruses BMV and CCMV by Native Mass Spectrometry

NARCIS (Netherlands)

van de Waterbeemd, Michiel; Snijder, Joost; Tsvetkova, Irina B.; Dragnea, Bogdan G.; Cornelissen, Jeroen J.; Heck, Albert J.R.

2016-01-01

Since the concept was first introduced by Brian Chait and co-workers in 1991, mass spectrometry of proteins and protein complexes under non-denaturing conditions (native MS) has strongly developed, through parallel advances in instrumentation, sample preparation, and data analysis tools. However,

Comparison of inductively coupled plasma mass spectrometry with inductively coupled plasma atomic emission spectrometry and instrumental neutron activation analysis for the determination of rare earth elements in Greek bauxites

International Nuclear Information System (INIS)

Ochsenkuehn-Petropoulou, Maria; Luck, Joachim

1991-01-01

Fore the determination of rare earth elements (REE) in bauxitic materials the techniques of inductively coupled plasma mass spectrometry (ICP-MS), inductively coupled plasma atomic emission spectrometry (ICP-AES) and instrumental neutron activation analysis (INAA) were compared. In the NIST (National Institute of Standards and Technology) bauxites SRM 697 Dominican, and SRM 69 b Arkansas, the concentration of some REEs were determined. With the reference bauxite BX-N of the ARNT (Association Nationale de la Recherche Technique) the precision and accuracy of ICP-AES for the determination of REEs in bauxites was tested. Furthermore, Greek bauxites of the Parnassos-Giona area were investigated. In a comparison of the three methods it was possible to calculate from the data series the precision of each method, which showed that the tendency found in the deviations for the different REEs is in accordance with published values. Also the limits of detection for REEs in bauxites were calculated and found to be in the same range as those in the literature. (author)

Mass Spectrometry Analyses of Multicellular Tumor Spheroids.

Science.gov (United States)

Acland, Mitchell; Mittal, Parul; Lokman, Noor A; Klingler-Hoffmann, Manuela; Oehler, Martin K; Hoffmann, Peter

2018-05-01

Multicellular tumor spheroids (MCTS) are a powerful biological in vitro model, which closely mimics the 3D structure of primary avascularized tumors. Mass spectrometry (MS) has established itself as a powerful analytical tool, not only to better understand and describe the complex structure of MCTS, but also to monitor their response to cancer therapeutics. The first part of this review focuses on traditional mass spectrometry approaches with an emphasis on elucidating the molecular characteristics of these structures. Then the mass spectrometry imaging (MSI) approaches used to obtain spatially defined information from MCTS is described. Finally the analysis of primary spheroids, such as those present in ovarian cancer, and the great potential that mass spectrometry analysis of these structures has for improved understanding of cancer progression and for personalized in vitro therapeutic testing is discussed. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

The emergence of mass spectrometry in biochemical research

OpenAIRE

1995-01-01

The initial steps toward routinely applying mass spectrometry in the biochemical laboratory have been achieved. In the past, mass spectrometry was confined to the realm of small, relatively stable molecules; large or thermally labile molecules did not survive the desorption and ionization processes intact. Electrospray ionization (ESI) and matrix-assisted laser desorption/ionization (MALDI) mass spectrometry allow for the analysis of both small and large biomolecules through "mild" desorption...

Zero voltage mass spectrometry probes and systems

Science.gov (United States)

Cooks, Robert Graham; Wleklinski, Michael Stanley; Bag, Soumabha; Li, Yafeng

2017-10-10

The invention generally relates to zero volt mass spectrometry probes and systems. In certain embodiments, the invention provides a system including a mass spectrometry probe including a porous material, and a mass spectrometer (bench-top or miniature mass spectrometer). The system operates without an application of voltage to the probe. In certain embodiments, the probe is oriented such that a distal end faces an inlet of the mass spectrometer. In other embodiments, the distal end of the probe is 5 mm or less from an inlet of the mass spectrometer.

Automated mass correction and data interpretation for protein open-access liquid chromatography-mass spectrometry.

Science.gov (United States)

Wagner, Craig D; Hall, John T; White, Wendy L; Miller, Luke A D; Williams, Jon D

2007-02-01

Characterization of recombinant protein purification fractions and final products by liquid chromatography-mass spectrometry (LC/MS) are requested more frequently each year. A protein open-access (OA) LC/MS system was developed in our laboratory to meet this demand. This paper compares the system that we originally implemented in our facilities in 2003 to the one now in use, and discusses, in more detail, recent enhancements that have improved its robustness, reliability, and data reporting capabilities. The system utilizes instruments equipped with reversed-phase chromatography and an orthogonal accelerated time-of-flight mass spectrometer fitted with an electrospray source. Sample analysis requests are accomplished using a simple form on a web-enabled laboratory information management system (LIMS). This distributed form is accessible from any intranet-connected company desktop computer. Automated data acquisition and processing are performed using a combination of in-house (OA-Self Service, OA-Monitor, and OA-Analysis Engine) and vendor-supplied programs (AutoLynx, and OpenLynx) located on acquisition computers and off-line processing workstations. Analysis results are then reported via the same web-based LIMS. Also presented are solutions to problems not addressed on commercially available, small-molecule OA-LC/MS systems. These include automated transforming of mass-to-charge (m/z) spectra to mass spectra and automated data interpretation that considers minor variants to the protein sequence-such as common post-translational modifications (PTMs). Currently, our protein OA-LC/MS platform runs on five LC/MS instruments located in three separate GlaxoSmithKline R&D sites in the US and UK. To date, more than 8000 protein OA-LC/MS samples have been analyzed. With these user friendly and highly automated OA systems in place, mass spectrometry plays a key role in assessing the quality of recombinant proteins, either produced at our facilities or bought from external

Mass spectrometry for biomarker development

Energy Technology Data Exchange (ETDEWEB)

Wu, Chaochao; Liu, Tao; Baker, Erin Shammel; Rodland, Karin D.; Smith, Richard D.

2015-06-19

Biomarkers potentially play a crucial role in early disease diagnosis, prognosis and targeted therapy. In the past decade, mass spectrometry based proteomics has become increasingly important in biomarker development due to large advances in technology and associated methods. This chapter mainly focuses on the application of broad (e.g. shotgun) proteomics in biomarker discovery and the utility of targeted proteomics in biomarker verification and validation. A range of mass spectrometry methodologies are discussed emphasizing their efficacy in the different stages in biomarker development, with a particular emphasis on blood biomarker development.

The Effect of Collimating Lens Focusing on Laser Beam Shape in Matrix Assisted Laser Desorption/Ionization Mass Spectrometry (MALDI-MS).

Science.gov (United States)

O'Rourke, Matthew B; Raymond, Benjamin B A; Djordjevic, Steven P; Padula, Matthew P

2018-03-01

Tissue imaging using matrix assisted laser desorption/ionization mass spectrometry (MALDI-MS) is a well-established technique that, in recent years, has seen wider adoption and novel application. Applications such imaging mass spectrometry (IMS) and biotyping are beginning to gain greater exposure and use; however, with limitations in optimization methods, producing the best result often relies on the ability to customize the physical characteristics of the instrumentation, a task that is challenging for most mass spectrometry laboratories. With this in mind, we have described the effect of making simple adjustments to the laser optics at the final collimating lens area, to adjust the laser beam size and shape in order to allow greater customization of the instrument for improving techniques such as IMS. We have therefore been able to demonstrate that improvements can be made without requiring the help of an electrical engineer or external funding in a way that only costs a small amount of time. Graphical Abstract ᅟ.

Instrumental analysis

Energy Technology Data Exchange (ETDEWEB)

Kim, Seung Jae; Seo, Seong Gyu

1995-03-15

This textbook deals with instrumental analysis, which consists of nine chapters. It has Introduction of analysis chemistry, the process of analysis and types and form of the analysis, Electrochemistry on basic theory, potentiometry and conductometry, electromagnetic radiant rays and optical components on introduction and application, Ultraviolet rays and Visible spectrophotometry, Atomic absorption spectrophotometry on introduction, flame emission spectrometry and plasma emission spectrometry. The others like infrared spectrophotometry, X-rays spectrophotometry and mass spectrometry, chromatography and the other instrumental analysis like radiochemistry.

Instrumental analysis

International Nuclear Information System (INIS)

Kim, Seung Jae; Seo, Seong Gyu

1995-03-01

This textbook deals with instrumental analysis, which consists of nine chapters. It has Introduction of analysis chemistry, the process of analysis and types and form of the analysis, Electrochemistry on basic theory, potentiometry and conductometry, electromagnetic radiant rays and optical components on introduction and application, Ultraviolet rays and Visible spectrophotometry, Atomic absorption spectrophotometry on introduction, flame emission spectrometry and plasma emission spectrometry. The others like infrared spectrophotometry, X-rays spectrophotometry and mass spectrometry, chromatography and the other instrumental analysis like radiochemistry.

Characterisation of the volatile profiles of infant formulas by proton transfer reaction-mass spectrometry and gas chromatography-mass spectrometry

NARCIS (Netherlands)

Ruth, van S.M.; Floris, V.; Fayoux, S.

2006-01-01

The volatile profiles of 13 infant formulas were evaluated by proton transfer reaction-mass spectrometry (PTR-MS) and gas chromatography¿mass spectrometry (GC¿MS). The infant formulas varied in brand (Aptamil, Cow & Gate, SMA), type (for different infant target groups) and physical form

Emerging mass spectrometry techniques for the direct analysis of microbial colonies

OpenAIRE

Fang, Jinshu; Dorrestein, Pieter C.

2014-01-01

One of the emerging areas in microbiology is detecting specialized metabolites produced by microbial colonies and communities with mass spectrometry. In this review/perspective, we illustrate the emerging mass spectrometry methodologies that enable the interrogation of specialized metabolites directly from microbial colonies. Mass spectrometry techniques such as imaging mass spectrometry and real-time mass spectrometry allow two and three dimensional visualization of the distri...

Mass spectrometry in oceanography

International Nuclear Information System (INIS)

Aggarwal, Suresh K.

2000-01-01

Mass spectrometry plays an important role in oceanography for various applications. Different types of inorganic as well as organic mass spectrometric techniques are being exploited world-wide to understand the different aspects of marine science, for palaeogeography, palaeoclimatology and palaeoecology, for isotopic composition and concentrations of different elements as well as for speciation studies. The present paper reviews some of the applications of atomic mass spectrometric techniques in the area of oceanography

Characterizing the lipid and metabolite changes associated with placental function and pregnancy complications using ion mobility spectrometry-mass spectrometry and mass spectrometry imaging

Energy Technology Data Exchange (ETDEWEB)

Burnum-Johnson, Kristin E.; Baker, Erin S.; Metz, Thomas O.

2017-12-01

Successful pregnancy is dependent upon discrete biological events, which include embryo implantation, decidualization, and placentation. Problems associated with each of these events can cause infertility or conditions such as preeclampsia. A greater understanding of the molecular changes associated with these complex processes is necessary to aid in identifying treatments for each condition. Previous nuclear magnetic resonance spectroscopy and mass spectrometry studies have been used to identify metabolites and lipids associated with pregnancy-related complications. However, due to limitations associated with conventional implementations of both techniques, novel technology developments are needed to more fully understand the initiation and development of pregnancy related problems at the molecular level. In this perspective, we describe current analytical techniques for metabolomic and lipidomic characterization of pregnancy complications and discuss the potential for new technologies such as ion mobility spectrometry-mass spectrometry and mass spectrometry imaging to contribute to a better understanding of the molecular changes that affect the placenta and pregnancy outcomes.

Electron-capture negative-ion mass spectrometry: a technique for environmental contaminant identification

International Nuclear Information System (INIS)

Stemmler, E.A.

1986-01-01

Electron capture negative ion mass spectrometry (ECNIMS) is a method used to generate negative ions in a mass spectrometer by electron-molecule reactions. This technique facilitates the sensitive and selective detection of many toxic contaminants in environmental samples. Applications of this technique have been hindered by the limited understanding of instrumental parameters, by the questionable reproducibility of negative ion mass spectra, and by the inability to interpret negative ion mass spectra. Instrumental parameters which were important to control include the ion source temperature, ion source pressure, sample concentration, and the focus lens potential. The ability to obtain reproducible spectra was demonstrated by measurement of the spectrum of decafluorotriphenylphosphine (DFTPP) over a period of one year. Negative ion fragmentation mechanisms were studied by measuring the spectra of structurally related classes of compounds and isotopically labelled compounds. These results were combined with data obtained by other researchers. Fragmentations characteristic of particular functional groups or molecular structures have been summarized. From this data set, guidelines for the interpretation of electron capture negative ion mass spectra have been developed

Recent development in isotope ratio mass spectrometry

International Nuclear Information System (INIS)

Platzner, I.

1992-01-01

Within the limited of this review the following topics will be briefly discussed: a) Accuracy, precision, internal relative standard deviation (RISD) and external relative standard deviation (RESD) of isotope ratio measurements. With advanced instrumentation and use of standard reference materials, high accuracy and RESD = 0.002% (or better) may be achieved; b) The advantages of modern automatic isotope ratio mass spectrometer are briefly described. Computer controlled operation and data acquisition, and multiple ion collection are the recent important improvement; c) The isotopic fractionation during the course of isotope ratio measurement is considered as a major source of errors in thermal ionization of metallic elements. The phenomenon in strontium, neodymium, uranium, lead and calcium and methods to correct the measured data are discussed; d) Applications of isotope ratio mass spectrometry in atomic weight determinations, the isotope dilution technique, isotope geology, and isotope effects in biological systems are described together with specific applications in various research and technology area. (author)

Resonance ionization mass spectrometry using tunable diode lasers

International Nuclear Information System (INIS)

Shaw, R.W.; Young, J.P.; Smith, D.H.

1990-01-01

Tunable semiconductor diode lasers will find many important applications in atomic spectroscopy. They exhibit the desirable attributes of lasers: narrow bandwidth, tunability, and spatial coherence. At the same time, they possess few of the disadvantages of other tunable lasers. They require no alignment, are simple to operate, and are inexpensive. Practical laser spectroscopic instruments can be envisioned. The authors have applied diode lasers to resonance ionization mass spectrometry (RIMS) of some of the lanthanide elements. Sub-Doppler resolution spectra have been recorded and have been used for atomic hyperfine structure analysis. Isotopically-selective ionization has been accomplished, even in cases where photons from a broadband dye laser are part of the overall ionization process and where the isotopic spectral shift is very small. A convenient RIMS instrument for isotope ratio measurements that employs only diode lasers, along with electric field ionization, should be possible

Mass spectrometry in life science research.

Science.gov (United States)

Lehr, Stefan; Markgraf, Daniel

2016-12-01

Investigating complex signatures of biomolecules by mass spectrometry approaches has become indispensable in molecular life science research. Nowadays, various mass spectrometry-based omics technologies are available to monitor qualitative and quantitative changes within hundreds or thousands of biological active components, including proteins/peptides, lipids and metabolites. These comprehensive investigations have the potential to decipher the pathophysiology of disease development at a molecular level and to monitor the individual response of pharmacological treatment or lifestyle intervention.

Phylogenetic Analysis Using Protein Mass Spectrometry.

Science.gov (United States)

Ma, Shiyong; Downard, Kevin M; Wong, Jason W H

2017-01-01

Through advances in molecular biology, comparative analysis of DNA sequences is currently the cornerstone in the study of molecular evolution and phylogenetics. Nevertheless, protein mass spectrometry offers some unique opportunities to enable phylogenetic analyses in organisms where DNA may be difficult or costly to obtain. To date, the methods of phylogenetic analysis using protein mass spectrometry can be classified into three categories: (1) de novo protein sequencing followed by classical phylogenetic reconstruction, (2) direct phylogenetic reconstruction using proteolytic peptide mass maps, and (3) mapping of mass spectral data onto classical phylogenetic trees. In this chapter, we provide a brief description of the three methods and the protocol for each method along with relevant tools and algorithms.

[Imaging Mass Spectrometry in Histopathologic Analysis].

Science.gov (United States)

Yamazaki, Fumiyoshi; Seto, Mitsutoshi

2015-04-01

Matrix-assisted laser desorption/ionization (MALDI)-imaging mass spectrometry (IMS) enables visualization of the distribution of a range of biomolecules by integrating biochemical information from mass spectrometry with positional information from microscopy. IMS identifies a target molecule. In addition, IMS enables global analysis of biomolecules containing unknown molecules by detecting the ratio of the molecular weight to electric charge without any target, which makes it possible to identify novel molecules. IMS generates data on the distribution of lipids and small molecules in tissues, which is difficult to visualize with either conventional counter-staining or immunohistochemistry. In this review, we firstly introduce the principle of imaging mass spectrometry and recent advances in the sample preparation method. Secondly, we present findings regarding biological samples, especially pathological ones. Finally, we discuss the limitations and problems of the IMS technique and clinical application, such as in drug development.

Cs+ ion source for secondary ion mass spectrometry

International Nuclear Information System (INIS)

Bentz, B.L.; Weiss, H.; Liebl, H.

1981-12-01

Various types of cesium ionization sources currently used in secondary ion mass spectrometry are briefly reviewed, followed by a description of the design and performance of a novel, thermal surface ionization Cs + source developed in this laboratory. The source was evaluated for secondary ion mass spectrometry applications using the COALA ion microprobe mass analyzer. (orig.)

A new processing scheme for ultra-high resolution direct infusion mass spectrometry data

Science.gov (United States)

Zielinski, Arthur T.; Kourtchev, Ivan; Bortolini, Claudio; Fuller, Stephen J.; Giorio, Chiara; Popoola, Olalekan A. M.; Bogialli, Sara; Tapparo, Andrea; Jones, Roderic L.; Kalberer, Markus

2018-04-01

High resolution, high accuracy mass spectrometry is widely used to characterise environmental or biological samples with highly complex composition enabling the identification of chemical composition of often unknown compounds. Despite instrumental advancements, the accurate molecular assignment of compounds acquired in high resolution mass spectra remains time consuming and requires automated algorithms, especially for samples covering a wide mass range and large numbers of compounds. A new processing scheme is introduced implementing filtering methods based on element assignment, instrumental error, and blank subtraction. Optional post-processing incorporates common ion selection across replicate measurements and shoulder ion removal. The scheme allows both positive and negative direct infusion electrospray ionisation (ESI) and atmospheric pressure photoionisation (APPI) acquisition with the same programs. An example application to atmospheric organic aerosol samples using an Orbitrap mass spectrometer is reported for both ionisation techniques resulting in final spectra with 0.8% and 8.4% of the peaks retained from the raw spectra for APPI positive and ESI negative acquisition, respectively.

Analysis of Nitro-aromatic and Nitramine Explosives by Atmospheric Pressure Chemical Ionization / High Performance Liquid Chromatography / Mass Spectrometry / Mass Spectrometry

International Nuclear Information System (INIS)

Hicks, B.J.; Han, W.; Robben, J.R.

2009-01-01

This procedure is capable of separating and quantifying twenty-nine high explosives and internal surrogates with a single injection. After the initial preparation step, the sample is introduced to the high performance liquid chromatograph for target separation, ionized by atmospheric pressure chemical ionization and the explosives of interest are isolated / quantified by mass spectrometry / mass spectrometry. Concentrations of the target explosives are measured relative to the response of both internal and external standard concentrations. A C-18 reverse phase high performance liquid chromatograph column is used for separation. Ionization is performed using both positive and negative atmospheric pressure chemical ionization resulting in a molecular ion with little fragmentation. These ions are isolated at the first quadrupole of the mass spectrometer, dissociated by collision with argon in the collision cell and the resulting daughter ions are isolated at the second quadrupole. These daughter ions then reach the detector where they are quantified. To date this procedure represents the most thorough high performance liquid chromatography / mass spectrometry / mass spectrometry explosives analysis available in the environmental chemistry market. (authors)

[Latest development in mass spectrometry for clinical application].

Science.gov (United States)

Takino, Masahiko

2013-09-01

Liquid chromatography-tandem mass spectrometry (LC-MS/MS) has seen enormous growth in special clinical chemistry laboratories. It significantly increases the analytic potential in clinical chemistry, especially in the field of low molecular weight biomarker analysis. This review summarizes the state of the art in mass spectrometry and related techniques for clinical application with a main focus on recent developments in LC-MS. Current trends in ionization techniques, automated online sample preparation techniques coupled with LC-MS, and ion mobility spectrometry are discussed. Emerging mass spectrometric approaches complementary to LC-MS are discussed as well.

Mass spectrometry: a revolution in clinical microbiology?

Science.gov (United States)

Lavigne, Jean-Philippe; Espinal, Paula; Dunyach-Remy, Catherine; Messad, Nourredine; Pantel, Alix; Sotto, Albert

2013-02-01

Recently, different bacteriological laboratory interventions that decrease reporting time have been developed. These promising new broad-based techniques have merit, based on their ability to identify rapidly many bacteria, organisms difficult to grow or newly emerging strains, as well as their capacity to track disease transmission. The benefit of rapid reporting of identification and/or resistance of bacteria can greatly impact patient outcomes, with an improvement in the use of antibiotics, in the reduction of the emergence of multidrug resistant bacteria and in mortality rates. Different techniques revolve around mass spectrometry (MS) technology: matrix-assisted laser desorption ionization time-of-flight mass spectrometry (MALDI-TOF MS), PCR combined with electrospray ionization-mass spectrometry (PCR/ESIMS), iPLEX MassArray system and other new evolutions combining different techniques. This report emphasizes the (r)evolution of these technologies in clinical microbiology.

NICHD Biomedical Mass Spectrometry Core Facility

Data.gov (United States)

Federal Laboratory Consortium — The NICHD Biomedical Mass Spectrometry Core Facility was created under the auspices of the Office of the Scientific Director to provide high-end mass-spectrometric...

Mass spectrometry for real-time quantitative breath analysis

Czech Academy of Sciences Publication Activity Database

Smith, D.; Španěl, Patrik; Herbig, J.; Beauchamp, J.

2014-01-01

Roč. 8, č. 2 (2014), 027101 ISSN 1752-7155 Institutional support: RVO:61388955 Keywords : breath analysis * proton transfer reaction mass spectrometry * selected ion flow tube mass spectrometry Subject RIV: CF - Physical ; Theoretical Chemistry Impact factor: 4.631, year: 2014

High-efficiency thermal ionization sources for mass spectrometry

International Nuclear Information System (INIS)

Olivares, Jose A.

1996-01-01

A version of the thermal ionization cavity (TIC) source developed specifically for use in mass spectrometry is presented. The performance of this ion source has been characterized extensively both with the use of an isotope separator and a quadrupole mass spectrometer. A detailed description of the TIC source for mass spectrometry is given along with the performance characteristics observed

Examining the Heterogeneous Genome Content of Multipartite Viruses BMV and CCMV by Native Mass Spectrometry

Science.gov (United States)

van de Waterbeemd, Michiel; Snijder, Joost; Tsvetkova, Irina B.; Dragnea, Bogdan G.; Cornelissen, Jeroen J.; Heck, Albert J. R.

2016-06-01

Since the concept was first introduced by Brian Chait and co-workers in 1991, mass spectrometry of proteins and protein complexes under non-denaturing conditions (native MS) has strongly developed, through parallel advances in instrumentation, sample preparation, and data analysis tools. However, the success rate of native MS analysis, particularly in heterogeneous mega-Dalton (MDa) protein complexes, still strongly depends on careful instrument modification. Here, we further explore these boundaries in native mass spectrometry, analyzing two related endogenous multipartite viruses: the Brome Mosaic Virus (BMV) and the Cowpea Chlorotic Mottle Virus (CCMV). Both CCMV and BMV are approximately 4.6 megadalton (MDa) in mass, of which approximately 1 MDA originates from the genomic content of the virion. Both viruses are produced as mixtures of three particles carrying different segments of the genome, varying by approximately 0.1 MDA in mass (~2%). This mixture of particles poses a challenging analytical problem for high-resolution native MS analysis, given the large mass scales involved. We attempt to unravel the particle heterogeneity using both Q-TOF and Orbitrap mass spectrometers extensively modified for analysis of very large assemblies. We show that manipulation of the charging behavior can provide assistance in assigning the correct charge states. Despite their challenging size and heterogeneity, we obtained native mass spectra with resolved series of charge states for both BMV and CCMV, demonstrating that native MS of endogenous multipartite virions is feasible.

Quantitation of Poly(ADP-Ribose) by Isotope Dilution Mass Spectrometry

DEFF Research Database (Denmark)

Zubel, Tabea; Martello, Rita; Bürkle, Alexander

2017-01-01

PARP inhibitors, which represent a novel class of promising chemotherapeutics. Previously, we have developed a bioanalytical platform based on isotope dilution mass spectrometry (LC-MS/MS) to quantify cellular PAR with unequivocal chemical specificity in absolute terms with femtomol sensitivity...... research, as well as in drug development (Martello et al. ACS Chem Biol 8(7):1567-1575, 2013; Mangerich et al. Toxicol Lett 244:56-71, 2016). Here, we present an improved and adjusted version of the original protocol by Martello/Mangerich et al., which uses UPLC-MS/MS instrumentation....

Analytical mass spectrometry

Energy Technology Data Exchange (ETDEWEB)

1990-01-01

This 43rd Annual Summer Symposium on Analytical Chemistry was held July 24--27, 1990 at Oak Ridge, TN and contained sessions on the following topics: Fundamentals of Analytical Mass Spectrometry (MS), MS in the National Laboratories, Lasers and Fourier Transform Methods, Future of MS, New Ionization and LC/MS Methods, and an extra session. (WET)

Statistical methods for mass spectrometry-based clinical proteomics

NARCIS (Netherlands)

Kakourou, A.

2018-01-01

The work presented in this thesis focuses on methods for the construction of diagnostic rules based on clinical mass spectrometry proteomic data. Mass spectrometry has become one of the key technologies for jointly measuring the expression of thousands of proteins in biological samples.

Sampling and analyte enrichment strategies for ambient mass spectrometry.

Science.gov (United States)

Li, Xianjiang; Ma, Wen; Li, Hongmei; Ai, Wanpeng; Bai, Yu; Liu, Huwei

2018-01-01

Ambient mass spectrometry provides great convenience for fast screening, and has showed promising potential in analytical chemistry. However, its relatively low sensitivity seriously restricts its practical utility in trace compound analysis. In this review, we summarize the sampling and analyte enrichment strategies coupled with nine modes of representative ambient mass spectrometry (desorption electrospray ionization, paper vhspray ionization, wooden-tip spray ionization, probe electrospray ionization, coated blade spray ionization, direct analysis in real time, desorption corona beam ionization, dielectric barrier discharge ionization, and atmospheric-pressure solids analysis probe) that have dramatically increased the detection sensitivity. We believe that these advances will promote routine use of ambient mass spectrometry. Graphical abstract Scheme of sampling stretagies for ambient mass spectrometry.

Fourier transform ion cyclotron resonance mass spectrometry

Science.gov (United States)

Marshall, Alan G.

1998-06-01

As for Fourier transform infrared (FT-IR) interferometry and nuclear magnetic resonance (NMR) spectroscopy, the introduction of pulsed Fourier transform techniques revolutionized ion cyclotron resonance mass spectrometry: increased speed (factor of 10,000), increased sensitivity (factor of 100), increased mass resolution (factor of 10,000-an improvement not shared by the introduction of FT techniques to IR or NMR spectroscopy), increased mass range (factor of 500), and automated operation. FT-ICR mass spectrometry is the most versatile technique for unscrambling and quantifying ion-molecule reaction kinetics and equilibria in the absence of solvent (i.e., the gas phase). In addition, FT-ICR MS has the following analytically important features: speed (~1 second per spectrum); ultrahigh mass resolution and ultrahigh mass accuracy for analysis of mixtures and polymers; attomole sensitivity; MSn with one spectrometer, including two-dimensional FT/FT-ICR/MS; positive and/or negative ions; multiple ion sources (especially MALDI and electrospray); biomolecular molecular weight and sequencing; LC/MS; and single-molecule detection up to 108 Dalton. Here, some basic features and recent developments of FT-ICR mass spectrometry are reviewed, with applications ranging from crude oil to molecular biology.

Ion Mobility Mass Spectrometry Direct Isotope Abundance Analysis

International Nuclear Information System (INIS)

Manard, Manuel J.; Weeks, Stephan; Kyle, Kevin

2010-01-01

The nuclear forensics community is currently engaged in the analysis of illicit nuclear or radioactive material for the purposes of non-proliferations and attribution. One technique commonly employed for gathering nuclear forensics information is isotope analysis. At present, the state-of-the-art methodology for obtaining isotopic distributions is thermal ionization mass spectrometry (TIMS). Although TIMS is highly accurate at determining isotope distributions, the technique requires an elementally pure sample to perform the measurement. The required radiochemical separations give rise to sample preparation times that can be in excess of one to two weeks. Clearly, the nuclear forensics community is in need of instrumentation and methods that can expedite their decision making process in the event of a radiological release or nuclear detonation. Accordingly, we are developing instrumentation that couples a high resolution IM drift cell to the front end of a MS. The IM cell provides a means of separating ions based upon their collision cross-section and mass-to-charge ratio (m/z). Two analytes with the same m/z, but with different collision cross-sections (shapes) would exit the cell at different times, essentially enabling the cell to function in a similar manner to a gas chromatography (GC) column. Thus, molecular and atomic isobaric interferences can be effectively removed from the ion beam. The mobility selected chemical species could then be introduced to a MS for high-resolution mass analysis to generate isotopic distributions of the target analytes. The outcome would be an IM/MS system capable of accurately measuring isotopic distributions while concurrently eliminating isobaric interferences and laboratory radiochemical sample preparation. The overall objective of this project is developing instrumentation and methods to produce near real-time isotope distributions with a modular mass spectrometric system that performs the required gas-phase chemistry and

Mass Spectrometry Imaging, an Emerging Technology in Neuropsychopharmacology

Science.gov (United States)

Shariatgorji, Mohammadreza; Svenningsson, Per; Andrén, Per E

2014-01-01

Mass spectrometry imaging is a powerful tool for directly determining the distribution of proteins, peptides, lipids, neurotransmitters, metabolites and drugs in neural tissue sections in situ. Molecule-specific imaging can be achieved using various ionization techniques that are suited to different applications but which all yield data with high mass accuracies and spatial resolutions. The ability to simultaneously obtain images showing the distributions of chemical species ranging from metal ions to macromolecules makes it possible to explore the chemical organization of a sample and to correlate the results obtained with specific anatomical features. The imaging of biomolecules has provided new insights into multiple neurological diseases, including Parkinson's and Alzheimer's disease. Mass spectrometry imaging can also be used in conjunction with other imaging techniques in order to identify correlations between changes in the distribution of important chemical species and other changes in the properties of the tissue. Here we review the applications of mass spectrometry imaging in neuroscience research and discuss its potential. The results presented demonstrate that mass spectrometry imaging is a useful experimental method with diverse applications in neuroscience. PMID:23966069

Mass spectrometry imaging, an emerging technology in neuropsychopharmacology.

Science.gov (United States)

Shariatgorji, Mohammadreza; Svenningsson, Per; Andrén, Per E

2014-01-01

Mass spectrometry imaging is a powerful tool for directly determining the distribution of proteins, peptides, lipids, neurotransmitters, metabolites and drugs in neural tissue sections in situ. Molecule-specific imaging can be achieved using various ionization techniques that are suited to different applications but which all yield data with high mass accuracies and spatial resolutions. The ability to simultaneously obtain images showing the distributions of chemical species ranging from metal ions to macromolecules makes it possible to explore the chemical organization of a sample and to correlate the results obtained with specific anatomical features. The imaging of biomolecules has provided new insights into multiple neurological diseases, including Parkinson's and Alzheimer's disease. Mass spectrometry imaging can also be used in conjunction with other imaging techniques in order to identify correlations between changes in the distribution of important chemical species and other changes in the properties of the tissue. Here we review the applications of mass spectrometry imaging in neuroscience research and discuss its potential. The results presented demonstrate that mass spectrometry imaging is a useful experimental method with diverse applications in neuroscience.

Atom counting with accelerator mass spectrometry

International Nuclear Information System (INIS)

Kutschera, Walter

1995-01-01

A brief review of the current status and some recent applications of accelerator mass spectrometry (AMS) are presented. Some connections to resonance ionization mass spectroscopy (RIS) as the alternate atom counting method are discussed

Guideline on Isotope Dilution Mass Spectrometry

Energy Technology Data Exchange (ETDEWEB)

Gaffney, Amy [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States)

2017-05-19

Isotope dilution mass spectrometry is used to determine the concentration of an element of interest in a bulk sample. It is a destructive analysis technique that is applicable to a wide range of analytes and bulk sample types. With this method, a known amount of a rare isotope, or ‘spike’, of the element of interest is added to a known amount of sample. The element of interest is chemically purified from the bulk sample, the isotope ratio of the spiked sample is measured by mass spectrometry, and the concentration of the element of interest is calculated from this result. This method is widely used, although a mass spectrometer required for this analysis may be fairly expensive.

Statistical analysis of proteomics, metabolomics, and lipidomics data using mass spectrometry

CERN Document Server

Mertens, Bart

2017-01-01

This book presents an overview of computational and statistical design and analysis of mass spectrometry-based proteomics, metabolomics, and lipidomics data. This contributed volume provides an introduction to the special aspects of statistical design and analysis with mass spectrometry data for the new omic sciences. The text discusses common aspects of design and analysis between and across all (or most) forms of mass spectrometry, while also providing special examples of application with the most common forms of mass spectrometry. Also covered are applications of computational mass spectrometry not only in clinical study but also in the interpretation of omics data in plant biology studies. Omics research fields are expected to revolutionize biomolecular research by the ability to simultaneously profile many compounds within either patient blood, urine, tissue, or other biological samples. Mass spectrometry is one of the key analytical techniques used in these new omic sciences. Liquid chromatography mass ...

Mass spectrometry for characterizing plant cell wall polysaccharides

Directory of Open Access Journals (Sweden)

Stefan eBauer

2012-03-01

Full Text Available Mass spectrometry is a selective and powerful technique to obtain identification and structural information on compounds present in complex mixtures. Since it requires only small sample amount it is an excellent tool for researchers interested in detecting changes in composition of complex carbohydrates of plants. This mini-review gives an overview of common mass spectrometry techniques applied to the analysis of plant cell wall carbohydrates. It presents examples in which mass spectrometry has been used to elucidate the structure of oligosaccharides derived from hemicelluloses and pectins and illustrates how information on sequence, linkages, branching and modifications are obtained from characteristic fragmentation patterns.

Proteomic Mass Spectrometry Imaging for Skin Cancer Diagnosis.

Science.gov (United States)

Lazova, Rossitza; Seeley, Erin H

2017-10-01

Mass spectrometry imaging can be successfully used for skin cancer diagnosis, particularly for the diagnosis of challenging melanocytic lesions. This method analyzes proteins within benign and malignant melanocytic tumor cells and, based on their differences, which constitute a unique molecular signature of 5 to 20 proteins, can render a diagnosis of benign nevus versus malignant melanoma. Mass spectrometry imaging may assist in the differentiation between metastases and nevi as well as between proliferative nodules in nevi and melanoma arising in a nevus. In the difficult area of atypical Spitzoid neoplasms, mass spectrometry diagnosis can predict clinical outcome better than histopathology. Copyright © 2017 Elsevier Inc. All rights reserved.

Mass Spectrometry in the Home and Garden

Science.gov (United States)

Pulliam, Christopher J.; Bain, Ryan M.; Wiley, Joshua S.; Ouyang, Zheng; Cooks, R. Graham

2015-02-01

Identification of active components in a variety of chemical products used directly by consumers is described at both trace and bulk levels using mass spectrometry. The combination of external ambient ionization with a portable mass spectrometer capable of tandem mass spectrometry provides high chemical specificity and sensitivity as well as allowing on-site monitoring. These experiments were done using a custom-built portable ion trap mass spectrometer in combination with the ambient ionization methods of paper spray, leaf spray, and low temperature plasma ionization. Bactericides, garden chemicals, air fresheners, and other products were examined. Herbicide applied to suburban lawns was detected in situ on single leaves 5 d after application.

Quantitative Thin-Layer Chromatography/Mass Spectrometry Analysis of Caffeine Using a Surface Sampling Probe Electrospray Ionization Tandem Mass Spectrometry System

Energy Technology Data Exchange (ETDEWEB)

Ford, Michael J [ORNL; Deibel, Michael A. [Earlham College; Tomkins, Bruce A [ORNL; Van Berkel, Gary J [ORNL

2005-01-01

Quantitative determination of caffeine on reversed-phase C8 thin-layer chromatography plates using a surface sampling electrospray ionization system with tandem mass spectrometry detection is reported. The thin-layer chromatography/electrospray tandem mass spectrometry method employed a deuterium-labeled caffeine internal standard and selected reaction monitoring detection. Up to nine parallel caffeine bands on a single plate were sampled in a single surface scanning experiment requiring 35 min at a surface scan rate of 44 {mu}m/s. A reversed-phase HPLC/UV caffeine assay was developed in parallel to assess the mass spectrometry method performance. Limits of detection for the HPLC/UV and thin-layer chromatography/electrospray tandem mass spectrometry methods determined from the calibration curve statistics were 0.20 ng injected (0.50 {mu}L) and 1.0 ng spotted on the plate, respectively. Spike recoveries with standards and real samples ranged between 97 and 106% for both methods. The caffeine content of three diet soft drinks (Diet Coke, Diet Cherry Coke, Diet Pepsi) and three diet sport drinks (Diet Turbo Tea, Speed Stack Grape, Speed Stack Fruit Punch) was measured. The HPLC/UV and mass spectrometry determinations were in general agreement, and these values were consistent with the quoted values for two of the three diet colas. In the case of Diet Cherry Coke and the diet sports drinks, the determined caffeine amounts using both methods were consistently higher (by 8% or more) than the literature values.

Quantification of steroid hormones in human serum by liquid chromatography-high resolution tandem mass spectrometry.

Science.gov (United States)

Matysik, Silke; Liebisch, Gerhard

2017-12-01

A limited specificity is inherent to immunoassays for steroid hormone analysis. To improve selectivity mass spectrometric analysis of steroid hormones by liquid chromatography-tandem mass spectrometry (LC-MS/MS) has been introduced in the clinical laboratory over the past years usually with low mass resolution triple-quadrupole instruments or more recently by high resolution mass spectrometry (HR-MS). Here we introduce liquid chromatography-high resolution tandem mass spectrometry (LC-MS/HR-MS) to further increase selectivity of steroid hormone quantification. Application of HR-MS demonstrates an enhanced selectivity compared to low mass resolution. Separation of isobaric interferences reduces background noise and avoids overestimation. Samples were prepared by automated liquid-liquid extraction with MTBE. The LC-MS/HR-MS method using a quadrupole-Orbitrap analyzer includes eight steroid hormones i.e. androstenedione, corticosterone, cortisol, cortisone, 11-deoxycortisol, 17-hydroxyprogesterone, progesterone, and testosterone. It has a run-time of 5.3min and was validated according to the U.S. Food and Drug Administration (FDA) and the European Medicines Agency (EMA) guidelines. For most of the analytes coefficient of variation were 10% or lower and LOQs were determined significantly below 1ng/ml. Full product ion spectra including accurate masses substantiate compound identification by matching their masses and ratios with authentic standards. In summary, quantification of steroid hormones by LC-MS/HR-MS is applicable for clinical diagnostics and holds also promise for highly selective quantification of other small molecules. Copyright © 2017 Elsevier B.V. All rights reserved.

High-accuracy mass spectrometry for fundamental studies.

Science.gov (United States)

Kluge, H-Jürgen

2010-01-01

Mass spectrometry for fundamental studies in metrology and atomic, nuclear and particle physics requires extreme sensitivity and efficiency as well as ultimate resolving power and accuracy. An overview will be given on the global status of high-accuracy mass spectrometry for fundamental physics and metrology. Three quite different examples of modern mass spectrometric experiments in physics are presented: (i) the retardation spectrometer KATRIN at the Forschungszentrum Karlsruhe, employing electrostatic filtering in combination with magnetic-adiabatic collimation-the biggest mass spectrometer for determining the smallest mass, i.e. the mass of the electron anti-neutrino, (ii) the Experimental Cooler-Storage Ring at GSI-a mass spectrometer of medium size, relative to other accelerators, for determining medium-heavy masses and (iii) the Penning trap facility, SHIPTRAP, at GSI-the smallest mass spectrometer for determining the heaviest masses, those of super-heavy elements. Finally, a short view into the future will address the GSI project HITRAP at GSI for fundamental studies with highly-charged ions.

Proceedings of the twelfth ISMAS triennial international conference on mass spectrometry

International Nuclear Information System (INIS)

Aggarwal, S.K.; Jaison, P.G.; Telmore, V.M.

2013-03-01

These Workshops are aimed at introducing the subject of Mass Spectrometry to novices, updating the Mass Spectrometrists with the latest developments in the field, exposing the participants to innumerable applications of Mass Spectrometry and providing a common forum for discussing the day-to-day problems when working with a Mass Spectrometer. The programme of these Workshops consists of Tutorials, Panel Discussions, Research Scholars' Presentations, Poster Presentations and Invited Lectures. The lectures include fundamentals of Mass Spectrometry, qualitative and quantitative aspects and data interpretation, maintenance of Mass Spectrometers, selection of a mass spectrometer, applications in various branches of science as well as recent advances in Mass Spectrometry. Papers relevant to INIS are indexed separately

Mass spectrometry of hyper-velocity impacts of organic micrograins.

Science.gov (United States)

Srama, Ralf; Woiwode, Wolfgang; Postberg, Frank; Armes, Steven P; Fujii, Syuji; Dupin, Damien; Ormond-Prout, Jonathan; Sternovsky, Zoltan; Kempf, Sascha; Moragas-Klostermeyer, Georg; Mocker, Anna; Grün, Eberhard

2009-12-01

The study of hyper-velocity impacts of micrometeoroids is important for the calibration of dust sensors in space applications. For this purpose, submicron-sized synthetic dust grains comprising either polystyrene or poly[bis(4-vinylthiophenyl)sulfide] were coated with an ultrathin overlayer of an electrically conductive organic polymer (either polypyrrole or polyaniline) and were accelerated to speeds between 3 and 35 km s(-1) using the Heidelberg Dust Accelerator facility. Time-of-flight mass spectrometry was applied to analyse the resulting ionic impact plasma using a newly developed Large Area Mass Analyser (LAMA). Depending on the projectile type and the impact speed, both aliphatic and aromatic molecular ions and cluster species were identified in the mass spectra with masses up to 400 u. Clusters resulting from the target material (silver) and mixed clusters of target and projectile species were also observed. Impact velocities of between 10 and 35 km s(-1) are suitable for a principal identification of organic materials in micrometeoroids, whereas impact speeds below approximately 10 km s(-1) allow for an even more detailed analysis. Molecular ions and fragments reflect components of the parent molecule, providing determination of even complex organic molecules embedded in a dust grain. In contrast to previous measurements with the Cosmic Dust Analyser instrument, the employed LAMA instrument has a seven times higher mass resolution--approximately 200--which allowed for a detailed analysis of the complex mass spectra. These fundamental studies are expected to enhance our understanding of cometary, interplanetary and interstellar dust grains, which travel at similar hyper-velocities and are known to contain both aliphatic and aromatic organic compounds. Copyright 2009 John Wiley & Sons, Ltd.

Metabolomics by Gas Chromatography-Mass Spectrometry: the combination of targeted and untargeted profiling

Science.gov (United States)

Fiehn, Oliver

2016-01-01

Gas chromatography-mass spectrometry (GC-MS)-based metabolomics is ideal for identifying and quantitating small molecular metabolites (metabolomics easily allows integrating targeted assays for absolute quantification of specific metabolites with untargeted metabolomics to discover novel compounds. Complemented by database annotations using large spectral libraries and validated, standardized standard operating procedures, GC-MS can identify and semi-quantify over 200 compounds per study in human body fluids (e.g., plasma, urine or stool) samples. Deconvolution software enables detection of more than 300 additional unidentified signals that can be annotated through accurate mass instruments with appropriate data processing workflows, similar to liquid chromatography-MS untargeted profiling (LC-MS). Hence, GC-MS is a mature technology that not only uses classic detectors (‘quadrupole’) but also target mass spectrometers (‘triple quadrupole’) and accurate mass instruments (‘quadrupole-time of flight’). This unit covers the following aspects of GC-MS-based metabolomics: (i) sample preparation from mammalian samples, (ii) acquisition of data, (iii) quality control, and (iv) data processing. PMID:27038389

Recent applications of gas chromatography with high-resolution mass spectrometry.

Science.gov (United States)

Špánik, Ivan; Machyňáková, Andrea

2018-01-01

Gas chromatography coupled to high-resolution mass spectrometry is a powerful analytical method that combines excellent separation power of gas chromatography with improved identification based on an accurate mass measurement. These features designate gas chromatography with high-resolution mass spectrometry as the first choice for identification and structure elucidation of unknown volatile and semi-volatile organic compounds. Gas chromatography with high-resolution mass spectrometry quantitative analyses was previously focused on the determination of dioxins and related compounds using magnetic sector type analyzers, a standing requirement of many international standards. The introduction of a quadrupole high-resolution time-of-flight mass analyzer broadened interest in this method and novel applications were developed, especially for multi-target screening purposes. This review is focused on the development and the most interesting applications of gas chromatography coupled to high-resolution mass spectrometry towards analysis of environmental matrices, biological fluids, and food safety since 2010. The main attention is paid to various approaches and applications of gas chromatography coupled to high-resolution mass spectrometry for non-target screening to identify contaminants and to characterize the chemical composition of environmental, food, and biological samples. The most interesting quantitative applications, where a significant contribution of gas chromatography with high-resolution mass spectrometry over the currently used methods is expected, will be discussed as well. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Comparison of gas chromatography/isotope ratio mass spectrometry and liquid chromatography/isotope ratio mass spectrometry for carbon stable-isotope analysis of carbohydrates

NARCIS (Netherlands)

Moerdijk-Poortvliet, Tanja C. W.; Schierbeek, Henk; Houtekamer, Marco; van Engeland, Tom; Derrien, Delphine; Stal, Lucas J.; Boschker, Henricus T. S.

2015-01-01

We compared gas chromatography/isotope ratio mass spectrometry (GC/IRMS) and liquid chromatography/isotope ratio mass spectrometry (LC/IRMS) for the measurement of δ(13)C values in carbohydrates. Contrary to GC/IRMS, no derivatisation is needed for LC/IRMS analysis of carbohydrates. Hence, although

Comparison of gas chromatography/isotope ratio mass spectrometry and liquid chromatography/isotope ratio mass spectrometry for carbon stable-isotope analysis of carbohydrates

NARCIS (Netherlands)

Moerdijk-Poortvliet, T.C.W.; Schierbeek, H.; Houtekamer, M.; van Engeland, T.; Derrien, D.; Stal, L.J.; Boschker, H.T.S.

2015-01-01

We compared gas chromatography/isotope ratio mass spectrometry (GC/IRMS) and liquid chromatography/isotope ratio mass spectrometry (LC/IRMS) for the measurement of d13C values in carbohydrates. Contrary to GC/IRMS, no derivatisation is needed for LC/IRMS analysis of carbohydrates. Hence, although

Comparison of gas chromatography/isotope ratio mass spectrometry and liquid chromatography/isotope ratio mass spectrometry for carbon stable-isotope analysis of carbohydrates

NARCIS (Netherlands)

Moerdijk-Poortvliet, T.C.W.; Schierbeek, H.; Houtekamer, M.; van Engeland, T.; Derrien, D.; Stal, L.J.; Boschker, H.T.S.

2015-01-01

Rationale: We compared gas chromatography/isotope ratio mass spectrometry (GC/IRMS) and liquid chromatography/isotope ratio mass spectrometry (LC/IRMS) for the measurement of δ13C values in carbohydrates. Contrary to GC/IRMS, no derivatisation is needed for LC/IRMS analysis of carbohydrates. Hence,

Mass Spectrometry Imaging under Ambient Conditions

Science.gov (United States)

Wu, Chunping; Dill, Allison L.; Eberlin, Livia S.; Cooks, R. Graham; Ifa, Demian R.

2012-01-01

Mass spectrometry imaging (MSI) has emerged as an important tool in the last decade and it is beginning to show potential to provide new information in many fields owing to its unique ability to acquire molecularly specific images and to provide multiplexed information, without the need for labeling or staining. In MSI, the chemical identity of molecules present on a surface is investigated as a function of spatial distribution. In addition to now standard methods involving MSI in vacuum, recently developed ambient ionization techniques allow MSI to be performed under atmospheric pressure on untreated samples outside the mass spectrometer. Here we review recent developments and applications of MSI emphasizing the ambient ionization techniques of desorption electrospray ionization (DESI), laser ablation electrospray ionization (LAESI), probe electrospray ionization (PESI), desorption atmospheric pressure photoionization (DAPPI), femtosecond laser desorption ionization (fs-LDI), laser electrospray mass spectrometry (LEMS), infrared laser ablation metastable-induced chemical ionization (IR-LAMICI), liquid microjunction surface sampling probe mass spectrometry (LMJ-SSP MS), nanospray desorption electrospray ionization (nano-DESI), and plasma sources such as the low temperature plasma (LTP) probe and laser ablation coupled to flowing atmospheric-pressure afterglow (LA-FAPA). Included are discussions of some of the features of ambient MSI including the ability to implement chemical reactions with the goal of providing high abundance ions characteristic of specific compounds of interest and the use of tandem mass spectrometry to either map the distribution of targeted molecules with high specificity or to provide additional MS information in the structural identification of compounds. We also describe the role of bioinformatics in acquiring and interpreting the chemical and spatial information obtained through MSI, especially in biological applications for tissue

MPAI (mass probes aided ionization) method for total analysis of biomolecules by mass spectrometry.

Science.gov (United States)

Honda, Aki; Hayashi, Shinichiro; Hifumi, Hiroki; Honma, Yuya; Tanji, Noriyuki; Iwasawa, Naoko; Suzuki, Yoshio; Suzuki, Koji

2007-01-01

We have designed and synthesized various mass probes, which enable us to effectively ionize various molecules to be detected with mass spectrometry. We call the ionization method using mass probes the "MPAI (mass probes aided ionization)" method. We aim at the sensitive detection of various biological molecules, and also the detection of bio-molecules by a single mass spectrometry serially without changing the mechanical settings. Here, we review mass probes for small molecules with various functional groups and mass probes for proteins. Further, we introduce newly developed mass probes for proteins for highly sensitive detection.

Analysis of mass spectrometry data in proteomics

DEFF Research Database (Denmark)

Matthiesen, Rune; Jensen, Ole N

2008-01-01

The systematic study of proteins and protein networks, that is, proteomics, calls for qualitative and quantitative analysis of proteins and peptides. Mass spectrometry (MS) is a key analytical technology in current proteomics and modern mass spectrometers generate large amounts of high-quality data...... that in turn allow protein identification, annotation of secondary modifications, and determination of the absolute or relative abundance of individual proteins. Advances in mass spectrometry-driven proteomics rely on robust bioinformatics tools that enable large-scale data analysis. This chapter describes...... some of the basic concepts and current approaches to the analysis of MS and MS/MS data in proteomics....

Expert systems technology applied to instrument operation and data acquisition of a triple quadrupole mass spectrometer (TQMS)

International Nuclear Information System (INIS)

Wong, C.M.

1984-01-01

This presentation covers the work done at Lawrence Livermore National Laboratory by some computer programmers and analytical chemists specializing in mass spectrometry to develop an expert system for real-time tuning and optimization of operations of a triple quadrupole mass spectrometer (TQMS). This capability is important to increase the sensitivity possible for selected compounds throughout the entire mass range of the instrument, rather than settling for the traditional normalized calibration which lowers sensitivity at both ends of the mass scale

Determination of 4-Methylimidazole in Ammonia Caramel Using Gas Chromatography–Tandem Mass Spectrometry (GC-MS/MS

Directory of Open Access Journals (Sweden)

Martyna N. Wieczorek

2018-01-01

Full Text Available One of Maillard reaction products formed in the production of ammonia caramel is 4(5-methylimidazole (4-MeI classified as carcinogen. A method of 4-MeI determination based on ion-pair extraction and derivatisation with isobutyl chloroformate with subsequent gas chromatography-tandem mass spectrometry analysis was proposed. Tandem mass spectrometry was applied to reduce the influence of matrix and increase the selectivity and sensitivity of the method. Triple quadrupole GC-MS system was used for this study. The collision energies were optimized for MRM mode. The detection (LOD and quantification limits (LOQ of the elaborated method were 17 and 37.8 μg kg−1, respectively, repeatability was <15% RSD for analyzed caramel samples, and the recovery for 4-MeI was 101%. Comparison of MS/MS with SIM detection on the same instrument proved almost 30 times lower LODs achieved by tandem mass spectrometry compared to SIM. Described method can be routinely used for monitoring 4-MeI as a quality and safety marker in the production of ammonia caramel.

Accelerator mass spectrometry-current status in techniques and applications

International Nuclear Information System (INIS)

Imamura, Mineo; Nagai, Hisao; Kobayashi, Koichi.

1991-01-01

Accelerator mass spectrometry (AMS) is the mass spectrometry by incorporating an accelerator. After samples are ionized, they are accelerated to a certain energy, and mass, energy, nuclear charge (atomic number) are distinguished, and ion counting is made one by one with a heavy ion detector. For the measurement of long half-life radioisotopes, mass spectrometry has been used because of the high sensitivity, but in low energy mass spectrometry, there are the difficulties due to the mixing of the molecular ions having nearly same mass and the existence of isobars. One of the methods solving these difficulties is an accelerator which enables background-free measurement. The progress of AMS is briefly described, and at present, it is carried out in about 30 facilities in the world. In AMS, the analysis is carried out in the order of the ionization of samples, the acceleration of beam, the electron stripping with a thin film, the sorting of the momentum and energy of beam and the identification of particles. The efficiency, sensitivity and accuracy of detection and the application are reported. (K.I.)

[Advances in mass spectrometry-based approaches for neuropeptide analysis].

Science.gov (United States)

Ji, Qianyue; Ma, Min; Peng, Xin; Jia, Chenxi; Ji, Qianyue

2017-07-25

Neuropeptides are an important class of endogenous bioactive substances involved in the function of the nervous system, and connect the brain and other neural and peripheral organs. Mass spectrometry-based neuropeptidomics are designed to study neuropeptides in a large-scale manner and obtain important molecular information to further understand the mechanism of nervous system regulation and the pathogenesis of neurological diseases. This review summarizes the basic strategies for the study of neuropeptides using mass spectrometry, including sample preparation and processing, qualitative and quantitative methods, and mass spectrometry imagining.

Secondary Ion Mass Spectrometry SIMS XI

Science.gov (United States)

Gillen, G.; Lareau, R.; Bennett, J.; Stevie, F.

2003-05-01

This volume contains 252 contributions presented as plenary, invited and contributed poster and oral presentations at the 11th International Conference on Secondary Ion Mass Spectrometry (SIMS XI) held at the Hilton Hotel, Walt Disney World Village, Orlando, Florida, 7 12 September, 1997. The book covers a diverse range of research, reflecting the rapid growth in advanced semiconductor characterization, ultra shallow depth profiling, TOF-SIMS and the new areas in which SIMS techniques are being used, for example in biological sciences and organic surface characterization. Papers are presented under the following categories: Isotopic SIMS Biological SIMS Semiconductor Characterization Techniques and Applications Ultra Shallow Depth Profiling Depth Profiling Fundamental/Modelling and Diffusion Sputter-Induced Topography Fundamentals of Molecular Desorption Organic Materials Practical TOF-SIMS Polyatomic Primary Ions Materials/Surface Analysis Postionization Instrumentation Geological SIMS Imaging Fundamentals of Sputtering Ion Formation and Cluster Formation Quantitative Analysis Environmental/Particle Characterization Related Techniques These proceedings provide an invaluable source of reference for both newcomers to the field and experienced SIMS users.

Identification of Fatty Acids, Phospholipids, and Their Oxidation Products Using Matrix-Assisted Laser Desorption Ionization Mass Spectrometry and Electrospray Ionization Mass Spectrometry

Science.gov (United States)

Harmon, Christopher W.; Mang, Stephen A.; Greaves, John; Finlayson-Pitts, Barbara J.

2010-01-01

Electrospray ionization mass spectrometry (ESI-MS) and matrix-assisted laser desorption ionization mass spectrometry (MALDI-MS) have found increasing application in the analysis of biological samples. Using these techniques to solve problems in analytical chemistry should be an essential component of the training of undergraduate chemists. We…

Ultratrace analysis of uranium and plutonium by mass spectrometry

International Nuclear Information System (INIS)

Wogman, N.A.; Wacker, J.F.; Olsen, K.B.; Petersen, S.L.; Farmer, O.T.; Kelley, J.M.; Eiden, G.C.; Maiti, T.C.

2002-01-01

Full text: Uranium and plutonium have traditionally been analyzed using alpha energy spectrometry. Both isotopic compositions and elemental abundances can be characterized on samples containing microgram to milligram quantities of uranium and nanogram to microgram quantities of plutonium. In the past ten years or so, considerable interest has developed in measuring nanograms quantities of uranium and sub-picogram quantities of plutonium in environmental samples. Such measurements require high sensitivity and as a consequence, sensitive mass spectrometric-based methods have been developed. Thus, the analysis of uranium and plutonium have gone from counting decays to counting atoms, with considerable increases in both sensitivity and precision for isotopic measurements. At the Pacific Northwest National Laboratory (PNNL), we have developed highly sensitive methods to analyze uranium and plutonium in environmental samples. The development of an ultratrace analysis capability for measuring uranium and plutonium has arisen from a need to detect and characterize environmental samples for signatures associated with nuclear industry processes. Our most sensitive well-developed methodologies employ thermal ionization mass spectrometry (TIMS), however, recent advances in inductively coupled plasma mass spectrometry (ICP-MS) have shown considerable promise for use in detecting uranium and plutonium at ultratrace levels. The work at PNNL has included the development of both chemical separation and purification techniques, as well as the development of mass spectrometric instrumentation and techniques. At the heart of our methodology for TIMS analysis is a procedure that utilizes 100-microliter-volumes of analyte for chemical processing to purify, separate, and load actinide elements into resin beads for subsequent mass spectrometric analysis. The resin bead technique has been combined with a thorough knowledge of the physicochemistry of thermal ion emission to achieve

Analysis of posttranslational modifications of proteins by tandem mass spectrometry

DEFF Research Database (Denmark)

Larsen, Martin Røssel; Trelle, Morten B; Thingholm, Tine E

2006-01-01

-temporal distribution in cells and tissues. Most PTMs can be detected by protein and peptide analysis by mass spectrometry (MS), either as a mass increment or a mass deficit relative to the nascent unmodified protein. Tandem mass spectrometry (MS/MS) provides a series of analytical features that are highly useful...

Imaging Mass Spectrometry in Neuroscience

Science.gov (United States)

2013-01-01

Imaging mass spectrometry is an emerging technique of great potential for investigating the chemical architecture in biological matrices. Although the potential for studying neurobiological systems is evident, the relevance of the technique for application in neuroscience is still in its infancy. In the present Review, a principal overview of the different approaches, including matrix assisted laser desorption ionization and secondary ion mass spectrometry, is provided with particular focus on their strengths and limitations for studying different neurochemical species in situ and in vitro. The potential of the various approaches is discussed based on both fundamental and biomedical neuroscience research. This Review aims to serve as a general guide to familiarize the neuroscience community and other biomedical researchers with the technique, highlighting its great potential and suitability for comprehensive and specific chemical imaging. PMID:23530951

Quantification of steroid conjugates using fast atom bombardment mass spectrometry

International Nuclear Information System (INIS)

Gaskell, S.J.

1990-01-01

Fast atom bombardment/mass spectrometry or liquid secondary ion mass spectrometry provides the capability for direct analysis of steroid conjugates (sulfates, glucuronides) without prior hydrolysis or derivatization. During the analysis of biologic extracts, limitations on the sensitivity of detection arise from the presence of co-extracted material which may suppress or obscure the analyte signal. A procedure is described for the quantitative determination of dehydroepiandrosterone sulfate in serum which achieved selective isolation of the analyte using immunoadsorption extraction and highly specific detection using tandem mass spectrometry. A stable isotope-labeled analog [( 2H2]dehydroepiandrosterone sulfate) was used as internal standard. Fast atom bombardment of dehydroepiandrosterone sulfate yielded abundant [M-H]- ions that fragmented following collisional activation to give HSO4-; m/z 97. During fast atom bombardment/tandem mass spectrometry of serum extracts, a scan of precursor ions fragmenting to give m/z 97 detected dehydroepiandrosterone sulfate and the [2H2]-labeled analog with a selectivity markedly superior to that observed using conventional mass spectrometry detection. Satisfactory agreement was observed between quantitative data obtained in this way and data obtained by gas chromatography/mass spectrometry of the heptafluorobutyrates of dehydroepiandrosterone sulfate and [2H2]dehydroepiandrosterone sulfate obtained by direct derivatization. 21 refs

Quantitative mass spectrometry: an overview

Science.gov (United States)

Urban, Pawel L.

2016-10-01

Mass spectrometry (MS) is a mainstream chemical analysis technique in the twenty-first century. It has contributed to numerous discoveries in chemistry, physics and biochemistry. Hundreds of research laboratories scattered all over the world use MS every day to investigate fundamental phenomena on the molecular level. MS is also widely used by industry-especially in drug discovery, quality control and food safety protocols. In some cases, mass spectrometers are indispensable and irreplaceable by any other metrological tools. The uniqueness of MS is due to the fact that it enables direct identification of molecules based on the mass-to-charge ratios as well as fragmentation patterns. Thus, for several decades now, MS has been used in qualitative chemical analysis. To address the pressing need for quantitative molecular measurements, a number of laboratories focused on technological and methodological improvements that could render MS a fully quantitative metrological platform. In this theme issue, the experts working for some of those laboratories share their knowledge and enthusiasm about quantitative MS. I hope this theme issue will benefit readers, and foster fundamental and applied research based on quantitative MS measurements. This article is part of the themed issue 'Quantitative mass spectrometry'.

Structural analyses of sucrose laurate regioisomers by mass spectrometry techniques

DEFF Research Database (Denmark)

Lie, Aleksander; Stensballe, Allan; Pedersen, Lars Haastrup

2015-01-01

6- And 6′-O-lauroyl sucrose were isolated and analyzed by matrix-assisted laser desorption/ionisation (MALDI) time-of-flight (TOF) mass spectrometry (MS), Orbitrap high-resolution (HR) MS, and electrospray-ionization (ESI) tandem mass spectrometry (MS/MS). The analyses aimed to explore the physic......6- And 6′-O-lauroyl sucrose were isolated and analyzed by matrix-assisted laser desorption/ionisation (MALDI) time-of-flight (TOF) mass spectrometry (MS), Orbitrap high-resolution (HR) MS, and electrospray-ionization (ESI) tandem mass spectrometry (MS/MS). The analyses aimed to explore.......8, respectively, and Orbitrap HRMS confirmed the mass of [M+Na]+ (m/z 547.2712). ESI-MS/MS on the precursor ion [M+Na]+ resulted in product ion mass spectra showing two high-intensity signals for each sample. 6-O-Lauroyl sucrose produced signals located at m/z 547.27 and m/z 385.21, corresponding to the 6-O...

Absorption Mode FT-ICR Mass Spectrometry Imaging

Energy Technology Data Exchange (ETDEWEB)

Smith, Donald F.; Kilgour, David P.; Konijnenburg, Marco; O' Connor, Peter B.; Heeren, Ronald M.

2013-12-03

Fourier transform ion cyclotron resonance mass spectrometry offers the highest mass resolving power for molecular imaging experiments. This high mass resolving power ensures that closely spaced peaks at the same nominal mass are resolved for proper image generation. Typically higher magnetic fields are used to increase mass resolving power. However, a gain in mass resolving power can also be realized by phase correction of the data for absorption mode display. In addition to mass resolving power, absorption mode offers higher mass accuracy and signal-to-noise ratio over the conventional magnitude mode. Here we present the first use of absorption mode for Fourier transform ion cyclotron resonance mass spectrometry imaging. The Autophaser algorithm is used to phase correct each spectrum (pixel) in the image and then these parameters are used by the Chameleon work-flow based data processing software to generate absorption mode ?Datacubes? for image and spectral viewing. Absorption mode reveals new mass and spatial features that are not resolved in magnitude mode and results in improved selected ion image contrast.

Detection of Radiation-Exposure Biomarkers by Differential Mobility Prefiltered Mass Spectrometry (DMS-MS).

Science.gov (United States)

Coy, Stephen L; Krylov, Evgeny V; Schneider, Bradley B; Covey, Thomas R; Brenner, David J; Tyburski, John B; Patterson, Andrew D; Krausz, Kris W; Fornace, Albert J; Nazarov, Erkinjon G

2010-04-15

Technology to enable rapid screening for radiation exposure has been identified as an important need, and, as a part of a NIH / NIAD effort in this direction, metabolomic biomarkers for radiation exposure have been identified in a recent series of papers. To reduce the time necessary to detect and measure these biomarkers, differential mobility spectrometry - mass spectrometry (DMS-MS) systems have been developed and tested. Differential mobility ion filters preselect specific ions and also suppress chemical noise created in typical atmospheric-pressure ionization sources (ESI, MALDI, and others). Differential-mobility-based ion selection is based on the field dependence of ion mobility, which, in turn, depends on ion characteristics that include conformation, charge distribution, molecular polarizability, and other properties, and on the transport gas composition which can be modified to enhance resolution. DMS-MS is able to resolve small-molecule biomarkers from nearly-isobaric interferences, and suppresses chemical noise generated in the ion source and in the mass spectrometer, improving selectivity and quantitative accuracy. Our planar DMS design is rapid, operating in a few milliseconds, and analyzes ions before fragmentation. Depending on MS inlet conditions, DMS-selected ions can be dissociated in the MS inlet expansion, before mass analysis, providing a capability similar to MS/MS with simpler instrumentation. This report presents selected DMS-MS experimental results, including resolution of complex test mixtures of isobaric compounds, separation of charge states, separation of isobaric biomarkers (citrate and isocitrate), and separation of nearly-isobaric biomarker anions in direct analysis of a bio-fluid sample from the radiation-treated group of a mouse-model study. These uses of DMS combined with moderate resolution MS instrumentation indicate the feasibility of field-deployable instrumentation for biomarker evaluation.

Sequencing Cyclic Peptides by Multistage Mass Spectrometry

Science.gov (United States)

Mohimani, Hosein; Yang, Yu-Liang; Liu, Wei-Ting; Hsieh, Pei-Wen; Dorrestein, Pieter C.; Pevzner, Pavel A.

2012-01-01

Some of the most effective antibiotics (e.g., Vancomycin and Daptomycin) are cyclic peptides produced by non-ribosomal biosynthetic pathways. While hundreds of biomedically important cyclic peptides have been sequenced, the computational techniques for sequencing cyclic peptides are still in their infancy. Previous methods for sequencing peptide antibiotics and other cyclic peptides are based on Nuclear Magnetic Resonance spectroscopy, and require large amount (miligrams) of purified materials that, for most compounds, are not possible to obtain. Recently, development of mass spectrometry based methods has provided some hope for accurate sequencing of cyclic peptides using picograms of materials. In this paper we develop a method for sequencing of cyclic peptides by multistage mass spectrometry, and show its advantages over single stage mass spectrometry. The method is tested on known and new cyclic peptides from Bacillus brevis, Dianthus superbus and Streptomyces griseus, as well as a new family of cyclic peptides produced by marine bacteria. PMID:21751357

Applications of Tandem Mass Spectrometry in the Structure Determination of Permethylated Sialic Acid-containing Oligosaccharides

International Nuclear Information System (INIS)

Yoo, Eun Sun; Yoon, In Mo

2005-01-01

Sets of sialic acid-containing trisaccharides having different internal and terminal linkages have been synthesized to develop a sensitive method for analysis of the reducing terminal linkage positions. The trisaccharides, sialyl(α 2-3)Gal(β 1-3)GalNAc and sialyl(α 2-3)Gal(β 1-X)GlcNAc where X=3, 4 and 6, were synthesized and examined using electrospray ionization (ESI)-collision induced dissociation (CID) tandem mass spectrometry (MS/MS). The compounds chosen for this study are related to terminal groups likely to be found on polylactosamine-like glycoproteins and glycolipids which occur on the surface of mammalian cells. The purpose of this study is to develop tandem mass spectrometral methods to determine detailed carbohydrate structures on permethylated or partially methylated oligosaccharides for future applications on biologically active glycoconjugates and to exploit a faster method of synthesizing a series of structural isomeric oligosaccharides to be used for further mass spectrometry and instrumental analysis

An Integrated Hot-Stage Microscope-Direct Analysis in Real Time-Mass Spectrometry System for Studying the Thermal Behavior of Materials.

Science.gov (United States)

Ashton, Gage P; Harding, Lindsay P; Parkes, Gareth M B

2017-12-19

This paper describes a new analytical instrument that combines a precisely temperature-controlled hot-stage with digital microscopy and Direct Analysis in Real Time-mass spectrometry (DART-MS) detection. The novelty of the instrument lies in its ability to monitor processes as a function of temperature through the simultaneous recording of images, quantitative color changes, and mass spectra. The capability of the instrument was demonstrated through successful application to four very varied systems including profiling an organic reaction, decomposition of silicone polymers, and the desorption of rhodamine B from an alumina surface. The multidimensional, real-time analytical data provided by this instrument allow for a much greater insight into thermal processes than could be achieved previously.

Detection of biological particles in ambient air using Bio-Aerosol Mass Spectrometry

International Nuclear Information System (INIS)

McJimpsey, E L; Steele, P T; Coffee, K R; Fergenson, D P; Riot, V J; Woods, B W; Gard, E E; Frank, M; Tobias, H J; Lebrilla, C

2006-01-01

The Bio-Aerosol Mass Spectrometry (BAMS) system is an instrument used for the real time detection and identification of biological aerosols. Particles are drawn from the atmosphere directly into vacuum and tracked as they scatter light from several continuous wave lasers. After tracking, the fluorescence of individual particles is excited by a pulsed 266nm or 355nm laser. Molecules from those particles with appropriate fluorescence properties are subsequently desorbed and ionized using a pulsed 266nm laser. Resulting ions are analyzed in a dual polarity mass spectrometer. During two field deployments at the San Francisco International Airport, millions of ambient particles were analyzed and a small but significant fraction were found to have fluorescent properties similar to Bacillus spores and vegetative cells. Further separation of non-biological background particles from potential biological particles was accomplished using laser desorption/ionization mass spectrometry. This has been shown to enable some level of species differentiation in specific cases, but the creation and observation of higher mass ions is needed to enable a higher level of specificity across more species. A soft ionization technique, matrix-assisted laser desorption/ionization (MALDI) is being investigated for this purpose. MALDI is particularly well suited for mass analysis of biomolecules since it allows for the generation of molecular ions from large mass compounds that would fragment under normal irradiation. Some of the initial results from a modified BAMS system utilizing this technique are described

Boundaries of mass resolution in native mass spectrometry

NARCIS (Netherlands)

Lössl, Philip|info:eu-repo/dai/nl/371559693; Snijder, Joost|info:eu-repo/dai/nl/338018328; Heck, Albert J R|info:eu-repo/dai/nl/105189332

Over the last two decades, native mass spectrometry (MS) has emerged as a valuable tool to study intact proteins and noncovalent protein complexes. Studied experimental systems range from small-molecule (drug)-protein interactions, to nanomachineries such as the proteasome and ribosome, to even

OBT measurement of vegetation by mass spectrometry and radiometry

International Nuclear Information System (INIS)

Tamari, T.; Kakiuchi, H.; Momoshima, N.; Sugihara, S.; Baglan, N.; Uda, T.

2011-01-01

We carried out OBT (organically bound tritium) measurement by two different methods those are radiometry and mass spectrometry and compared the applicability of these methods for environmental tritium analysis. The dried grass sample was used for the experiments. To eliminate the exchangeable OBT, the sample was washed with tritium free water before analysis. Three times washing reduced the tritium activity in the labile sites below the detectable level. In radiometry the sample was combusted to convert the OBT as well as other hydrogen isotopes to. water and tritium activity in the water was measured by liquid scintillation counting (LSC). In mass spectrometry, the sample was kept in a glass container and 3 He produced by tritium decay was measured by mass spectrometry. The results were in good agreement suggesting applicability of these methods for environmental tritium analysis. The mass spectrometry is more suitable for environmental tritium research because of a lower detection limit than that of the LSC. (authors)

Development of stereotactic mass spectrometry for brain tumor surgery.

Science.gov (United States)

Agar, Nathalie Y R; Golby, Alexandra J; Ligon, Keith L; Norton, Isaiah; Mohan, Vandana; Wiseman, Justin M; Tannenbaum, Allen; Jolesz, Ferenc A

2011-02-01

Surgery remains the first and most important treatment modality for the majority of solid tumors. Across a range of brain tumor types and grades, postoperative residual tumor has a great impact on prognosis. The principal challenge and objective of neurosurgical intervention is therefore to maximize tumor resection while minimizing the potential for neurological deficit by preserving critical tissue. To introduce the integration of desorption electrospray ionization mass spectrometry into surgery for in vivo molecular tissue characterization and intraoperative definition of tumor boundaries without systemic injection of contrast agents. Using a frameless stereotactic sampling approach and by integrating a 3-dimensional navigation system with an ultrasonic surgical probe, we obtained image-registered surgical specimens. The samples were analyzed with ambient desorption/ionization mass spectrometry and validated against standard histopathology. This new approach will enable neurosurgeons to detect tumor infiltration of the normal brain intraoperatively with mass spectrometry and to obtain spatially resolved molecular tissue characterization without any exogenous agent and with high sensitivity and specificity. Proof of concept is presented in using mass spectrometry intraoperatively for real-time measurement of molecular structure and using that tissue characterization method to detect tumor boundaries. Multiple sampling sites within the tumor mass were defined for a patient with a recurrent left frontal oligodendroglioma, World Health Organization grade II with chromosome 1p/19q codeletion, and mass spectrometry data indicated a correlation between lipid constitution and tumor cell prevalence. The mass spectrometry measurements reflect a complex molecular structure and are integrated with frameless stereotaxy and imaging, providing 3-dimensional molecular imaging without systemic injection of any agents, which can be implemented for surgical margins delineation of

Mass Spectrometry of Halopyrazolium Salts

DEFF Research Database (Denmark)

Larsen, Elfinn; Egsgaard, Helge; Pande, U. C.

1983-01-01

Eleven halogen substituted 1-methyl-2-phenylpyrazolium bromides or chlorides were investigated by field desorption, field ionization, and electron impact mass spectrometry. Dealkylation was found to be the predominant thermal decomposition. An exchange between covalent and ionic halogen prior...

Analytical mass spectrometry. Abstracts

Energy Technology Data Exchange (ETDEWEB)

1990-12-31

This 43rd Annual Summer Symposium on Analytical Chemistry was held July 24--27, 1990 at Oak Ridge, TN and contained sessions on the following topics: Fundamentals of Analytical Mass Spectrometry (MS), MS in the National Laboratories, Lasers and Fourier Transform Methods, Future of MS, New Ionization and LC/MS Methods, and an extra session. (WET)

Use of mass spectrometry for study of coordination compounds

International Nuclear Information System (INIS)

Gehrbehlehu, N.V.; Indrichan, K.M.

1981-01-01

A review on mass-spectrometry of coordination compounds including the works published up to 1979 inclusive is provided. Mainly the products of metals with bi- and tetradentate ligands are considered using the method. Mo and Be carboxylates for which molecular ions lines are found in mass-spectra are studied. The study of mass-spectra for VO chelates with thiosemicarbazone of salicyl aldehyde is carried out. Application of the mass-spectrometry method permits to establish the mass of coordination compounds, the structure of complexes, dentate structure and the way of ligand coordination, the bond strength [ru

A qualitative study of amlodipine and its related compounds by electrospray ionization tandem mass spectrometry.

Science.gov (United States)

Gibbons, John; Pugh, Jonathan; Dimopoulos-Italiano, Gina; Pike, Richard

2006-01-01

A comprehensive structural analysis of amlodipine and certain related compounds was performed by electrospray ionization tandem mass spectrometry. Triple quadrupole and quadrupole time-of-flight instruments were used to provide collision-induced dissociation and accurate mass measurement for selected product and second-generation product ions. A unique ion rearrangement was observed, which was found to be characteristic of certain dihydropyridines. This study provides a fundamental understanding of the fragmentation of these compounds. The structural elucidation of an unknown impurity is presented as an example. Copyright (c) 2006 John Wiley & Sons, Ltd.

Multi-elemental analysis of aqueous geochemical samples by quadrupole inductively coupled plasma-mass spectrometry (ICP-MS)

Science.gov (United States)

Wolf, Ruth E.; Adams, Monique

2015-01-01

Typically, quadrupole inductively coupled plasma-mass spectrometry (ICP-MS) is used to determine as many as 57 major, minor, and trace elements in aqueous geochemical samples, including natural surface water and groundwater, acid mine drainage water, and extracts or leachates from geological samples. The sample solution is aspirated into the inductively coupled plasma (ICP) which is an electrodeless discharge of ionized argon gas at a temperature of approximately 6,000 degrees Celsius. The elements in the sample solution are subsequently volatilized, atomized, and ionized by the ICP. The ions generated are then focused and introduced into a quadrupole mass filter which only allows one mass to reach the detector at a given moment in time. As the settings of the mass analyzer change, subsequent masses are allowed to impact the detector. Although the typical quadrupole ICP-MS system is a sequential scanning instrument (determining each mass separately), the scan speed of modern instruments is on the order of several thousand masses per second. Consequently, typical total sample analysis times of 2–3 minutes are readily achievable for up to 57 elements.

Applications of mass spectrometry in the trace element analysis of biological materials

International Nuclear Information System (INIS)

Moens, L.

1997-01-01

The importance of mass spectrometry for the analysis of biological material is illustrated by reviewing the different mass spectrometric methods applied and describing some typical applications published recently. Though atomic absorption spectrometry is used in the majority of analyses of biological material, most mass spectrometric methods have been used to some extent for trace element determination in biomedical research. The relative importance of the different methods is estimated by reviewing recent research papers. It is striking that especially inductively coupled plasma mass spectrometry is increasingly being applied, partly because the method can be used on-line after chromatographic separation, in speciation studies. Mass spectrometric methods prove to offer unique possibilities in stable isotope tracer studies and for this purpose also experimentally demanding methods such as thermal ionization mass spectrometry and accelerator mass spectrometry are frequently used. (orig.)

Determination of uranium in urine - Measurement of isotope ratios and quantification by use of inductively coupled plasma mass spectrometry

NARCIS (Netherlands)

Krystek, Petra; Ritsema, R.

2002-01-01

For analysis of uranium in urine determination of the isotope ratio and quantification were investigated by high-resolution inductively coupled plasma mass spectrometry (HR ICP-MS). The instrument used (ThermoFinniganMAT ELEMENT2) is a single-collector MS and, therefore, a stable sample-introduction

A Review of the Emerging Field of Underwater Mass Spectrometry

Directory of Open Access Journals (Sweden)

Emily Chua

2016-11-01

Full Text Available Mass spectrometers are versatile sensor systems, owing to their high sensitivity and ability to simultaneously measure multiple chemical species. Over the last two decades, traditional laboratory-based membrane inlet mass spectrometers have been adapted for underwater use. Underwater mass spectrometry has drastically improved our capability to monitor a broad suite of gaseous compounds (e.g., dissolved atmospheric gases, light hydrocarbons, and volatile organic compounds in the aquatic environment. Here we provide an overview of the progress made in the field of underwater mass spectrometry since its inception in the 1990s to the present. In particular, we discuss the approaches undertaken by various research groups in developing in situ mass spectrometers. We also provide examples to illustrate how underwater mass spectrometers have been used in the field. Finally, we present future trends in the field of in situ mass spectrometry. Most of these efforts are aimed at improving the quality and spatial and temporal scales of chemical measurements in the ocean. By providing up-to-date information on underwater mass spectrometry, this review offers guidance for researchers interested in adapting this technology as well as goals for future progress in the field.

Open Access UHPSFC/MS - an additional analytical resource for an academic mass spectrometry facility.

Science.gov (United States)

Herniman, Julie M; Langley, G John

2016-08-15

Many compounds submitted for analysis in Chemistry at the University of Southampton do not retain, elute or ionize using open access reversed-phase ultra-high-performance liquid chromatography/mass spectrometry (RP-UHPLC/MS) and require analysis via infusion. An ultra-high-performance supercritical fluid chromatography mass spectrometry approach was implemented to afford high-throughput analysis of these compounds with chromatographic separation. A UPC(2) -TQD MS system has been incorporated into the open access MS provision within Chemistry at the University of Southampton, using an ESCi source (electrospray and atmospheric pressure chemical ionization) and an atmospheric pressure photoionization (APPI) source. Access to instrumentation is enabled via a web-based interface (RemoteAnalyzer™). Compounds such as fluorosugars, fullerenes, phosphoramidites, porphyrins, and rotaxanes exhibiting properties incompatible with RP-UHPLC/MS have been analyzed using automated chromatography and mass spectrometry methods. The speedy return of data enables research in these areas to progress unhindered by sample type. The provision of an electronic web format enables easy incorporation of chromatograms and mass spectra into electronic files and reports. The implementation of UHPSFC/MS increases access to a wide range of chemistries incompatible with reversed-phase chromatography and polar solvents, enabling more than 90% of submitted samples to be analyzed using an open access approach. Further, chromatographic separation is provided where previously flow injection or infusion analyses were the only options. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

Correcting mass shifts: A lock mass-free recalibration procedure for mass spectrometry imaging data

Czech Academy of Sciences Publication Activity Database

Kulkarni, P.; Kaftan, F.; Kynast, P.; Svatoš, Aleš; Böcker, S.

2015-01-01

Roč. 407, č. 25 (2015), s. 7603-7613 ISSN 1618-2642 Institutional support: RVO:61388963 Keywords : mass spectrometry imaging * recalibration * mass shift correction * data processing Subject RIV: CB - Analytical Chemistry , Separation Impact factor: 3.125, year: 2015

Mass spectrometry in epigenetic research

DEFF Research Database (Denmark)

Beck, Hans Christian

2010-01-01

cancers has gained tremendous interest in recent years, and many of these inhibitors are currently undergoing clinical trials. Despite intense research, however, the exact molecular mechanisms of action of these molecules remain, to a wide extent, unclear. The recent application of mass spectrometry...

Liquid chromatography-mass spectrometry in forensic toxicology.

Science.gov (United States)

Van Bocxlaer, J F; Clauwaert, K M; Lambert, W E; Deforce, D L; Van den Eeckhout, E G; De Leenheer, A P

2000-01-01

Liquid chromatography-mass spectrometry has evolved from a topic of mainly research interest into a routinely usable tool in various application fields. With the advent of new ionization approaches, especially atmospheric pressure, the technique has established itself firmly in many areas of research. Although many applications prove that LC-MS is a valuable complementary analytical tool to GC-MS and has the potential to largely extend the application field of mass spectrometry to hitherto "MS-phobic" molecules, we must recognize that the use of LC-MS in forensic toxicology remains relatively rare. This rarity is all the more surprising because forensic toxicologists find themselves often confronted with the daunting task of actually searching for evidence materials on a scientific basis without any indication of the direction in which to search. Through the years, mass spectrometry, mainly in the GC-MS form, has gained a leading role in the way such quandaries are tackled. The advent of robust, bioanalytically compatible combinations of liquid chromatographic separation with mass spectrometric detection really opens new perspectives in terms of mass spectrometric identification of difficult molecules (e.g., polar metabolites) or biopolymers with toxicological relevance, high throughput, and versatility. Of course, analytical toxicologists are generally mass spectrometry users rather than mass spectrometrists, and this difference certainly explains the slow start of LC-MS in this field. Nevertheless, some valuable applications have been published, and it seems that the introduction of the more universal atmospheric pressure ionization interfaces really has boosted interests. This review presents an overview of what has been realized in forensic toxicological LC-MS. After a short introduction into LC-MS interfacing operational characteristics (or limitations), it covers applications that range from illicit drugs to often abused prescription medicines and some

Novel product ions of 2-aminoanilide and benzimidazole Ag(I) complexes using electrospray ionization with multi-stage tandem mass spectrometry.

Science.gov (United States)

Johnson, Byron S; Burinsky, David J; Burova, Svetlana A; Davis, Roman; Fitzgerald, Russ N; Matsuoka, Richard T

2012-05-15

The 2-aminoaniline scaffold is of significant value to the pharmaceutical industry and is embedded in a number of pharmacophores including 2-aminoanilides and benzimidazoles. A novel application of coordination ion spray mass spectrometry (CIS-MS) for interrogating the silver ion (Ag(+)) complexes of a homologous series of these compounds using multi-stage tandem mass spectrometry is described. Unlike the ubiquitous alkali metal ion complexes, Ag(+) complexes of 2-aminoanilides and benzimidazoles were found to yield [M - H](+) ions in significant abundance via gas-phase elimination of the metal hydride (AgH) resulting in unique product ion cascades. Sample introduction was by liquid chromatography with mass spectrometry analysis performed on a hybrid linear ion trap/orbitrap instrument capable of high-resolution measurements. Rigorous structural characterization by multi-stage tandem mass spectrometry using [M +  H](+), [M - H](-) and [M - H](+) precursor ions derived from ESI and CIS experiments was performed for the homologous series of 2-aminoanilide and benzimidazole compounds. A full tabular comparison of structural information resulting from these product ion cascades was produced. Multi-stage tandem mass spectrometry of [M - H](+) ions resulting from Ag(+) complexes of 2-aminoanilides and benzimidazoles in CIS-MS experiments produced unique product ion cascades that exhibited complementary structural information to that obtained from tandem mass spectrometry of [M  +  H](+) and [M - H](-) ions by electrospray ionization (ESI). These observations may be broadly applicable to other compounds that are observed to form Ag(+) complexes and eliminate AgH. Copyright © 2012 John Wiley & Sons, Ltd.

Analysis of [U-13C6]glucose in human plasma using liquid chromatography/isotope ratio mass spectrometry compared with two other mass spectrometry techniques

NARCIS (Netherlands)

Schierbeek, H.; Moerdijk-Poortvliet, T.C.W.; van den Akker, C.H.P.; te Braake, F.W.J.; Boschker, H.T.S.; van Goudoever, J.B.

2009-01-01

The use of stable isotope labelled glucose provides insight into glucose metabolism. The 13C-isotopic enrichment of glucose is usually measured by gas chromatography/mass spectrometry (GC/MS) or gas chromatography/combustion/isotope ratio mass spectrometry (GC/C/IRMS). However, in both techniques

The Assessment of Selectivity in Different Quadrupole-Orbitrap Mass Spectrometry Acquisition Modes

Science.gov (United States)

Berendsen, Bjorn J. A.; Wegh, Robin S.; Meijer, Thijs; Nielen, Michel W. F.

2015-02-01

Selectivity of the confirmation of identity in liquid chromatography (tandem) mass spectrometry using Q-Orbitrap instrumentation was assessed using different acquisition modes based on a representative experimental data set constructed from 108 samples, including six different matrix extracts and containing over 100 analytes each. Single stage full scan, all ion fragmentation, and product ion scanning were applied. By generating reconstructed ion chromatograms using unit mass window in targeted MS2, selected reaction monitoring (SRM), regularly applied using triple-quadrupole instruments, was mimicked. This facilitated the comparison of single stage full scan, all ion fragmentation, (mimicked) SRM, and product ion scanning applying a mass window down to 1 ppm. Single factor Analysis of Variance was carried out on the variance (s2) of the mass error to determine which factors and interactions are significant parameters with respect to selectivity. We conclude that selectivity is related to the target compound (mainly the mass defect), the matrix, sample clean-up, concentration, and mass resolution. Selectivity of the different instrumental configurations was quantified by counting the number of interfering peaks observed in the chromatograms. We conclude that precursor ion selection significantly contributes to selectivity: monitoring of a single product ion at high mass accuracy with a 1 Da precursor ion window proved to be equally selective or better to monitoring two transition products in mimicked SRM. In contrast, monitoring a single fragment in all ion fragmentation mode results in significantly lower selectivity versus mimicked SRM. After a thorough inter-laboratory evaluation study, the results of this study can be used for a critical reassessment of the current identification points system and contribute to the next generation of evidence-based and robust performance criteria in residue analysis and sports doping.

Two-step Laser Time-of-Flight Mass Spectrometry to Elucidate Organic Diversity in Planetary Surface Materials.

Science.gov (United States)

Getty, Stephanie A.; Brinckerhoff, William B.; Cornish, Timothy; Li, Xiang; Floyd, Melissa; Arevalo, Ricardo Jr.; Cook, Jamie Elsila; Callahan, Michael P.

2013-01-01

Laser desorption/ionization time-of-flight mass spectrometry (LD-TOF-MS) holds promise to be a low-mass, compact in situ analytical capability for future landed missions to planetary surfaces. The ability to analyze a solid sample for both mineralogical and preserved organic content with laser ionization could be compelling as part of a scientific mission pay-load that must be prepared for unanticipated discoveries. Targeted missions for this instrument capability include Mars, Europa, Enceladus, and small icy bodies, such as asteroids and comets.

Atmospheric pressure photo ionization hydrogen/deuterium exchange mass spectrometry--a method to differentiate isomers by mass spectrometry.

Science.gov (United States)

Ahmed, Arif; Kim, Sunghwan

2013-12-01

In this report, a method for in-source hydrogen/deuterium (H/D) exchange at atmospheric pressure is reported. The method was named atmospheric pressure photo ionization hydrogen/deuterium exchange mass spectrometry (APPI HDX MS). H/D exchange was performed by mixing samples dissolved in toluene with CH3OD solvent and analyzing the mixture using atmospheric pressure photo ionization mass spectrometry (APPI-MS). The APPI HDX spectra obtained with contact times between the analyte solution and methanol-OD (CH3OD) of atmospheric pressure. H/D exchange can be performed in any laboratory with a mass spectrometer and a commercial APPI source. Using this method, multiple H/D exchanges of aromatic hydrogen and/or H/D exchange of active hydrogen were observed. These results demonstrated that H/D exchange can be used to distinguish between isomers containing primary, secondary, and tertiary amines, as well as pyridine and pyrrole functional groups.

Mass spectrometry with particle accelerator

International Nuclear Information System (INIS)

Anon.

1983-01-01

The heavy ion accelerator use is renewing the ultrasensitive mass spectrometry in extending the detection limits. These new devices allow the measurement of rare isotope ratio, as 10 Be, 14 C, 26 Al, 36 Cl or 41 Ca, from the earth natural reservoirs [fr

Accelerator mass spectrometry: state of the art

Energy Technology Data Exchange (ETDEWEB)

Tuniz, C. [Australian Nuclear Science and Technology Organisation, Lucas Heights, NSW (Australia)

1996-12-31

Accelerator Mass Spectrometry (AMS) is the analytical technique of choice for the detection of long-lived radionuclides which cannot be practically analysed with decay counting or conventional mass spectrometry. The main use of AMS has been in the analysis of radiocarbon and other cosmogenic radionuclides for archaeological, geological and environmental applications. In addition, AMS has been recently applied in biomedicine to study exposure of human tissues to chemicals and biomolecules at attomole levels. There is also a world-wide effort to analyse rare nuclides of heavier masses, such as long-lived actinides, with important applications in safeguards and nuclear waste disposal. The use of AMS is limited by the expensive accelerator technology required and there are several attempts to develop smaller and cheaper AMS spectrometers. 5 refs.

Accelerator mass spectrometry: state of the art

Energy Technology Data Exchange (ETDEWEB)

Tuniz, C [Australian Nuclear Science and Technology Organisation, Lucas Heights, NSW (Australia)

1997-12-31

Accelerator Mass Spectrometry (AMS) is the analytical technique of choice for the detection of long-lived radionuclides which cannot be practically analysed with decay counting or conventional mass spectrometry. The main use of AMS has been in the analysis of radiocarbon and other cosmogenic radionuclides for archaeological, geological and environmental applications. In addition, AMS has been recently applied in biomedicine to study exposure of human tissues to chemicals and biomolecules at attomole levels. There is also a world-wide effort to analyse rare nuclides of heavier masses, such as long-lived actinides, with important applications in safeguards and nuclear waste disposal. The use of AMS is limited by the expensive accelerator technology required and there are several attempts to develop smaller and cheaper AMS spectrometers. 5 refs.

Radiation Biomarker Research Using Mass Spectrometry

National Research Council Canada - National Science Library

Bach, Stephan B; Hubert, Walter

2007-01-01

.... This review is intended to give an overview of mass spectrometry and its application to biological systems and biomarker discovery and how that might relate to relevant radiation dosimetry studies...

Inorganic trace analysis by laser ionization mass spectrometry

International Nuclear Information System (INIS)

Becker, S.; Dietze, H.J.

1991-01-01

Among the different spectrometric techniques for trace analysis Laser Ionization Mass Spectrometry (LIMS) is well established as a trace analytic method with a wide coverage. In the LIMS the sample material is evaporated and ionized by means of a focused pulsed laser beam in a laser microplasma, which is formed in the spot area of the irradiated sample. All chemical elements in the sample materials are evaporated and ionized in the laser plasma. The formed ions are separated according to mass and energy by a time-of-flight, quadrupole or double focusing mass spectrometer. In this review the characteristics and analytical features, some recent developments, and applications of laser ionization mass spectrometry in inorganic trace analysis are described. (orig.)

Laser ionization mass spectrometry in inorganic trace analysis

International Nuclear Information System (INIS)

Becker, J.S.; Dietze, H.J.

1992-01-01

Among the different spectrometric techniques for trace analysis Laser Ionization Mass Spectrometry (LIMS) is well established as a trace analytical method. With the LIMS technique the sample material is evaporated and ionized by means of a focused pulsed laser in a laser microplasma, which is formed in the spot area of the irradiated sample. All chemical elements in the sample materials are evaporated and ionized in the laser plasma. The ions formed are separated according to their mass and energy by a time-of-flight, quadrupole or double focusing mass spectrometer. In this review the characteristics and analytical features, some recent developments and applications of laser ionization mass spectrometry in inorganic trace analysis are described. (orig.)

Hands-on Electrospray Ionization-Mass Spectrometry for Upper-Level Undergraduate and Graduate Students

Science.gov (United States)

Stock, Naomi L.; March, Raymond E.

2014-01-01

Electrospray ionization-mass spectrometry (ESI-MS) is a powerful technique for the detection, identification, and quantification of organic compounds. As mass spectrometers have become more user-friendly and affordable, many students--often with little experience in mass spectrometry--find themselves needing to incorporate mass spectrometry into…

Identification of chemical components in Baidianling Capsule based on gas chromatography-mass spectrometry and high-performance liquid chromatography combined with Fourier transform ion cyclotron resonance mass spectrometry.

Science.gov (United States)

Wu, Wenying; Chen, Yu; Wang, Binjie; Sun, Xiaoyang; Guo, Ping; Chen, Xiaohui

2017-08-01

Baidianling Capsule, which is made from 16 Chinese herbs, has been widely used for treating vitiligo clinically. In this study, the sensitive and rapid method has been developed for the analysis of chemical components in Baidianling Capsule by gas chromatography-mass spectrometry in combination with retention indices and high-performance liquid chromatography combined with Fourier transform ion cyclotron resonance mass spectrometry. Firstly, a total of 110 potential volatile compounds obtained from different extraction procedures including alkanes, alkenes, alkynes, ketones, ethers, aldehydes, alcohols, phenols, organic acids, esters, furans, pyrrole, acid amides, heterocycles, and oxides were detected from Baidianling Capsule by gas chromatography-mass spectrometry, of which 75 were identified by mass spectrometry in combination with the retention index. Then, a total of 124 components were tentatively identified by high-performance liquid chromatography combined with Fourier transform ion cyclotron resonance mass spectrometry. Fifteen constituents from Baidianling Capsule were accurately identified by comparing the retention times with those of reference compounds, others were identified by comparing the retention times and mass spectrometry data, as well as retrieving the reference literature. This study provides a practical strategy for rapidly screening and identifying the multiple constituents of a complex traditional Chinese medicine. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Mass Spectrometry Applications for Toxicology.

Science.gov (United States)

Mbughuni, Michael M; Jannetto, Paul J; Langman, Loralie J

2016-12-01

Toxicology is a multidisciplinary study of poisons, aimed to correlate the quantitative and qualitative relationships between poisons and their physiological and behavioural effects in living systems. Other key aspects of toxicology focus on elucidation of the mechanisms of action of poisons and development of remedies and treatment plans for associated toxic effects. In these endeavours, Mass spectrometry (MS) has become a powerful analytical technique with a wide range of application used in the Toxicological analysis of drugs, poisons, and metabolites of both. To date, MS applications have permeated all fields of toxicology which include; environmental, clinical, and forensic toxicology. While many different analytical applications are used in these fields, MS and its hyphenated applications such as; gas chromatography MS (GC-MS), liquid chromatography MS (LC-MS), inductively coupled plasma ionization MS (ICP-MS), tandem mass spectrometry (MS/MS and MS n ) have emerged as powerful tools used in toxicology laboratories. This review will focus on these hyphenated MS technologies and their applications for toxicology.

Mass Spectrometry Applications for Toxicology

Science.gov (United States)

Mbughuni, Michael M.; Jannetto, Paul J.

2016-01-01

Toxicology is a multidisciplinary study of poisons, aimed to correlate the quantitative and qualitative relationships between poisons and their physiological and behavioural effects in living systems. Other key aspects of toxicology focus on elucidation of the mechanisms of action of poisons and development of remedies and treatment plans for associated toxic effects. In these endeavours, Mass spectrometry (MS) has become a powerful analytical technique with a wide range of application used in the Toxicological analysis of drugs, poisons, and metabolites of both. To date, MS applications have permeated all fields of toxicology which include; environmental, clinical, and forensic toxicology. While many different analytical applications are used in these fields, MS and its hyphenated applications such as; gas chromatography MS (GC-MS), liquid chromatography MS (LC-MS), inductively coupled plasma ionization MS (ICP-MS), tandem mass spectrometry (MS/MS and MSn) have emerged as powerful tools used in toxicology laboratories. This review will focus on these hyphenated MS technologies and their applications for toxicology. PMID:28149262

Identifying modifications in RNA by MALDI mass spectrometry

DEFF Research Database (Denmark)

Douthwaite, Stephen; Kirpekar, Finn

2007-01-01

as RNA modifications added in cell-free in vitro systems. MALDI-MS is particularly useful in cases in which other techniques such as those involving primer extension or chromatographic analyses are not practicable. To date, MALDI-MS has been used to localize rRNA modifications that are involved......Posttranscriptional modifications on the base or sugar of ribonucleosides generally result in mass increases that can be measured by mass spectrometry. Matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS) is a direct and accurate means of determining the masses of RNAs. Mass...... spectra produced by MALDI are relatively straightforward to interpret, because they are dominated by singly charged ions, making it possible to analyze complex mixtures of RNA oligonucleotides ranging from trinucleotides up to 20-mers. Analysis of modifications within much longer RNAs, such as ribosomal...

Enantioselectivity of mass spectrometry: challenges and promises.

Science.gov (United States)

Awad, Hanan; El-Aneed, Anas

2013-01-01

With the fast growing market of pure enantiomer drugs and bioactive molecules, new chiral-selective analytical tools have been instigated including the use of mass spectrometry (MS). Even though MS is one of the best analytical tools that has efficiently been used in several pharmaceutical and biological applications, traditionally MS is considered as a "chiral-blind" technique. This limitation is due to the MS inability to differentiate between two enantiomers of a chiral molecule based merely on their masses. Several approaches have been explored to assess the potential role of MS in chiral analysis. The first approach depends on the use of MS-hyphenated techniques utilizing fast and sensitive chiral separation tools such as liquid chromatography (LC), gas chromatography (GC), and capillary electrophoresis (CE) coupled to MS detector. More recently, several alternative separation techniques have been evaluated such as supercritical fluid chromatography (SFC) and capillary electrochromatography (CEC); the latter being a hybrid technique that combines the efficiency of CE with the selectivity of LC. The second approach is based on using the MS instrument solely for the chiral recognition. This method depends on the behavioral differences between enantiomers towards a foreign molecule and the ability of MS to monitor such differences. These behavioral differences can be divided into three types: (i) differences in the enantiomeric affinity for association with the chiral selector, (ii) differences of the enantiomeric exchange rate with a foreign reagent, and (iii) differences in the complex MS dissociation behaviors of the enantiomers. Most recently, ion mobility spectrometry was introduced to qualitatively and quantitatively evaluate chiral compounds. This article provides an overview of MS role in chiral analysis by discussing MS based methodologies and presenting the challenges and promises associated with each approach. © 2013 Wiley Periodicals, Inc.

Applications of accelerator mass spectrometry to nuclear physics and astrophysics

International Nuclear Information System (INIS)

Guo Zhiyu; Zhang Chuan

2002-01-01

As an ultra high sensitive analyzing method, accelerator mass spectrometry is playing an important role in the studies of nuclear physics and astrophysics. The accelerator mass spectrometry (AMS) applications in searching for violation of Pauli exclusion principle and study on supernovae are discussed as examples

Quantitation of Acrylamide in Foods by High-Resolution Mass Spectrometry

NARCIS (Netherlands)

Troise, A.D.; Fogliano, Vincenzo

2016-01-01

The use of liquid chromatography high-resolution mass spectrometry (LC-HRMS) and direct analysis real-time high-resolution mass spectrometry (DART-HRMS) defines a new scenario in the analysis of thermal-induced toxicants, such as acrylamide. Several factors contribute to the definition of the

Practical aspects of trapped ion mass spectrometry, 5 applications of ion trapping devices

CERN Document Server

March, Raymond E

2009-01-01

Examines ion/neutral and ion/ion reactions, ion spectroscopy, and the structural characterization of proteins and peptides using quadropole ion trap mass spectrometry, Fourier transform - ion cyclotron resonance (FT-ICR) mass spectrometry, and traveling wave ion mobility mass spectrometry.

Hydrogen/deuterium exchange in mass spectrometry.

Science.gov (United States)

Kostyukevich, Yury; Acter, Thamina; Zherebker, Alexander; Ahmed, Arif; Kim, Sunghwan; Nikolaev, Eugene

2018-03-30

The isotopic exchange approach is in use since the first observation of such reactions in 1933 by Lewis. This approach allows the investigation of the pathways of chemical and biochemical reactions, determination of structure, composition, and conformation of molecules. Mass spectrometry has now become one of the most important analytical tools for the monitoring of the isotopic exchange reactions. Investigation of conformational dynamics of proteins, quantitative measurements, obtaining chemical, and structural information about individual compounds of the complex natural mixtures are mainly based on the use of isotope exchange in combination with high resolution mass spectrometry. The most important reaction is the Hydrogen/Deuterium exchange, which is mainly performed in the solution. Recently we have developed the approach allowing performing of the Hydrogen/Deuterium reaction on-line directly in the ionization source under atmospheric pressure. Such approach simplifies the sample preparation and can accelerate the exchange reaction so that certain hydrogens that are considered as non-labile will also participate in the exchange. The use of in-ionization source H/D exchange in modern mass spectrometry for structural elucidation of molecules serves as the basic theme in this review. We will focus on the mechanisms of the isotopic exchange reactions and on the application of in-ESI, in-APCI, and in-APPI source Hydrogen/Deuterium exchange for the investigation of petroleum, natural organic matter, oligosaccharides, and proteins including protein-protein complexes. The simple scenario for adaptation of H/D exchange reactions into mass spectrometric method is also highlighted along with a couple of examples collected from previous studies. © 2018 Wiley Periodicals, Inc.

Mass spectrometry in grape and wine chemistry. Part II: The consumer protection.

Science.gov (United States)

Flamini, Riccardo; Panighel, Annarita

2006-01-01

Controls in food industry are fundamental to protect the consumer health. For products of high quality, warranty of origin and identity is required and analytical control is very important to prevent frauds. In this article, the "state of art" of mass spectrometry in enological chemistry as a consumer safety contribute is reported. Gas chromatography-mass spectrometry (GC/MS) and liquid-chromatography-mass spectrometry (LC/MS) methods have been developed to determine pesticides, ethyl carbamate, and compounds from the yeast and bacterial metabolism in wine. The presence of pesticides in wine is mainly linked to the use of dicarboxyimide fungicides on vineyard shortly before the harvest to prevent the Botrytis cinerea attack of grape. Pesticide residues are regulated at maximum residue limits in grape of low ppm levels, but significantly lower levels in wine have to be detected, and mass spectrometry offers effective and sensitive methods. Moreover, mass spectrometry represent an advantageous alternative to the radioactive-source-containing electron capture detector commonly used in GC analysis of pesticides. Analysis of ochratoxin A (OTA) in wine by LC/MS and multiple mass spectrometry (MS/MS) permits to confirm the toxin presence without the use of expensive immunoaffinity columns, or time and solvent consuming sample derivatization procedures. Inductively coupled plasma-mass spectrometry (ICP/MS) is used to control heavy metals contamination in wine, and to verify the wine origin and authenticity. Isotopic ratio-mass spectrometry (IRMS) is applied to reveal wine watering and sugar additions, and to determine the product origin and traceability.

Elucidating rhizosphere processes by mass spectrometry – A review

International Nuclear Information System (INIS)

Rugova, Ariana; Puschenreiter, Markus; Koellensperger, Gunda; Hann, Stephan

2017-01-01

The presented review discusses state-of-the-art mass spectrometric methods, which have been developed and applied for investigation of chemical processes in the soil-root interface, the so-called rhizosphere. Rhizosphere soil's physical and chemical characteristics are to a great extent influenced by a complex mixture of compounds released from plant roots, i.e. root exudates, which have a high impact on nutrient and trace element dynamics in the soil-root interface as well as on microbial activities or soil physico-chemical characteristics. Chemical characterization as well as accurate quantification of the compounds present in the rhizosphere is a major prerequisite for a better understanding of rhizosphere processes and requires the development and application of advanced sampling procedures in combination with highly selective and sensitive analytical techniques. During the last years, targeted and non-targeted mass spectrometry-based methods have emerged and their combination with specific separation methods for various elements and compounds of a wide polarity range have been successfully applied in several studies. With this review we critically discuss the work that has been conducted within the last decade in the context of rhizosphere research and elemental or molecular mass spectrometry emphasizing different separation techniques as GC, LC and CE. Moreover, selected applications such as metal detoxification or nutrient acquisition will be discussed regarding the mass spectrometric techniques applied in studies of root exudates in plant-bacteria interactions. Additionally, a more recent isotope probing technique as novel mass spectrometry based application is highlighted. - Highlights: • State-of-the-art mass spectrometry methods developed and applied in rhizosphere research are reviewed. • Elemental and molecular mass spectrometry emphasizing different separation techniques (GC, LC or CE) are discussed. • Case studies on metal detoxification and

Elucidating rhizosphere processes by mass spectrometry – A review

Energy Technology Data Exchange (ETDEWEB)

Rugova, Ariana [Division of Analytical Chemistry, Department of Chemistry, University of Natural Resources and Life Sciences-BOKU, Vienna (Austria); Puschenreiter, Markus [Department of Forest and Soil Sciences, Rhizosphere Ecology and Biogeochemistry Group, University of Natural Resources and Life Sciences-BOKU, Vienna (Austria); Koellensperger, Gunda [Institute of Analytical Chemistry, Faculty of Chemistry, University of Vienna, Vienna (Austria); Hann, Stephan, E-mail: stephan.hann@boku.ac.at [Division of Analytical Chemistry, Department of Chemistry, University of Natural Resources and Life Sciences-BOKU, Vienna (Austria)

2017-03-01

The presented review discusses state-of-the-art mass spectrometric methods, which have been developed and applied for investigation of chemical processes in the soil-root interface, the so-called rhizosphere. Rhizosphere soil's physical and chemical characteristics are to a great extent influenced by a complex mixture of compounds released from plant roots, i.e. root exudates, which have a high impact on nutrient and trace element dynamics in the soil-root interface as well as on microbial activities or soil physico-chemical characteristics. Chemical characterization as well as accurate quantification of the compounds present in the rhizosphere is a major prerequisite for a better understanding of rhizosphere processes and requires the development and application of advanced sampling procedures in combination with highly selective and sensitive analytical techniques. During the last years, targeted and non-targeted mass spectrometry-based methods have emerged and their combination with specific separation methods for various elements and compounds of a wide polarity range have been successfully applied in several studies. With this review we critically discuss the work that has been conducted within the last decade in the context of rhizosphere research and elemental or molecular mass spectrometry emphasizing different separation techniques as GC, LC and CE. Moreover, selected applications such as metal detoxification or nutrient acquisition will be discussed regarding the mass spectrometric techniques applied in studies of root exudates in plant-bacteria interactions. Additionally, a more recent isotope probing technique as novel mass spectrometry based application is highlighted. - Highlights: • State-of-the-art mass spectrometry methods developed and applied in rhizosphere research are reviewed. • Elemental and molecular mass spectrometry emphasizing different separation techniques (GC, LC or CE) are discussed. • Case studies on metal detoxification

Towards airborne nanoparticle mass spectrometry with nanomechanical string resonators

DEFF Research Database (Denmark)

Schmid, Silvan; Kurek, Maksymilian; Boisen, Anja

2013-01-01

airborne nanoparticle sensors. Recently, nanomechanical mass spectrometry was established. One of the biggest challenges of nanomechanical sensors is the low efficiency of diffusion-based sampling. We developed an inertial-based sampling method that enables the efficient sampling of airborne nanoparticles...... mode. Mass spectrometry of airborne nanoparticles requires the simultaneous operation in the first and second mode, which can be implemented in the transduction scheme of the resonator. The presented results lay the cornerstone for the realization of a portable airborne nanoparticle mass spectrometer....

Standard practice for alternate actinide calibration for inductively coupled plasma-mass spectrometry

CERN Document Server

American Society for Testing and Materials. Philadelphia

2004-01-01

1.1 This practice provides guidance for an alternate linear calibration for the determination of selected actinide isotopes in appropriately prepared aqueous solutions by Inductively Coupled Plasma-Mass Spectrometry (ICP-MS). This alternate calibration is mass bias adjusted using thorium-232 (232Th) and uranium-238 (238U) standards. One of the benefits of this standard practice is the ability to calibrate for the analysis of highly radioactive actinides using calibration standards at much lower specific activities. Environmental laboratories may find this standard practice useful if facilities are not available to handle the highly radioactive standards of the individual actinides of interest. 1.2 The instrument response for a series of determinations of known concentration of 232Th and 238U defines the mass versus response relationship. For each standard concentration, the slope of the line defined by 232Th and 238U is used to derive linear calibration curves for each mass of interest using interference equ...

Detection of sputtered molecular doubly charged anions: a comparison of secondary-ion mass spectrometry (SIMS) and accelerator mass spectrometry (AMS)

International Nuclear Information System (INIS)

Gnaser, Hubert; Golser, Robin; Kutschera, Walter; Priller, Alfred; Steier, Peter; Vockenhuber, Christof

2004-01-01

The detection of small molecular dianions by secondary-ion mass spectrometry (SIMS) and by accelerator mass spectrometry (AMS) is compared. In SIMS, the existence of these dianions can be identified safely if the total mass number of the molecule is odd and the dianion is hence detected at a half-integral mass number. The occurrence of fragmentation processes which may interfere with this scheme, is illustrated by means of the energy spectra of singly and doubly charged negative cluster ions. As compared to SIMS, AMS can rely, in addition, on the break-up of molecular species in the stripping process: this allows to monitor the simultaneous arrival of several atomic constituents with a clear energetic pattern in coincidence at the detector. This feature is exemplified for the C 10 2- dianion

The use of mass spectrometry to analyze dried blood spots.

Science.gov (United States)

Wagner, Michel; Tonoli, David; Varesio, Emmanuel; Hopfgartner, Gérard

2016-01-01

Dried blood spots (DBS) typically consist in the deposition of small volumes of capillary blood onto dedicated paper cards. Comparatively to whole blood or plasma samples, their benefits rely in the fact that sample collection is easier and that logistic aspects related to sample storage and shipment can be relatively limited, respectively, without the need of a refrigerator or dry ice. Originally, this approach has been developed in the sixties to support the analysis of phenylalanine for the detection of phenylketonuria in newborns using bacterial inhibition test. In the nineties tandem mass spectrometry was established as the detection technique for phenylalanine and tyrosine. DBS became rapidly recognized for their clinical value: they were widely implemented in pediatric settings with mass spectrometric detection, and were closely associated to the debut of newborn screening (NBS) programs, as a part of public health policies. Since then, sample collection on paper cards has been explored with various analytical techniques in other areas more or less successfully regarding large-scale applications. Moreover, in the last 5 years a regain of interest for DBS was observed and originated from the bioanalytical community to support drug development (e.g., PK studies) or therapeutic drug monitoring mainly. Those recent applications were essentially driven by improved sensitivity of triple quadrupole mass spectrometers. This review presents an overall view of all instrumental and methodological developments for DBS analysis with mass spectrometric detection, with and without separation techniques. A general introduction to DBS will describe their advantages and historical aspects of their emergence. A second section will focus on blood collection, with a strong emphasis on specific parameters that can impact quantitative analysis, including chromatographic effects, hematocrit effects, blood effects, and analyte stability. A third part of the review is dedicated to

Isotope dilution mass spectrometry as the primary method of measurement for the amount of matter. Application to cadmium determination in biological materials and comparison with instrumental neutron activation analysis

International Nuclear Information System (INIS)

Munoz, Luis; Gras, Nuri; Quejido, Alberto; Ferrada, Carlos

2001-01-01

A primary method of measurement as defined by the Consultative Committee on the Quantity of Matter (Comite Consultatif pour la Quantite de Matiere, CCQM) of the International Bureau of Weights and Measurements (Bureau International des Poids et Mesures, BIPM), is one whose measurement process is perfectly known, has valid theoretical foundations and is fully described and answers to an equation that relates what is measured with what is intended to be measured without any significant empirical correction factors. It is also a method that has insignificant systematic errors, where only magnitudes from the International System of Units (SI) are used and where, preferably, the uncertainties are small ones. They are, therefore, procedures that do not need instrumental calibration. The absolute methods of measurement allow a chain of traceability to be formed between the result obtained and the magnitude of the SI assigned to what is measured. So the results are said to be traceable to the SI. One of the methods that meets these requirements and is recognized as the primary method by the CCQM is Isotope Dilution Mass Spectrometry (IDMS). Through a project of Technical Cooperation with the International Atomic Energy Agency in the area of Chemical Metrology, the CCHEN obtained training in CIEMAT, Spain, in IDMS and its applications to the analysis of biological samples. This work describes the first experience carried out entirely in Chilean laboratories, applying IDMS to the determination of cadmium in the biological reference materials Oyster Tissue 15566-A from the NIST, United States, Dogfish Liver, DOLT-2 from the NRC-CNRC, Canada and Poplar Leaves GBW07604 from the NRCC, China. The samples were traced with an isotope enriched spike 111 Cd and then shaken to obtain the isotopic exchange. Once dissolved, the isotopic relationship 111 Cd/ 114 Cd was determined in the samples using mass spectrometry with plasma source. These results were compared with those obtained

Laser mass spectrometry for DNA sequencing, disease diagnosis, and fingerprinting

Energy Technology Data Exchange (ETDEWEB)

Winston Chen, C.H.; Taranenko, N.I.; Zhu, Y.F.; Chung, C.N.; Allman, S.L.

1997-03-01

Since laser mass spectrometry has the potential for achieving very fast DNA analysis, the authors recently applied it to DNA sequencing, DNA typing for fingerprinting, and DNA screening for disease diagnosis. Two different approaches for sequencing DNA have been successfully demonstrated. One is to sequence DNA with DNA ladders produced from Snager`s enzymatic method. The other is to do direct sequencing without DNA ladders. The need for quick DNA typing for identification purposes is critical for forensic application. The preliminary results indicate laser mass spectrometry can possibly be used for rapid DNA fingerprinting applications at a much lower cost than gel electrophoresis. Population screening for certain genetic disease can be a very efficient step to reducing medical costs through prevention. Since laser mass spectrometry can provide very fast DNA analysis, the authors applied laser mass spectrometry to disease diagnosis. Clinical samples with both base deletion and point mutation have been tested with complete success.

A mass spectrometry proteomics data management platform.

Science.gov (United States)

Sharma, Vagisha; Eng, Jimmy K; Maccoss, Michael J; Riffle, Michael

2012-09-01

Mass spectrometry-based proteomics is increasingly being used in biomedical research. These experiments typically generate a large volume of highly complex data, and the volume and complexity are only increasing with time. There exist many software pipelines for analyzing these data (each typically with its own file formats), and as technology improves, these file formats change and new formats are developed. Files produced from these myriad software programs may accumulate on hard disks or tape drives over time, with older files being rendered progressively more obsolete and unusable with each successive technical advancement and data format change. Although initiatives exist to standardize the file formats used in proteomics, they do not address the core failings of a file-based data management system: (1) files are typically poorly annotated experimentally, (2) files are "organically" distributed across laboratory file systems in an ad hoc manner, (3) files formats become obsolete, and (4) searching the data and comparing and contrasting results across separate experiments is very inefficient (if possible at all). Here we present a relational database architecture and accompanying web application dubbed Mass Spectrometry Data Platform that is designed to address the failings of the file-based mass spectrometry data management approach. The database is designed such that the output of disparate software pipelines may be imported into a core set of unified tables, with these core tables being extended to support data generated by specific pipelines. Because the data are unified, they may be queried, viewed, and compared across multiple experiments using a common web interface. Mass Spectrometry Data Platform is open source and freely available at http://code.google.com/p/msdapl/.

Transitioning from Targeted to Comprehensive Mass Spectrometry Using Genetic Algorithms.

Science.gov (United States)

Jaffe, Jacob D; Feeney, Caitlin M; Patel, Jinal; Lu, Xiaodong; Mani, D R

2016-11-01

Targeted proteomic assays are becoming increasingly popular because of their robust quantitative applications enabled by internal standardization, and they can be routinely executed on high performance mass spectrometry instrumentation. However, these assays are typically limited to 100s of analytes per experiment. Considerable time and effort are often expended in obtaining and preparing samples prior to targeted analyses. It would be highly desirable to detect and quantify 1000s of analytes in such samples using comprehensive mass spectrometry techniques (e.g., SWATH and DIA) while retaining a high degree of quantitative rigor for analytes with matched internal standards. Experimentally, it is facile to port a targeted assay to a comprehensive data acquisition technique. However, data analysis challenges arise from this strategy concerning agreement of results from the targeted and comprehensive approaches. Here, we present the use of genetic algorithms to overcome these challenges in order to configure hybrid targeted/comprehensive MS assays. The genetic algorithms are used to select precursor-to-fragment transitions that maximize the agreement in quantification between the targeted and the comprehensive methods. We find that the algorithm we used provided across-the-board improvement in the quantitative agreement between the targeted assay data and the hybrid comprehensive/targeted assay that we developed, as measured by parameters of linear models fitted to the results. We also found that the algorithm could perform at least as well as an independently-trained mass spectrometrist in accomplishing this task. We hope that this approach will be a useful tool in the development of quantitative approaches for comprehensive proteomics techniques. Graphical Abstract ᅟ.

High Resolution Mass Spectrometry of Polyfluorinated Polyether-Based Formulation

Science.gov (United States)

Dimzon, Ian Ken; Trier, Xenia; Frömel, Tobias; Helmus, Rick; Knepper, Thomas P.; de Voogt, Pim

2016-02-01

High resolution mass spectrometry (HRMS) was successfully applied to elucidate the structure of a polyfluorinated polyether (PFPE)-based formulation. The mass spectrum generated from direct injection into the MS was examined by identifying the different repeating units manually and with the aid of an instrument data processor. Highly accurate mass spectral data enabled the calculation of higher-order mass defects. The different plots of MW and the nth-order mass defects (up to n = 3) could aid in assessing the structure of the different repeating units and estimating their absolute and relative number per molecule. The three major repeating units were -C2H4O-, -C2F4O-, and -CF2O-. Tandem MS was used to identify the end groups that appeared to be phosphates, as well as the possible distribution of the repeating units. Reversed-phase HPLC separated of the polymer molecules on the basis of number of nonpolar repeating units. The elucidated structure resembles the structure in the published manufacturer technical data. This analytical approach to the characterization of a PFPE-based formulation can serve as a guide in analyzing not just other PFPE-based formulations but also other fluorinated and non-fluorinated polymers. The information from MS is essential in studying the physico-chemical properties of PFPEs and can help in assessing the risks they pose to the environment and to human health.

Probing the Composition, Assembly and Activity of Protein Molecular Machines using Native Mass Spectrometry

NARCIS (Netherlands)

van de Waterbeemd, M.J.

2017-01-01

Native mass spectrometry and mass spectrometry in general, are powerful analytical tools for studying proteins and protein complexes. Native mass spectrometry may provide accurate mass measurements of large macromolecular assemblies enabling the investigation of their composition and stoichiometry.

Focusing procedures in time-of-flight mass spectrometry

International Nuclear Information System (INIS)

Ioanoviciu, D.

2002-01-01

Time-of-flight mass spectrometry is a fast growing field due to its ability to handle very fast processes and due to its theoretically unlimited mass range. The performances of the time-of-flight mass analysers are heavily dependent on the progress in ion optics, a periodically reviewed field. In this presentation the various focusing procedures in time-of-flight mass spectrometry are reviewed. For ions of the same charge and mass flight time differences result from different potentials at the location of formation and from the initial velocity spread. There is no simultaneous space and velocity focusing in time-of-flight mass spectrometry. Space focusing of first and second order can be reached in time-of-flight mass analysers having two homogeneous electric field ion sources followed by a field free space in front of the detector. Single and double stage homogeneous electric field mirrors can focus in time ions of different energies. These different energies result when ions leaving different initial sites and arriving simultaneously to an intermediate space focus. Convenient mass dispersion can be obtained by including a mirror. Initial velocity focusing is obtained by the delayed extraction procedure in drift space and mirror time-of-flight mass analysers. Post source pulse focusing aims at the same purpose. Ion source electrodes of hyperbolic shape, operated by high voltage pulses can bring major improvements of the resolution, especially at high masses. For each focusing procedure the geometric and/or electric conditions are given as well as the aberrations allowing the mass resolution determination. The various focusing procedures are compared and a prediction of their future performances was tempted. (author)

Quantitative correlations between collision induced dissociation mass spectrometry coupled with electrospray ionization or atmospheric pressure chemical ionization mass spectrometry - Experiment and theory

Science.gov (United States)

Ivanova, Bojidarka; Spiteller, Michael

2018-04-01

The problematic that we consider in this paper treats the quantitative correlation model equations between experimental kinetic and thermodynamic parameters of coupled electrospray ionization (ESI) mass spectrometry (MS) or atmospheric pressure chemical ionization (APCI) mass spectrometry with collision induced dissociation mass spectrometry, accounting for the fact that the physical phenomena and mechanisms of ESI- and APCI-ion formation are completely different. There are described forty two fragment reactions of three analytes under independent ESI- and APCI-measurements. The developed new quantitative models allow us to study correlatively the reaction kinetics and thermodynamics using the methods of mass spectrometry, which complementary application with the methods of the quantum chemistry provide 3D structural information of the analytes. Both static and dynamic quantum chemical computations are carried out. The object of analyses are [2,3-dimethyl-4-(4-methyl-benzoyl)-2,3-di-p-tolyl-cyclobutyl]-p-tolyl-methanone (1) and the polycyclic aromatic hydrocarbons derivatives of dibenzoperylen (2) and tetrabenzo [a,c,fg,op]naphthacene (3), respectively. As far as (1) is known to be a product of [2π+2π] cycloaddition reactions of chalcone (1,3-di-p-tolyl-propenone), however producing cyclic derivatives with different stereo selectivity, so that the study provide crucial data about the capability of mass spectrometry to provide determine the stereo selectivity of the analytes. This work also first provides quantitative treatment of the relations '3D molecular/electronic structures'-'quantum chemical diffusion coefficient'-'mass spectrometric diffusion coefficient', thus extending the capability of the mass spectrometry for determination of the exact 3D structure of the analytes using independent measurements and computations of the diffusion coefficients. The determination of the experimental diffusion parameters is carried out within the 'current monitoring method

Hydrogen Exchange Mass Spectrometry

Science.gov (United States)

Mayne, Leland

2018-01-01

Hydrogen exchange (HX) methods can reveal much about the structure, energetics, and dynamics of proteins. The addition of mass spectrometry (MS) to an earlier fragmentation-separation HX analysis now extends HX studies to larger proteins at high structural resolution and can provide information not available before. This chapter discusses experimental aspects of HX labeling, especially with respect to the use of MS and the analysis of MS data. PMID:26791986

Portable Dew Point Mass Spectrometry System for Real-Time Gas and Moisture Analysis

Science.gov (United States)

Arkin, C.; Gillespie, Stacey; Ratzel, Christopher

2010-01-01

A portable instrument incorporates both mass spectrometry and dew point measurement to provide real-time, quantitative gas measurements of helium, nitrogen, oxygen, argon, and carbon dioxide, along with real-time, quantitative moisture analysis. The Portable Dew Point Mass Spectrometry (PDP-MS) system comprises a single quadrupole mass spectrometer and a high vacuum system consisting of a turbopump and a diaphragm-backing pump. A capacitive membrane dew point sensor was placed upstream of the MS, but still within the pressure-flow control pneumatic region. Pressure-flow control was achieved with an upstream precision metering valve, a capacitance diaphragm gauge, and a downstream mass flow controller. User configurable LabVIEW software was developed to provide real-time concentration data for the MS, dew point monitor, and sample delivery system pressure control, pressure and flow monitoring, and recording. The system has been designed to include in situ, NIST-traceable calibration. Certain sample tubing retains sufficient water that even if the sample is dry, the sample tube will desorb water to an amount resulting in moisture concentration errors up to 500 ppm for as long as 10 minutes. It was determined that Bev-A-Line IV was the best sample line to use. As a result of this issue, it is prudent to add a high-level humidity sensor to PDP-MS so such events can be prevented in the future.

Time‐of‐flight secondary ion mass spectrometry imaging of biological samples with delayed extraction for high mass and high spatial resolutions

Science.gov (United States)

Vanbellingen, Quentin P.; Elie, Nicolas; Eller, Michael J.; Della‐Negra, Serge; Touboul, David

2015-01-01

Rationale In Time‐of‐Flight Secondary Ion Mass Spectrometry (TOF‐SIMS), pulsed and focused primary ion beams enable mass spectrometry imaging, a method which is particularly useful to map various small molecules such as lipids at the surface of biological samples. When using TOF‐SIMS instruments, the focusing modes of the primary ion beam delivered by liquid metal ion guns can provide either a mass resolution of several thousand or a sub‐µm lateral resolution, but the combination of both is generally not possible. Methods With a TOF‐SIMS setup, a delayed extraction applied to secondary ions has been studied extensively on rat cerebellum sections in order to compensate for the effect of long primary ion bunches. Results The use of a delayed extraction has been proven to be an efficient solution leading to unique features, i.e. a mass resolution up to 10000 at m/z 385.4 combined with a lateral resolution of about 400 nm. Simulations of ion trajectories confirm the experimental determination of optimal delayed extraction and allow understanding of the behavior of ions as a function of their mass‐to‐charge ratio. Conclusions Although the use of a delayed extraction has been well known for many years and is very popular in MALDI, it is much less used in TOF‐SIMS. Its full characterization now enables secondary ion images to be recorded in a single run with a submicron spatial resolution and with a mass resolution of several thousand. This improvement is very useful when analyzing lipids on tissue sections, or rare, precious, or very small size samples. © 2015 The Authors. Rapid Communications in Mass Spectrometry published by John Wiley & Sons Ltd. PMID:26395603

Mass spectrometry applied to high temperature chemistry, (2)

International Nuclear Information System (INIS)

Asano, Mitsuru; Kato, Eiichi; Sata, Toshiyuki.

1980-01-01

The application of mass spectrometry to high temperature chemistry is reviewed. As a blanket material for fusion reactors, the behavior of lithium has been investigated by using mass analysers. The enthalpies of the chemical reactions of metallic lithium were obtained. The enthalpies of isomolecular exchange reactions and the derived atomization energies of LiD, Li 2 D and Li 2 D 2 were also obtained by mass spectrometry. The thermomechanical character of lithium oxide was studied. The vaporization behaviors of LiCrO 2 and Li 5 FeO 4 were studied with a quadrupole mass analyser. The vaporization of cobalt from nickel alloy was studied. The evaporated ions were analysed with a mass analyser. The measurement of the vaporized molecules of metals and fused silicate was made by mass spectrometry. The activities of Fe-V system were determined by measuring the ion current ratio. The activities of Fe-V-Cr system were also obtained. The vapor pressure of phosphor from Fe-P alloys can be measured. The activity coefficients and interaction parameters for the dilute solutions of elements, such as Mn, Al, Cu, Cr, Co, Ni, Si, Ti, V, B, Zr, Mo, C, S, and P, dissolved in liquid iron are shown in a table. The activities of NaCl-KCl system were derived by measuring the ion current ratio and by monomer-dimer method. (Kato, T.)

Time of flight secondary ion mass spectrometry: A powerful high throughput screening tool

International Nuclear Information System (INIS)

Smentkowski, Vincent S.; Ostrowski, Sara G.

2007-01-01

Combinatorial materials libraries are becoming more complicated; successful screening of these libraries requires the development of new high throughput screening methodologies. Time of flight secondary ion mass spectrometry (ToF-SIMS) is a surface analytical technique that is able to detect and image all elements (including hydrogen which is problematic for many other analysis instruments) and molecular fragments, with high mass resolution, during a single measurement. Commercial ToF-SIMS instruments can image 500 μm areas by rastering the primary ion beam over the region of interest. In this work, we will show that large area analysis can be performed, in one single measurement, by rastering the sample under the ion beam. We show that an entire 70 mm diameter wafer can be imaged in less than 90 min using ToF-SIMS stage (macro)rastering techniques. ToF-SIMS data sets contain a wealth of information since an entire high mass resolution mass spectrum is saved at each pixel in an ion image. Multivariate statistical analysis (MVSA) tools are being used in the ToF-SIMS community to assist with data interpretation; we will demonstrate that MVSA tools provide details that were not obtained using manual (univariate) analysis

Easy instrumental analysis

International Nuclear Information System (INIS)

Ko, Myeong Su; Kim, Tae Hwa; Park, Gyu Hyeon; Yang, Jong Beom; Oh, Chang Hwan; Lee, Kyoung Hye

2010-04-01

This textbook describes instrument analysis in easy way with twelve chapters. The contents of the book are pH measurement on principle, pH meter, pH measurement, examples of the experiments, centrifugation, Absorptiometry, Fluorescent method, Atomic absorption analysis, Gas-chromatography, Gas chromatography-mass spectrometry, High performance liquid chromatography liquid chromatograph-mass spectrometry, Electrophoresis on practical case and analysis of the result and examples, PCR on principle, device, application and examples and Enzyme-linked immunosorbent assay with indirect ELISA, sandwich ELISA and ELISA reader.

Easy instrumental analysis

Energy Technology Data Exchange (ETDEWEB)

Ko, Myeong Su; Kim, Tae Hwa; Park, Gyu Hyeon; Yang, Jong Beom; Oh, Chang Hwan; Lee, Kyoung Hye

2010-04-15

This textbook describes instrument analysis in easy way with twelve chapters. The contents of the book are pH measurement on principle, pH meter, pH measurement, examples of the experiments, centrifugation, Absorptiometry, Fluorescent method, Atomic absorption analysis, Gas-chromatography, Gas chromatography-mass spectrometry, High performance liquid chromatography liquid chromatograph-mass spectrometry, Electrophoresis on practical case and analysis of the result and examples, PCR on principle, device, application and examples and Enzyme-linked immunosorbent assay with indirect ELISA, sandwich ELISA and ELISA reader.

Identification of keratinocyte specific markers using phage display and mass spectrometry

DEFF Research Database (Denmark)

Jensen, K.B.; Jensen, O.N.; Ravn, P.

2003-01-01

and mass spectrometry that allows identification of cell type-specific protein markers. The most important features of the method are (i) reduction of experimental noise originating from background binding of phage particles and (ii) isolation of affinity binders after a single round of selection, which...... antigens were subsequently identified by mass spectrometry as laminin-5, plectin, and fibronectin. The combination of phage display technology with mass spectrometry methods for protein identification is a general and promising approach for proteomic analysis of cell surface complexity....

Mass spectrometry of large molecules

International Nuclear Information System (INIS)

Facchetti, S.

1985-01-01

The lectures in this volume were given at a course on mass spectrometry of large molecules, organized within the framework of the Training and Education programme of the Joint Research Centre of the European Communities. Although first presented in 1983, most of the lectures have since been updated by their authors. (orig.)

Methods for recalibration of mass spectrometry data

Science.gov (United States)

Tolmachev, Aleksey V [Richland, WA; Smith, Richard D [Richland, WA

2009-03-03

Disclosed are methods for recalibrating mass spectrometry data that provide improvement in both mass accuracy and precision by adjusting for experimental variance in parameters that have a substantial impact on mass measurement accuracy. Optimal coefficients are determined using correlated pairs of mass values compiled by matching sets of measured and putative mass values that minimize overall effective mass error and mass error spread. Coefficients are subsequently used to correct mass values for peaks detected in the measured dataset, providing recalibration thereof. Sub-ppm mass measurement accuracy has been demonstrated on a complex fungal proteome after recalibration, providing improved confidence for peptide identifications.

Probabilistic consensus scoring improves tandem mass spectrometry peptide identification.

Science.gov (United States)

Nahnsen, Sven; Bertsch, Andreas; Rahnenführer, Jörg; Nordheim, Alfred; Kohlbacher, Oliver

2011-08-05

Database search is a standard technique for identifying peptides from their tandem mass spectra. To increase the number of correctly identified peptides, we suggest a probabilistic framework that allows the combination of scores from different search engines into a joint consensus score. Central to the approach is a novel method to estimate scores for peptides not found by an individual search engine. This approach allows the estimation of p-values for each candidate peptide and their combination across all search engines. The consensus approach works better than any single search engine across all different instrument types considered in this study. Improvements vary strongly from platform to platform and from search engine to search engine. Compared to the industry standard MASCOT, our approach can identify up to 60% more peptides. The software for consensus predictions is implemented in C++ as part of OpenMS, a software framework for mass spectrometry. The source code is available in the current development version of OpenMS and can easily be used as a command line application or via a graphical pipeline designer TOPPAS.

Gas Chromatography and Mass Spectrometry Measurements and Protocols for Database and Library Development Relating to Organic Species in Support of the Mars Science Laboratory

Science.gov (United States)

Misra, P.; Garcia, R.; Mahaffy, P. R.

2010-04-01

An organic contaminant database and library has been developed for use with the Sample Analysis at Mars (SAM) instrumentation utilizing laboratory-based Gas Chromatography-Mass Spectrometry measurements of pyrolyzed and baked material samples.

Parsimonious Charge Deconvolution for Native Mass Spectrometry

Science.gov (United States)

2018-01-01

Charge deconvolution infers the mass from mass over charge (m/z) measurements in electrospray ionization mass spectra. When applied over a wide input m/z or broad target mass range, charge-deconvolution algorithms can produce artifacts, such as false masses at one-half or one-third of the correct mass. Indeed, a maximum entropy term in the objective function of MaxEnt, the most commonly used charge deconvolution algorithm, favors a deconvolved spectrum with many peaks over one with fewer peaks. Here we describe a new “parsimonious” charge deconvolution algorithm that produces fewer artifacts. The algorithm is especially well-suited to high-resolution native mass spectrometry of intact glycoproteins and protein complexes. Deconvolution of native mass spectra poses special challenges due to salt and small molecule adducts, multimers, wide mass ranges, and fewer and lower charge states. We demonstrate the performance of the new deconvolution algorithm on a range of samples. On the heavily glycosylated plasma properdin glycoprotein, the new algorithm could deconvolve monomer and dimer simultaneously and, when focused on the m/z range of the monomer, gave accurate and interpretable masses for glycoforms that had previously been analyzed manually using m/z peaks rather than deconvolved masses. On therapeutic antibodies, the new algorithm facilitated the analysis of extensions, truncations, and Fab glycosylation. The algorithm facilitates the use of native mass spectrometry for the qualitative and quantitative analysis of protein and protein assemblies. PMID:29376659

Field Sample Preparation Method Development for Isotope Ratio Mass Spectrometry

International Nuclear Information System (INIS)

Leibman, C.; Weisbrod, K.; Yoshida, T.

2015-01-01

Non-proliferation and International Security (NA-241) established a working group of researchers from Los Alamos National Laboratory (LANL), Pacific Northwest National Laboratory (PNNL) and Savannah River National Laboratory (SRNL) to evaluate the utilization of in-field mass spectrometry for safeguards applications. The survey of commercial off-the-shelf (COTS) mass spectrometers (MS) revealed no instrumentation existed capable of meeting all the potential safeguards requirements for performance, portability, and ease of use. Additionally, fieldable instruments are unlikely to meet the International Target Values (ITVs) for accuracy and precision for isotope ratio measurements achieved with laboratory methods. The major gaps identified for in-field actinide isotope ratio analysis were in the areas of: 1. sample preparation and/or sample introduction, 2. size reduction of mass analyzers and ionization sources, 3. system automation, and 4. decreased system cost. Development work in 2 through 4, numerated above continues, in the private and public sector. LANL is focusing on developing sample preparation/sample introduction methods for use with the different sample types anticipated for safeguard applications. Addressing sample handling and sample preparation methods for MS analysis will enable use of new MS instrumentation as it becomes commercially available. As one example, we have developed a rapid, sample preparation method for dissolution of uranium and plutonium oxides using ammonium bifluoride (ABF). ABF is a significantly safer and faster alternative to digestion with boiling combinations of highly concentrated mineral acids. Actinides digested with ABF yield fluorides, which can then be analyzed directly or chemically converted and separated using established column chromatography techniques as needed prior to isotope analysis. The reagent volumes and the sample processing steps associated with ABF sample digestion lend themselves to automation and field

Method optimization and quality assurance in speciation analysis using high performance liquid chromatography with detection by inductively coupled plasma mass spectrometry

DEFF Research Database (Denmark)

Larsen, Erik Huusfeldt

1998-01-01

Achievement of optimum selectivity, sensitivity and robustness in speciation analysis using high performance liquid chromatography (HPLC) with inductively coupled mass spectrometry (ICP-MS) detection requires that each instrumental component is selected and optimized with a view to the ideal....... The optimized anion and cation exchange HPLC-ICP-MS systems were used for arsenic speciation in contaminated ground water and in an in-house shrimp reference sample. For the purpose of verification, HPLC coupled with tandem mass spectrometry with electrospray ionization was additionally used for arsenic...... a mass balance of the analytes in each fraction of the extraction procedure, by recovery of spikes and by employing and comparing independent techniques. The urgent need for reference materials certified for elemental species is stressed....

Nanostructure-initiator mass spectrometry biometrics

Science.gov (United States)

Leclerc, Marion; Bowen, Benjamin; Northen, Trent

2015-09-08

Several embodiments described herein are drawn to methods of identifying an analyte on a subject's skin, methods of generating a fingerprint, methods of determining a physiological change in a subject, methods of diagnosing health status of a subject, and assay systems for detecting an analyte and generating a fingerprint, by nanostructure-initiator mass spectrometry (NIMS).

Functional genomics by mass spectrometry

DEFF Research Database (Denmark)

Andersen, Jens S.; Mann, M

2000-01-01

Systematic analysis of the function of genes can take place at the oligonucleotide or protein level. The latter has the advantage of being closest to function, since it is proteins that perform most of the reactions necessary for the cell. For most protein based ('proteomic') approaches to gene f...... numbers of intact proteins by mass spectrometry directly. Examples from this laboratory illustrate biological problem solving by modern mass spectrometric techniques. These include the analysis of the structure and function of the nucleolus and the analysis of signaling complexes....

Determination of ultra-low levels of uranium using resonance ionization mass spectrometry

International Nuclear Information System (INIS)

Kiran Kumar, P.V.; Acharyulu, G.V.S.G.

2015-01-01

The determination of isotopic composition of actinides like U and Pu is important, due to their distribution in the environment as a result of nuclear weapons testing, fuel reprocessing, reactor operations and to a smaller extent from accidental releases. The analytical methods like fission track analysis (FTA), thermal ionization mass spectrometry (TIMS), inductively coupled plasma mass spectrometry (ICPMS) and resonance ionization mass spectrometry (RIMS) have evolved as sensitive techniques. Resonance Ionization Mass Spectrometry yields rapid isotopic signature data for material containing actinides without requiring time-consuming sample preparation and chemical separation procedures. In this paper, authors presented the details of the methodology and results for low-level detection of uranium using RIMS

Optimization Of A Mass Spectrometry Process

International Nuclear Information System (INIS)

Lopes, Jose; Alegria, F. Correa; Redondo, Luis; Barradas, N. P.; Alves, E.; Rocha, Jorge

2011-01-01

In this paper we present and discuss a system developed in order to optimize the mass spectrometry process of an ion implanter. The system uses a PC to control and display the mass spectrum. The operator interacts with the I/O board, that interfaces with the computer and the ion implanter by a LabVIEW code. Experimental results are shown and the capabilities of the system are discussed.

New simultaneous thermogravimetry and modulated molecular beam mass spectrometry apparatus for quantitative thermal decomposition studies

International Nuclear Information System (INIS)

Behrens, R. Jr.

1987-01-01

A new type of instrument has been designed and constructed to measure quantitatively the gas phase species evolving during thermal decompositions. These measurements can be used for understanding the kinetics of thermal decomposition, determining the heats of formation and vaporization of high-temperature materials, and analyzing sample contaminants. The new design allows measurements to be made on the same time scale as the rates of the reactions being studied, provides a universal detection technique to study a wide range of compounds, gives quantitative measurements of decomposition products, and minimizes interference from the instrument on the measurements. The instrument design is based on a unique combination of thermogravimetric analysis (TGA), differential thermal analysis (DTA), and modulated beam mass spectroscopy (MBMS) which are brought together into a symbiotic relationship through the use of differentially pumped vacuum systems, modulated molecular beam techniques, and computer control and data-acquisition systems. A data analysis technique that calculates partial pressures in the reaction cell from the simultaneous microbalance force measurements and the modulated mass spectrometry measurements has been developed. This eliminates the need to know the ionization cross section, the ion dissociation channels, the quadrupole transmission, and the ion detector sensitivity for each thermal decomposition product prior to quantifying the mass spectral data. The operation of the instrument and the data analysis technique are illustrated with the thermal decomposition of contaminants from a precipitated palladium powder

Paradigms in isotope dilution mass spectrometry for elemental speciation analysis

International Nuclear Information System (INIS)

Meija, Juris; Mester, Zoltan

2008-01-01

Isotope dilution mass spectrometry currently stands out as the method providing results with unchallenged precision and accuracy in elemental speciation. However, recent history of isotope dilution mass spectrometry has shown that the extent to which this primary ratio measurement method can deliver accurate results is still subject of active research. In this review, we will summarize the fundamental prerequisites behind isotope dilution mass spectrometry and discuss their practical limits of validity and effects on the accuracy of the obtained results. This review is not to be viewed as a critique of isotope dilution; rather its purpose is to highlight the lesser studied aspects that will ensure and elevate current supremacy of the results obtained from this method

Introduction of organic/hydro-organic matrices in inductively coupled plasma optical emission spectrometry and mass spectrometry: a tutorial review. Part II. Practical considerations.

Science.gov (United States)

Leclercq, Amélie; Nonell, Anthony; Todolí Torró, José Luis; Bresson, Carole; Vio, Laurent; Vercouter, Thomas; Chartier, Frédéric

2015-07-23

Inductively coupled plasma optical emission spectrometry (ICP-OES) and mass spectrometry (ICP-MS) are increasingly used to carry out analyses in organic/hydro-organic matrices. The introduction of such matrices into ICP sources is particularly challenging and can be the cause of numerous drawbacks. This tutorial review, divided in two parts, explores the rich literature related to the introduction of organic/hydro-organic matrices in ICP sources. Part I provided theoretical considerations associated with the physico-chemical properties of such matrices, in an attempt to understand the induced phenomena. Part II of this tutorial review is dedicated to more practical considerations on instrumentation, instrumental and operating parameters, as well as analytical strategies for elemental quantification in such matrices. Two important issues are addressed in this part: the first concerns the instrumentation and optimization of instrumental and operating parameters, pointing out (i) the description, benefits and drawbacks of different kinds of nebulization and desolvation devices and the impact of more specific instrumental parameters such as the injector characteristics and the material used for the cone; and, (ii) the optimization of operating parameters, for both ICP-OES and ICP-MS. Even if it is at the margin of this tutorial review, Electrothermal Vaporization and Laser Ablation will also be shortly described. The second issue is devoted to the analytical strategies for elemental quantification in such matrices, with particular insight into the isotope dilution technique, particularly used in speciation analysis by ICP-coupled separation techniques. Copyright © 2015 Elsevier B.V. All rights reserved.

Fast and Efficient XML Data Access for Next-Generation Mass Spectrometry.

Science.gov (United States)

Röst, Hannes L; Schmitt, Uwe; Aebersold, Ruedi; Malmström, Lars

2015-01-01

In mass spectrometry-based proteomics, XML formats such as mzML and mzXML provide an open and standardized way to store and exchange the raw data (spectra and chromatograms) of mass spectrometric experiments. These file formats are being used by a multitude of open-source and cross-platform tools which allow the proteomics community to access algorithms in a vendor-independent fashion and perform transparent and reproducible data analysis. Recent improvements in mass spectrometry instrumentation have increased the data size produced in a single LC-MS/MS measurement and put substantial strain on open-source tools, particularly those that are not equipped to deal with XML data files that reach dozens of gigabytes in size. Here we present a fast and versatile parsing library for mass spectrometric XML formats available in C++ and Python, based on the mature OpenMS software framework. Our library implements an API for obtaining spectra and chromatograms under memory constraints using random access or sequential access functions, allowing users to process datasets that are much larger than system memory. For fast access to the raw data structures, small XML files can also be completely loaded into memory. In addition, we have improved the parsing speed of the core mzML module by over 4-fold (compared to OpenMS 1.11), making our library suitable for a wide variety of algorithms that need fast access to dozens of gigabytes of raw mass spectrometric data. Our C++ and Python implementations are available for the Linux, Mac, and Windows operating systems. All proposed modifications to the OpenMS code have been merged into the OpenMS mainline codebase and are available to the community at https://github.com/OpenMS/OpenMS.

Fast and Efficient XML Data Access for Next-Generation Mass Spectrometry.

Directory of Open Access Journals (Sweden)

Hannes L Röst

Full Text Available In mass spectrometry-based proteomics, XML formats such as mzML and mzXML provide an open and standardized way to store and exchange the raw data (spectra and chromatograms of mass spectrometric experiments. These file formats are being used by a multitude of open-source and cross-platform tools which allow the proteomics community to access algorithms in a vendor-independent fashion and perform transparent and reproducible data analysis. Recent improvements in mass spectrometry instrumentation have increased the data size produced in a single LC-MS/MS measurement and put substantial strain on open-source tools, particularly those that are not equipped to deal with XML data files that reach dozens of gigabytes in size.Here we present a fast and versatile parsing library for mass spectrometric XML formats available in C++ and Python, based on the mature OpenMS software framework. Our library implements an API for obtaining spectra and chromatograms under memory constraints using random access or sequential access functions, allowing users to process datasets that are much larger than system memory. For fast access to the raw data structures, small XML files can also be completely loaded into memory. In addition, we have improved the parsing speed of the core mzML module by over 4-fold (compared to OpenMS 1.11, making our library suitable for a wide variety of algorithms that need fast access to dozens of gigabytes of raw mass spectrometric data.Our C++ and Python implementations are available for the Linux, Mac, and Windows operating systems. All proposed modifications to the OpenMS code have been merged into the OpenMS mainline codebase and are available to the community at https://github.com/OpenMS/OpenMS.

Detection of trace organics in Mars analog samples containing perchlorate by laser desorption/ionization mass spectrometry.

Science.gov (United States)

Li, Xiang; Danell, Ryan M; Brinckerhoff, William B; Pinnick, Veronica T; van Amerom, Friso; Arevalo, Ricardo D; Getty, Stephanie A; Mahaffy, Paul R; Steininger, Harald; Goesmann, Fred

2015-02-01

Evidence from recent Mars missions indicates the presence of perchlorate salts up to 1 wt % level in the near-surface materials. Mixed perchlorates and other oxychlorine species may complicate the detection of organic molecules in bulk martian samples when using pyrolysis techniques. To address this analytical challenge, we report here results of laboratory measurements with laser desorption mass spectrometry, including analyses performed on both commercial and Mars Organic Molecule Analyzer (MOMA) breadboard instruments. We demonstrate that the detection of nonvolatile organics in selected spiked mineral-matrix materials by laser desorption/ionization (LDI) mass spectrometry is not inhibited by the presence of up to 1 wt % perchlorate salt. The organics in the sample are not significantly degraded or combusted in the LDI process, and the parent molecular ion is retained in the mass spectrum. The LDI technique provides distinct potential benefits for the detection of organics in situ on the martian surface and has the potential to aid in the search for signs of life on Mars.

Incorporating Biological Mass Spectrometry into Undergraduate Teaching Labs, Part 2: Peptide Identification via Molecular Mass Determination

Science.gov (United States)

Arnquist, Isaac J.; Beussman, Douglas J.

2009-01-01

Mass spectrometry has become a routine analytical tool in the undergraduate curriculum in the form of GC-MS. While relatively few undergraduate programs have incorporated biological mass spectrometry into their programs, the importance of these techniques, as demonstrated by their recognition with the 2002 Nobel Prize, will hopefully lead to…

Multidimensional chromatography coupled to mass spectrometry in analysing complex proteomics samples

NARCIS (Netherlands)

Horvatovich, Peter; Hoekman, Berend; Govorukhina, Natalia; Bischoff, Rainer

Multidimensional chromatography coupled to mass spectrometry (LC(n)-MS) provides more separation power and an extended measured dynamic concentration range to analyse complex proteomics samples than one dimensional liquid chromatography coupled to mass spectrometry (1D-LC-MS). This review gives an

High-Performance Liquid Chromatography-Mass Spectrometry.

Science.gov (United States)

Vestal, Marvin L.

1984-01-01

Reviews techniques for online coupling of high-performance liquid chromatography with mass spectrometry, emphasizing those suitable for application to nonvolatile samples. Also summarizes the present status, strengths, and weaknesses of various techniques and discusses potential applications of recently developed techniques for combined liquid…

Symposium on fast atom and ion induced mass spectrometry of nonvolatile organic solids

International Nuclear Information System (INIS)

McNeal, C.J.

1982-01-01

The mechanisms of molecular and fragment ion production and the various parameters affecting ion yields were discussed by 6 invited speakers from Europe, Canada, and the US at this symposium. The work reported was almost equally divided between that using low-energy (keV) primary ion (or atom) beams, e.g. fast atom bombardment mass spectrometry (FABMS) and secondary ion mass spectrometry (SIMS) and that using high energy (MeV) particles, e.g. heavy ion induced mass spectrometry (HIIDMS) and 252 Cf-plasma desorption mass spectrometry ( 252 Cf-PDMS). Both theoretical foundations and observed experimental results for both techniques are included

Laser microprobe mass spectrometry: Potential and limitations for inorganic and organic micro-analysis. Pt. 1

International Nuclear Information System (INIS)

Vaeck, I. van; Gijbels, R.

1990-01-01

Laser microprobe mass spectrometry (LMMS) employs a highly focused UV laser beam to ionise a microvolume in the order of 1 μm 3 . The ions produced are then mass-separated in a time-of-flight (TOF) or a Fourier Transform (FT) mass spectrometer. TOF LMMS allows element localisation, detailed speciation of inorganic substances and structural information of organic molecules. Quantitation is difficult. This paper focuses on instrumental aspects and inorganic analysis. Organic applications are treated in part II of this series. Selected examples illustrate that TOF LMMS is a valuable tool for the qualitative characterisation of micro-samples. Also, the applicability to the analysis with high spatial resolution is shown. The current technology and the prospects from the recent FTMS development are discussed. (orig.)

Subcellular analysis by laser ablation electrospray ionization mass spectrometry

Science.gov (United States)

Vertes, Akos; Stolee, Jessica A; Shrestha, Bindesh

2014-12-02

In various embodiments, a method of laser ablation electrospray ionization mass spectrometry (LAESI-MS) may generally comprise micro-dissecting a cell comprising at least one of a cell wall and a cell membrane to expose at least one subcellular component therein, ablating the at least one subcellular component by an infrared laser pulse to form an ablation plume, intercepting the ablation plume by an electrospray plume to form ions, and detecting the ions by mass spectrometry.

Mass spectrometry in identification of ecotoxicants including chemical and biological warfare agents

International Nuclear Information System (INIS)

Lebedev, Albert T.

2005-01-01

Mass spectrometry is a unique tool to detect and identify trace levels of organic and bioorganic compounds as well as microorganisms in the environment. The range of potential chemical warfare (CW) and biological warfare (BW) agents is very broad. An important advantage of mass spectrometry over other techniques involves potential for full spectrum detection of chemical and biological agents including mid-spectrum materials (i.e. bioactive peptides, toxins, etc.) for which biological approaches are inadequate. Being very fast (seconds and minutes), extremely sensitive (zeptomoles 10 -21 ), and informative (detailed qualitative and quantitative composition of mixtures containing hundreds of chemicals), mass spectrometry is a principal analytical tool at the sites of destruction of CW. Due to its unique features, mass spectrometry is applied not only for the detection of CW agents, but for the analysis of products of metabolism and degradation of these agents in organisms or environment as well. The present paper deals with some examples of successful application of mass spectrometry for the analyses of ecotoxicants, chemical warfare agents, explosives, and microorganisms including biology warfare agents

Interpretation of Tandem Mass Spectrometry (MSMS) Spectra for Peptide Analysis

DEFF Research Database (Denmark)

Hjernø, Karin; Højrup, Peter

2015-01-01

The aim of this chapter is to give a short introduction to peptide analysis by mass spectrometry (MS) and interpretation of fragment mass spectra. Through examples and guidelines we demonstrate how to understand and validate search results and how to perform de novo sequencing based on the often...... very complex fragmentation pattern obtained by tandem mass spectrometry (also referred to as MSMS). The focus is on simple rules for interpretation of MSMS spectra of tryptic as well as non-tryptic peptides....

Plutonium determination in urine by techniques of mass spectrometry

International Nuclear Information System (INIS)

Hernandez M, H.; Yllera de Ll, A.

2013-10-01

The objective of this study was to develop an analytic method for quantification and plutonium reappraisal in plane tables of alpha spectrometry be means of the mass spectrometry technique of high resolution with plasma source inductively coupled and desolvator Aridus (Aridus-Hr-Icp-Ms) and mass spectrometry with accelerator (AMS). The obtained results were, the recovery percentage of Pu in the plane table was of ∼ 90% and activity minimum detectable obtained with Aridus-Hr-Icp-Ms and AMS was of ∼ 3 and ∼ 0.4 f g of 239 Pu, respectively. Conclusion, the results demonstrate the aptitude of the Aridus-Hr-Icp-Ms and AMS techniques in the Pu reappraisal in plane tables with bigger speed and precision, improving the values notably of the activity minimum detectable that can be obtained with the alpha spectrometry (∼ 50 f g of 239 Pu). (author)

Present and future prospects of accelerator mass spectrometry

International Nuclear Information System (INIS)

Kutschera, W.

1987-04-01

Accelerator Mass Spectrometry (AMS) has become a powerful technique for measuring extremely low abundances (10 -10 to 10 -15 relative to stable isotopes) of long-lived radioisotopes with half-lives in the range from 10 2 to 10 8 years. With a few exceptions, tandem accelerators turned out to be the most useful instruments for AMS measurements. Both natural (mostly cosmogenic) and man-made (anthropogenic) radioisotopes are studied with this technique. In some cases very low concentrations of stable isotope are also measured. Applications of AMS cover a large variety of fields including anthropology, archaeology, oceanography, hydrology, climatology, volcanology, minerals exploration, cosmochemistry, meteoritics, glaciology, sedimentary processes, geochronology, environmental physics, astrophysics, nuclear and particle physics. Present and future prospects of AMS are discussed as an interplay between the continuous development of new techniques and the investigation of problems in the above mentioned fields. Typical factors to be considered are energy range and type of accelerator, and the possibilities of dedicated versus partial use of new or existing accelerators

Determination of total uranium by mass spectrometry utilizing the isotopic dilution technique

International Nuclear Information System (INIS)

Cretella, R.F.; Noutary, C.J.; Servant, R.E.

1981-01-01

The isotopic dilution associated to mass spectrometry is a high-sensitivity technique that allows to work with microquantities of the sample, making it possible to analize the content in highly radioactive solutions with excellent accuracy and minimum risk. The proposed technique is described and its results are discussed through the analysis of: 1) A synthetic sample that simulates dissolved spent fuel elements; 2) Uranium dioxide of nuclear purity and 3) Uranium concentrate. 233 U(ORNL) was employed as a tracer and a Nuclide 12-90-SU mass spectrometer of simple magnetic focus as measurement instrument. The accuracy reached in the analyses is better than 0.5% with a reliability of 95%. The analysis of the errors shows that their main contributing source are the errors in the measurement of the isotopic ratios. (M.E.L.) [es

Surface ionization mass spectrometry of opiates

International Nuclear Information System (INIS)

Usmanov, D.T.

2009-07-01

Key words: surface ionization, adsorption, heterogeneous reactions, surface ionization mass spectrometry, thermodesorption surface ionization spectroscopy, thermoemitter, opiates, extracts of biosamples. Subjects of study. The mass - spectrometric study of thermal - ion emission: surface ionization of opiates by on the surface of oxidized refractory metals. Purpose of work is to establish the regularities of surface ionization (SI) of multi-atomic molecule opiates and their mixtures develop the scientific base of SI methods for high sensitive and selective detection and analysis of these substances in the different objects, including biosamples. Methods of study: surface ionization mass spectrometry, thermodesorption surface ionization spectroscopy. The results obtained and their novelty. For the first time, SI of molecule opiates on the oxidized tungsten surface has been studied and their SI mass-spectra and temperature dependences of ion currents have been obtained, the characteristic heterogeneous reactions of an adsorbed molecules and the channels of monomolecular decays vibrationally-excited ions on their way in mass-spectrometry have been revealed, sublimation energy has been defined, the activation energy of E act , of these decays has been estimated for given period of time. Additivity of the SI mass-spectra of opiate mixtures of has been established under conditions of joint opiate adsorption. High selectivity of SI allows the extracts of biosamples to be analyzed without their preliminary chromatographic separation. The opiates are ionized by SI with high efficiency (from 34 C/mol to 112 C/mol), which provides high sensitivity of opiate detection by SI/MS and APTDSIS methods from - 10 -11 g in the samples under analysis. Practical value. The results of these studies create the scientific base for novel SI methods of high sensitive detection and analysis of the trace amounts of opiates in complicated mixtures, including biosamples without their preliminary

Quantitating subcellular metabolism with multi-isotope imaging mass spectrometry

OpenAIRE

Steinhauser, Matthew L.; Bailey, Andrew; Senyo, Samuel E.; Guillermier, Christelle; Perlstein, Todd S.; Gould, Alex P.; Lee, Richard T.; Lechene, Claude P.

2012-01-01

Mass spectrometry with stable isotope labels has been seminal in discovering the dynamic state of living matter 1,2 but is limited to bulk tissues or cells. We developed multi-isotope imaging mass spectrometry (MIMS) that allowed us to view and measure stable isotope incorporation with sub-micron resolution 3,4 . Here we apply MIMS to diverse organisms, including Drosophila, mice, and humans. We test the “immortal strand hypothesis,” which predicts that during asymmetric stem cell division ch...

Analysis of chirality by femtosecond laser ionization mass spectrometry.

Science.gov (United States)

Horsch, Philipp; Urbasch, Gunter; Weitzel, Karl-Michael

2012-09-01

Recent progress in the field of chirality analysis employing laser ionization mass spectrometry is reviewed. Emphasis is given to femtosecond (fs) laser ionization work from the author's group. We begin by reviewing fundamental aspects of determining circular dichroism (CD) in fs-laser ionization mass spectrometry (fs-LIMS) discussing an example from the literature (resonant fs-LIMS of 3-methylcyclopentanone). Second, we present new data indicating CD in non-resonant fs-LIMS of propylene oxide. Copyright © 2012 Wiley Periodicals, Inc., A Wiley Company.

From whole-body sections down to cellular level, multiscale imaging of phospholipids by MALDI mass spectrometry.

Science.gov (United States)

Chaurand, Pierre; Cornett, Dale S; Angel, Peggi M; Caprioli, Richard M

2011-02-01

Significant progress in instrumentation and sample preparation approaches have recently expanded the potential of MALDI imaging mass spectrometry to the analysis of phospholipids and other endogenous metabolites naturally occurring in tissue specimens. Here we explore some of the requirements necessary for the successful analysis and imaging of phospholipids from thin tissue sections of various dimensions by MALDI time-of-flight mass spectrometry. We address methodology issues relative to the imaging of whole-body sections such as those cut from model laboratory animals, sections of intermediate dimensions typically prepared from individual organs, as well as the requirements for imaging areas of interests from these sections at a cellular scale spatial resolution. We also review existing limitations of MALDI imaging MS technology relative to compound identification. Finally, we conclude with a perspective on important issues relative to data exploitation and management that need to be solved to maximize biological understanding of the tissue specimen investigated.

Mass Spectrometry Market: Value chain and stakeholder analysis up to 2024

OpenAIRE

Smita Deshmukh

2016-01-01

Transparency Market Research Reports incorporated a definite business overview and investigation inclines on "Mass Spectrometry Market". This report likewise incorporates more illumination about fundamental review of the business including definitions, requisitions and worldwide business sector industry structure. Read Full Report: http://www.transparencymarketresearch.com/mass-spectrometry-market.html

Mass Spectrometry-Based Proteomics for Pre-Eclampsia and Preterm Birth

Directory of Open Access Journals (Sweden)

Kai P. Law

2015-05-01

Full Text Available Pregnancy-related complications such as pre-eclampsia and preterm birth now represent a notable burden of adverse health. Pre-eclampsia is a hypertensive disorder unique to pregnancy. It is an important cause of maternal death worldwide and a leading cause of fetal growth restriction and iatrogenic prematurity. Fifteen million infants are born preterm each year globally, but more than one million of those do not survive their first month of life. Currently there are no predictive tests available for diagnosis of these pregnancy-related complications and the biological mechanisms of the diseases have not been fully elucidated. Mass spectrometry-based proteomics have all the necessary attributes to provide the needed breakthrough in understanding the pathophysiology of complex human diseases thorough the discovery of biomarkers. The mass spectrometry methodologies employed in the studies for pregnancy-related complications are evaluated in this article. Top-down proteomic and peptidomic profiling by laser mass spectrometry, liquid chromatography or capillary electrophoresis coupled to mass spectrometry, and bottom-up quantitative proteomics and targeted proteomics by liquid chromatography mass spectrometry have been applied to elucidate protein biomarkers and biological mechanism of pregnancy-related complications. The proteomes of serum, urine, amniotic fluid, cervical-vaginal fluid, placental tissue, and cytotrophoblastic cells have all been investigated. Numerous biomarkers or biomarker candidates that could distinguish complicated pregnancies from healthy controls have been proposed. Nevertheless, questions as to the clinically utility and the capacity to elucidate the pathogenesis of the pre-eclampsia and preterm birth remain to be answered.

Mass Spectrometry-Based Proteomics for Pre-Eclampsia and Preterm Birth

Science.gov (United States)

Law, Kai P.; Han, Ting-Li; Tong, Chao; Baker, Philip N.

2015-01-01

Pregnancy-related complications such as pre-eclampsia and preterm birth now represent a notable burden of adverse health. Pre-eclampsia is a hypertensive disorder unique to pregnancy. It is an important cause of maternal death worldwide and a leading cause of fetal growth restriction and iatrogenic prematurity. Fifteen million infants are born preterm each year globally, but more than one million of those do not survive their first month of life. Currently there are no predictive tests available for diagnosis of these pregnancy-related complications and the biological mechanisms of the diseases have not been fully elucidated. Mass spectrometry-based proteomics have all the necessary attributes to provide the needed breakthrough in understanding the pathophysiology of complex human diseases thorough the discovery of biomarkers. The mass spectrometry methodologies employed in the studies for pregnancy-related complications are evaluated in this article. Top-down proteomic and peptidomic profiling by laser mass spectrometry, liquid chromatography or capillary electrophoresis coupled to mass spectrometry, and bottom-up quantitative proteomics and targeted proteomics by liquid chromatography mass spectrometry have been applied to elucidate protein biomarkers and biological mechanism of pregnancy-related complications. The proteomes of serum, urine, amniotic fluid, cervical-vaginal fluid, placental tissue, and cytotrophoblastic cells have all been investigated. Numerous biomarkers or biomarker candidates that could distinguish complicated pregnancies from healthy controls have been proposed. Nevertheless, questions as to the clinically utility and the capacity to elucidate the pathogenesis of the pre-eclampsia and preterm birth remain to be answered. PMID:26006232

Contribution to high-temperature chromatography and high-temperature-gas-chromatography-mass spectrometry of lipids

International Nuclear Information System (INIS)

Aichholz, R.

1998-04-01

This thesis describes the use of high temperature gas chromatography for the investigation of unusual triacylglycerols, cyanolipids and bees waxes. The used glass capillary columns were pretreated and coated with tailor made synthesized high temperature stable polysiloxane phases. The selective separation properties of the individual columns were tested with a synthetic lipid mixture. Suitable derivatization procedures for the gaschromatographic analyses of neutral lipids, containing multiple bonds as well as hydroxy-, epoxy-, and carboxyl groups, were developed and optimized. Therefore conjugated olefinic-, conjugated olefinic-acetylenic-, hydroxy-, epoxy-, and conjugated olefinic keto triacylglycerols in miscellaneous plant seed oils as well as hydroxy monoesters, diesters and hydroxy diesters in bees waxes could be analysed directly with high temperature gas chromatography for the first time. In order to elucidate the structures of separated lipid compounds, high temperature gas chromatography was coupled to mass spectrometry and tandem mass spectrometry, respectively. Comparable analytical systems are hitherto not commercial available. Therefore instrumental prerequisites for a comprehensive and detailed analysis of seed oils and bees waxes were established. In GC/MS commonly two ionization methods are used, electron impact ionization and chemical ionization. For the analysis of lipids the first is of limited use only. Due to intensive fragmentation only weak molecular ions are observed. In contrast, the chemical ionization yields in better results. Dominant quasi molecular ions enable an unambiguous determination of the molecular weight. Moreover, characteristic fragment ions provide important indications of certain structural features of the examined compounds. Nevertheless, in some cases the chromatographic resolution was insufficient in order to separate all compounds present in natural lipid mixtures. Owing to the selected detection with mass spectrometry

Automated, parallel mass spectrometry imaging and structural identification of lipids

DEFF Research Database (Denmark)

Ellis, Shane R.; Paine, Martin R.L.; Eijkel, Gert B.

2018-01-01

We report a method that enables automated data-dependent acquisition of lipid tandem mass spectrometry data in parallel with a high-resolution mass spectrometry imaging experiment. The method does not increase the total image acquisition time and is combined with automatic structural assignments....... This lipidome-per-pixel approach automatically identified and validated 104 unique molecular lipids and their spatial locations from rat cerebellar tissue....

Mass Spectrometry Imaging of Drugs of Abuse in Hair.

Science.gov (United States)

Flinders, Bryn; Cuypers, Eva; Porta, Tiffany; Varesio, Emmanuel; Hopfgartner, Gérard; Heeren, Ron M A

2017-01-01

Hair testing is a powerful tool routinely used for the detection of drugs of abuse. The analysis of hair is highly advantageous as it can provide prolonged drug detectability versus that in biological fluids and chronological information about drug intake based on the average growth of hair. However, current methodology requires large amounts of hair samples and involves complex time-consuming sample preparation followed by gas or liquid chromatography coupled with mass spectrometry. Mass spectrometry imaging is increasingly being used for the analysis of single hair samples, as it provides more accurate and visual chronological information in single hair samples.Here, two methods for the preparation of single hair samples for mass spectrometry imaging are presented.The first uses an in-house built cutting apparatus to prepare longitudinal sections, the second is a method for embedding and cryo-sectioning hair samples in order to prepare cross-sections all along the hair sample.

Analytical applications of resonance ionization mass spectrometry (RIMS)

International Nuclear Information System (INIS)

Fassett, J.D.; Travis, J.C.

1988-01-01

A perspective on the role of resonance ionization mass spectrometry (RIMS) in the field of analytical chemistry is presented. RIMS provides new, powerful, and complementary capabilities relative to traditional methods of inorganic mass spectrometry. Much of the initial work in RIMS has been to illustrate these capabilities and define the potential of RIMS in the generalized field of chemical analysis. Three areas of application are reviewed here: (1) noble gas measurements; (2) materials analysis using isotope dilution (IDMS); and, (3) solids analysis using direct sampling. The role of RIMS is discussed relative to the more traditional mass spectrometric methods of analysis in these areas. The applications are meant to illustrate the present state-of-the-art as well as point to the future state-of-the-art of RIMS in chemical analysis. (author)

Analysis of organic compounds by secondary neutral mass spectrometry (SNMS) and secondary ion mass spectrometry (SIMS)

International Nuclear Information System (INIS)

Ewinger, H.P.

1993-05-01

This study is about the use of secondary neutral mass spectrometry (SNMS) and secondary ion mass spectrometry (SIMS) as analytical techniques with depth resolution in determining organic components in environmental solid microparticles. The first application of plasma SNMS to organic compounds revealed the spectra to be composed mainly of signals from the atoms of all participating elements, such as C, H, O, N, S, P, and Cl. In addition, signals produced by multi-atomic clusters can be detected, such as CH, C 2 , CH 2 , C 2 H, and C 3 , as well as signals indicating the presence of organic compounds with hetero elements, such as OH, NH, and CN. Their intensity decreases very markedly with increasing numbers of atoms. Among the signals from bi-atomic clusters, those coming from elements with large mass differences are most intense. The use of plasma SNMS with organic compounds has shown that, except for spurious chemical reactions induced by ion bombardment and photodesorption by the photons of the plasma, it is possible to analyze with resolution in depth, elements of organic solids. A more detailed molecular characterization of organic compounds is possible by means of SIMS on the basis of multi-atomic fragments and by comparison with suitable signal patterns. (orig./BBR) [de

Impact of automation on mass spectrometry.

Science.gov (United States)

Zhang, Yan Victoria; Rockwood, Alan

2015-10-23

Mass spectrometry coupled to liquid chromatography (LC-MS and LC-MS/MS) is an analytical technique that has rapidly grown in popularity in clinical practice. In contrast to traditional technology, mass spectrometry is superior in many respects including resolution, specificity, multiplex capability and has the ability to measure analytes in various matrices. Despite these advantages, LC-MS/MS remains high cost, labor intensive and has limited throughput. This specialized technology requires highly trained personnel and therefore has largely been limited to large institutions, academic organizations and reference laboratories. Advances in automation will be paramount to break through this bottleneck and increase its appeal for routine use. This article reviews these challenges, shares perspectives on essential features for LC-MS/MS total automation and proposes a step-wise and incremental approach to achieve total automation through reducing human intervention, increasing throughput and eventually integrating the LC-MS/MS system into the automated clinical laboratory operations. Copyright © 2015 Elsevier B.V. All rights reserved.

Investigation of Elemental Mass Spectrometry in Pharmacology for Peptide Quantitation at Femtomolar Levels.

Directory of Open Access Journals (Sweden)

Emmanuelle Cordeau

Full Text Available In the search of new robust and environmental-friendly analytical methods able to answer quantitative issues in pharmacology, we explore liquid chromatography (LC associated with elemental mass spectrometry (ICP-MS to monitor peptides in such complex biological matrices. The novelty is to use mass spectrometry to replace radiolabelling and radioactivity measurements, which represent up-to now the gold standard to measure organic compound concentrations in life science. As a proof of concept, we choose the vasopressin (AVP/V1A receptor system for model pharmacological assays. The capacity of ICP-MS to provide highly sensitive quantitation of metallic and hetero elements, whatever the sample medium, prompted us to investigate this technique in combination with appropriate labelling of the peptide of interest. Selenium, that is scarcely present in biological media, was selected as a good compromise between ICP-MS response, covalent tagging ability using conventional sulfur chemistry and peptide detection specificity. Applying selenium monitoring by elemental mass spectrometry in pharmacology is challenging due to the very high salt content and organic material complexity of the samples that produces polyatomic aggregates and thus potentially mass interferences with selenium detection. Hyphenation with a chromatographic separation was found compulsory. Noteworthy, we aimed to develop a straightforward quantitative protocol that can be performed in any laboratory equipped with a standard macrobore LC-ICP-MS system, in order to avoid time-consuming sample treatment or special implementation of instrumental set-up, while allowing efficient suppression of all mass interferences to reach the targeted sensitivity. Significantly, a quantification limit of 57 ng Se L-1 (72 femtomoles of injected Se was achieved, the samples issued from the pharmacological assays being directly introduced into the LC-ICP-MS system. The established method was successfully

Helium-3 mass spectrometry for low-level tritium analysis of environmental samples

International Nuclear Information System (INIS)

Surano, K.A.; Hudson, G.B.; Failor, R.A.; Sims, J.M.; Holland, R.C.; MacLean, S.C.; Garrison, J.C.

1991-04-01

Helium-3 ( 3 He) mass spectrometry for the analysis of low-level tritium ( 3 H) concentrations in environmental sample matrices was compared with conventional low-level β-decay counting methods. The mass-spectrometry method compared favorably, equaling or surpassing conventional decay-counting methods with respect to most criteria. Additional research and method refinements may make 3 He mass spectrometry the method of choice for routine, low-level to very-low-level 3 H measurements in a wide variety of environmental samples in the future

Determination of 5-fluorouracil in plasma with HPLC-tandem mass spectrometry

NARCIS (Netherlands)

van Kuilenburg, A. B. P.; van Lenthe, H.; Maring, J. G.; van Gennip, A. H.

2006-01-01

In this article, we describe a fast and specific method to measure 5FU with HPLC tandem-mass spectrometry. Reversed-phase HPLC was combined with electrospray ionization tandem mass spectrometry and detection was performed by multiple-reaction monitoring. Stable-isotope-labeled 5FU (1,3-15N2-5FU) was

Impact of comprehensive two-dimensional gas chromatography with mass spectrometry on food analysis.

Science.gov (United States)

Tranchida, Peter Q; Purcaro, Giorgia; Maimone, Mariarosa; Mondello, Luigi

2016-01-01

Comprehensive two-dimensional gas chromatography with mass spectrometry has been on the separation-science scene for about 15 years. This three-dimensional method has made a great positive impact on various fields of research, and among these that related to food analysis is certainly at the forefront. The present critical review is based on the use of comprehensive two-dimensional gas chromatography with mass spectrometry in the untargeted (general qualitative profiling and fingerprinting) and targeted analysis of food volatiles; attention is focused not only on its potential in such applications, but also on how recent advances in comprehensive two-dimensional gas chromatography with mass spectrometry will potentially be important for food analysis. Additionally, emphasis is devoted to the many instances in which straightforward gas chromatography with mass spectrometry is a sufficiently-powerful analytical tool. Finally, possible future scenarios in the comprehensive two-dimensional gas chromatography with mass spectrometry food analysis field are discussed. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

A MASSive Laboratory Tour. An Interactive Mass Spectrometry Outreach Activity for Children

Science.gov (United States)

Jungmann, Julia H.; Mascini, Nadine E.; Kiss, Andras; Smith, Donald F.; Klinkert, Ivo; Eijkel, Gert B.; Duursma, Marc C.; Cillero Pastor, Berta; Chughtai, Kamila; Chughtai, Sanaullah; Heeren, Ron M. A.

2013-07-01

It is imperative to fascinate young children at an early stage in their education for the analytical sciences. The exposure of the public to mass spectrometry presently increases rapidly through the common media. Outreach activities can take advantage of this exposure and employ mass spectrometry as an exquisite example of an analytical science in which children can be fascinated. The presented teaching modules introduce children to mass spectrometry and give them the opportunity to experience a modern research laboratory. The modules are highly adaptable and can be applied to young children from the age of 6 to 14 y. In an interactive tour, the students explore three major scientific concepts related to mass spectrometry; the building blocks of matter, charged particle manipulation by electrostatic fields, and analyte identification by mass analysis. Also, the students carry out a mass spectrometry experiment and learn to interpret the resulting mass spectra. The multistage, inquiry-based tour contains flexible methods, which teach the students current-day research techniques and possible applications to real research topics. Besides the scientific concepts, laboratory safety and hygiene are stressed and the students are enthused for the analytical sciences by participating in "hands-on" work. The presented modules have repeatedly been successfully employed during laboratory open days. They are also found to be extremely suitable for (early) high school science classes during laboratory visit-focused field trips.

Large geometry secondary ion mass spectrometry (LG-SIMS) for the enhancement of nuclear safeguards applications

International Nuclear Information System (INIS)

Helberg, P.M.L.; Wallenius, M.; Vincent, C.; Albert, N.; Peres, P.; Truyens, J.

2013-01-01

A new LG-SIMS (Large Geometry Secondary Ion Mass Spectrometry) laboratory is currently being established at the Joint Research Centre, the Institute of Transuranium Elements for the purpose of improving the analytical capabilities within the European Commission. The laboratory will mainly be used for analysing uranium bearing aerosol particles collected on cotton swipes from nuclear Safeguards inspections but it will also be used for Nuclear Forensics and other Safeguards related applications. Until recently, this type of analysis has predominantly been performed using the small geometry CAMECA IMS 3F-7F instrument series. These instruments provide both particle screening and isotope ratio capabilities. The performance of these instruments was however limited by the occurrence of isobaric interferences, in particular for the minor isotopes ( 234 U, 236 U), that could not be resolved without compromising the transmission of the instrument. A recent breakthrough to solve this problem has been the implementation of Large Geometry SIMS, the CAMECA 1270 / 1280 / 1280-HR models, for this type of analysis. This instrument has originally been developed for geosciences applications requiring both high transmission and high mass resolution capabilities. This came out to be a key instrumental advantage also for uranium particle analyses, as it allows efficient removal of common molecular interferences with minimum loss in transmission. Furthermore an electrostatic ion optical device has been added for increasing the mass dispersion which allows the simultaneous detection of all uranium isotopes. The Automated Particle Measurement (APM) software has been developed to perform screening measurement in an automated mode. Combined with the APM screening software, LG-SIMS instruments greatly improve the overall performance and throughput of isotopic analyses of U particles for nuclear Safeguards purposes. The paper is followed by the slides of the presentation. (A.C.)

Stable isotope mass spectrometry in petroleum exploration

International Nuclear Information System (INIS)

Mathur, Manju

1997-01-01

The stable isotope mass spectrometry plays an important role to evaluate the stable isotopic composition of hydrocarbons. The isotopic ratios of certain elements in petroleum samples reflect certain characteristics which are useful for petroleum exploration

Fast DNA analysis by laser mass spectrometry for human genome analysis

International Nuclear Information System (INIS)

Tang, K.; Taranenko, N. I.; Allman, S. L.; Chang, L. Y.; Chen, C. H.

1995-01-01

Fast DNA sequencing by laser mass spectrometry is possible if the following 3 criteria are met: (1) Size of DNA fragment should be greater than 300 nucleotides. (2) Enough sensitivity to detect DNA produce from polymerases chain reactins (PCR). (3) Higher resolution of mass spectr. So far, the firt 2 criteria are met: If the resolution can be significantly improve, fast DNA sequencing by laser mass spectrometry weil be a reality in the near feature

Pyrolysis - gas chromatography - mass spectrometry of lignins

Energy Technology Data Exchange (ETDEWEB)

Martin, F; Saiz-Jimenez, C; Gonzalez-Vila, F J

1979-01-01

Milled wood lignins from spruce, beech and bamboo were pyrolysed. The high-boiling products of pyrolysis were studied by GLC and mass spectrometry. The forty-three products identified provide information on the structural units of lignin.

LILBID-mass spectrometry of the mitochondrial preprotein translocase TOM

International Nuclear Information System (INIS)

Mager, Frauke; Lintzel, Julia; Nussberger, Stephan; Sokolova, Lucie; Brutschy, Bernhard

2010-01-01

In the present work we applied a novel mass spectrometry method termed laser-induced liquid bead ion desorption mass spectrometry (LILBID-MS) to the outer mitochondrial membrane protein translocon TOM to analyze its subunit composition and stoichiometry. With TOM core complex, purified at high pH, we demonstrate that a TOM core complex of Neurospora crassa is composed of at least two Tom40 and Tom22 molecules, respectively, and more than five small Tom subunits between 5.5 and 6.4 kDa. We show that the multiprotein complex has a total molecular mass higher than 170 depending on the number of Tom5, Tom6 and Tom7 molecules bound.

LILBID-mass spectrometry of the mitochondrial preprotein translocase TOM

Science.gov (United States)

Mager, Frauke; Sokolova, Lucie; Lintzel, Julia; Brutschy, Bernhard; Nussberger, Stephan

2010-11-01

In the present work we applied a novel mass spectrometry method termed laser-induced liquid bead ion desorption mass spectrometry (LILBID-MS) to the outer mitochondrial membrane protein translocon TOM to analyze its subunit composition and stoichiometry. With TOM core complex, purified at high pH, we demonstrate that a TOM core complex of Neurospora crassa is composed of at least two Tom40 and Tom22 molecules, respectively, and more than five small Tom subunits between 5.5 and 6.4 kDa. We show that the multiprotein complex has a total molecular mass higher than 170 depending on the number of Tom5, Tom6 and Tom7 molecules bound.

Triple quadrupole tandem mass spectrometry: A real alternative to high resolution magnetic sector instrument for the analysis of polychlorinated dibenzo-p-dioxins, furans and dioxin-like polychlorinated biphenyls.

Science.gov (United States)

García-Bermejo, Ángel; Ábalos, Manuela; Sauló, Jordi; Abad, Esteban; González, María José; Gómara, Belén

2015-08-19

This paper reports on the optimisation, characterisation, validation and applicability of gas chromatography coupled to triple quadrupole mass spectrometry in its tandem operation mode (GC-QqQ(MS/MS) for the quantification of polychlorinated dibenzo-p-dioxins and furans (PCDD/Fs, dioxins) and dioxin-like polychlorinated biphenyls (DL-PCBs) in environmental and food matrices. MS/MS parameters were selected to achieve the high sensitivity and selectivity required for the analysis of this type of compounds and samples. Good repeatability for areas (RSD = 1-10%, for PCDD/Fs and DL-PCBs) and for ion transition ratios (RSD = 0.3-10%, for PCDD/Fs, and 0.2-15%, for DL-PCBs) and low instrumental limits of detection, 0.07-0.75 pg μL(-1) (for dioxins) and 0.05-0.63 pg μL(-1) (for DL-PCBs), were obtained. A comparative study of the congener specific determination using both GC-QqQ(MS/MS) and gas chromatography-high resolution mass spectrometry (GC-HRMS) was also performed by analysing several fortified samples and certified reference materials (CRMs) with low (feed and foodstuffs), median (sewage sludge) and high (fly ash) toxic equivalency (TEQ) concentration levels, i.e. 0.60, 1.83, 72.9 and 3609 pg WHO-TEQ(PCDD/Fs) g(-1). The agreement between the results obtained for the total TEQs (dioxins) on GC-QqQ(MS/MS) and GC-HRMS in all the investigated samples were within the range of ±4%, and that of DL-PCBs at concentration levels of 0.84 pg WHO-TEQs (DL-PCBs) g(-1), in the case of feedstuffs, was 0.11%. Both instrumental methods have similar and comparable linearity, precision and accuracy. The GC-QqQ(MS/MS) sensitivity, lower than that of GC-HRMS, is good enough (iLODs in the down to low pg levels) to detect the normal concentrations of these compounds in food and environmental samples. These results make GC-QqQ(MS/MS) suitable for the quantitative analysis of dioxins and DL-PCBs and a real alternative tool to the reference sector HRMS instruments. Copyright © 2015 Elsevier

Laser desorption mass spectrometry for biomolecule detection and its applications

Science.gov (United States)

Winston Chen, C. H.; Sammartano, L. J.; Isola, N. R.; Allman, S. L.

2001-08-01

During the past few years, we developed and used laser desorption mass spectrometry for biomolecule detections. Matrix-assisted laser desorption/ionization (MALDI) was successfully used to detect DNA fragments with the size larger than 3000 base pairs. It was also successfully used to sequence DNA with both enzymatic and chemical degradation methods to produce DNA ladders. We also developed MALDI with fragmentation for direct DNA sequencing for short DNA probes. Since laser desorption mass spectrometry for DNA detection has the advantages of fast speed and no need of labeling, it has a great potential for molecular diagnosis for disease and person identification by DNA fingerprinting. We applied laser desorption mass spectrometry to succeed in the diagnosis of cystic fibrosis and several other nerve degenerative diseases such as Huntington's disease. We also succeeded in demonstrating DNA typing for forensic applications.

Laser desorption mass spectrometry for biomolecule detection and its applications

International Nuclear Information System (INIS)

Winston Chen, C.H.; Allman, S.L.; Sammartano, L.J.; Isola, N.R.

2001-01-01

During the past few years, we developed and used laser desorption mass spectrometry for biomolecule detections. Matrix-assisted laser desorption/ionization (MALDI) was successfully used to detect DNA fragments with the size larger than 3000 base pairs. It was also successfully used to sequence DNA with both enzymatic and chemical degradation methods to produce DNA ladders. We also developed MALDI with fragmentation for direct DNA sequencing for short DNA probes. Since laser desorption mass spectrometry for DNA detection has the advantages of fast speed and no need of labeling, it has a great potential for molecular diagnosis for disease and person identification by DNA fingerprinting. We applied laser desorption mass spectrometry to succeed in the diagnosis of cystic fibrosis and several other nerve degenerative diseases such as Huntington's disease. We also succeeded in demonstrating DNA typing for forensic applications

Elucidating rhizosphere processes by mass spectrometry - A review.

Science.gov (United States)

Rugova, Ariana; Puschenreiter, Markus; Koellensperger, Gunda; Hann, Stephan

2017-03-01

The presented review discusses state-of-the-art mass spectrometric methods, which have been developed and applied for investigation of chemical processes in the soil-root interface, the so-called rhizosphere. Rhizosphere soil's physical and chemical characteristics are to a great extent influenced by a complex mixture of compounds released from plant roots, i.e. root exudates, which have a high impact on nutrient and trace element dynamics in the soil-root interface as well as on microbial activities or soil physico-chemical characteristics. Chemical characterization as well as accurate quantification of the compounds present in the rhizosphere is a major prerequisite for a better understanding of rhizosphere processes and requires the development and application of advanced sampling procedures in combination with highly selective and sensitive analytical techniques. During the last years, targeted and non-targeted mass spectrometry-based methods have emerged and their combination with specific separation methods for various elements and compounds of a wide polarity range have been successfully applied in several studies. With this review we critically discuss the work that has been conducted within the last decade in the context of rhizosphere research and elemental or molecular mass spectrometry emphasizing different separation techniques as GC, LC and CE. Moreover, selected applications such as metal detoxification or nutrient acquisition will be discussed regarding the mass spectrometric techniques applied in studies of root exudates in plant-bacteria interactions. Additionally, a more recent isotope probing technique as novel mass spectrometry based application is highlighted. Copyright © 2017 Elsevier B.V. All rights reserved.

Estimation of the quantification uncertainty from flow injection and liquid chromatography transient signals in inductively coupled plasma mass spectrometry

International Nuclear Information System (INIS)

Laborda, Francisco; Medrano, Jesus; Castillo, Juan R.

2004-01-01

The quality of the quantitative results obtained from transient signals in high-performance liquid chromatography-inductively coupled plasma mass spectrometry (HPLC-ICPMS) and flow injection-inductively coupled plasma mass spectrometry (FI-ICPMS) was investigated under multielement conditions. Quantification methods were based on multiple-point calibration by simple and weighted linear regression, and double-point calibration (measurement of the baseline and one standard). An uncertainty model, which includes the main sources of uncertainty from FI-ICPMS and HPLC-ICPMS (signal measurement, sample flow rate and injection volume), was developed to estimate peak area uncertainties and statistical weights used in weighted linear regression. The behaviour of the ICPMS instrument was characterized in order to be considered in the model, concluding that the instrument works as a concentration detector when it is used to monitorize transient signals from flow injection or chromatographic separations. Proper quantification by the three calibration methods was achieved when compared to reference materials, although the double-point calibration allowed to obtain results of the same quality as the multiple-point calibration, shortening the calibration time. Relative expanded uncertainties ranged from 10-20% for concentrations around the LOQ to 5% for concentrations higher than 100 times the LOQ

The future of the accelerator mass spectrometry of rare long-lived radioactive isotopes

International Nuclear Information System (INIS)

Litherland, A.E.

1990-01-01

Accelerators, originally designed for nuclear physics, can be added to mass spectrometric apparatus to increase the sensitivity so that isotope ratios in the range 10 -12 to 10 -15 can be measured routinely. This significant improvement of high-sensitivity mass spectrometry has been called Accelerator Mass Spectrometry. The present article addresses the basic principles of accelerator mass spectrometry and some recent applications which show its versatility. In particular, it is noted that accelerator mass spectrometry could play an increasing role in the measurement of the levels of long lived radioactivities in the environment, including the actinides, which result from human activities such as the use of nuclear power. To fulfill this promise, continued research and development is necessary to provide ion sources, various types of heavy ion accelerators and peripheral magnetic and electric analysers. (N.K.)

Determination of iodine in oyster tissue by isotope dilution laser resonance ionization mass spectrometry

International Nuclear Information System (INIS)

Fassett, J.D.; Murphy, T.J.

1990-01-01

The technique of laser resonance ionization mass spectrometry has been combined with isotope dilution analysis to determine iodine in oyster tissue. The long-lived radioisotope, 129I, was used to spike the samples. Samples were equilibrated with the 129I, wet ashed under controlled conditions, and iodine separated by coprecipitation with silver chloride. The analyte was dried as silver ammonium iodide upon a tantalum filament from which iodine was thermally desorbed in the resonance ionization mass spectrometry instrument. A single-color, two-photon resonant plus one-photon ionization scheme was used to form positive iodine ions. Long-lived iodine signals were achieved from 100 ng of iodine. The precision of 127I/129I measurement has been evaluated by replicate determinations of the spike, the spike calibration samples, and the oyster tissue samples and was 1.0%. Measurement precision among samples was 1.9% for the spike calibration and 1.4% for the oyster tissue. The concentration of iodine determined in SRM 1566a, Oyster Tissue, was 4.44 micrograms/g with an estimate of the overall uncertainty for the analysis of +/- 0.12 microgram/g

Analytical capabilities of laser-probe mass spectrometry

International Nuclear Information System (INIS)

Kovalev, I.D.; Madsimov, G.A.; Suchkov, A.I.; Larin, N.V.

1978-01-01

The physical bases and quantitative analytical procedures of laser-probe mass spectrometry are considered in this review. A comparison is made of the capabilities of static and dynamic mass spectrometers. Techniques are studied for improving the analytical characteristics of laser-probe mass spectrometers. The advantages, for quantitative analysis, of the Q-switched mode over the normal pulse mode for lasers are: (a) the possibility of analysing metals, semiconductors and insulators without the use of standards; and (b) the possibility of layer-by-layer and local analysis. (Auth.)

Practical aspects and trends in analytical organic mass spectrometry

International Nuclear Information System (INIS)

Schlunegger, U.P.

1981-01-01

Proceeding from the fundamentals of mass spectrometry (MS), some more recent developments of analytical organic MS are shown in comparison with conventional MS. Sections are headed: the vacuum, production of ions in the mass spectrometer, ions in the analyzer of a mass spectrometer, general considerations, practice of modern MS: selected examples

SU-8 as a material for lab-on-a-chip-based mass spectrometry.

Science.gov (United States)

Arscott, Steve

2014-10-07

This short review focuses on the application of SU-8 for the microchip-based approach to the miniaturization of mass spectrometry. Chip-based mass spectrometry will make the technology commonplace and bring benefits such as lower costs and autonomy. The chip-based miniaturization of mass spectrometry necessitates the use of new materials which are compatible with top-down fabrication involving both planar and non-planar processes. In this context, SU-8 is a very versatile epoxy-based, negative tone resist which is sensitive to ultraviolet radiation, X-rays and electron beam exposure. It has a very wide thickness range, from nanometres to millimetres, enabling the formation of mechanically rigid, very high aspect ratio, vertical, narrow width structures required to form microfluidic slots and channels for laboratory-on-a-chip design. It is also relatively chemically resistant and biologically compatible in terms of the liquid solutions used for mass spectrometry. This review looks at the impact and potential of SU-8 on the different parts of chip-based mass spectrometry - pre-treatment, ionization processes, and ion sorting and detection.

Laser sputter neutral mass spectrometry

Energy Technology Data Exchange (ETDEWEB)

King, B.V.; Clarke, M.; Hu, H.; Betz [Newcastle Univ., NSW (Australia). Dept. of Physics

1993-12-31

Laser sputter neutral mass spectrometry (LSNMS) is an emerging technique for highly sensitive surface analysis. In this technique a target is bombarded with a pulsed beam of keV ions. The sputtered particles are intercepted by a high intensity pulsed laser beam above the surface and ionised with almost 100% efficiency. The photions may then be mass analysed using a quadrupole or, more commonly, using time of flight (TOF) techniques. In this method photoions are extracted from the ionisation region, accelerated to a known energy E{sub o} and strike a channelplate detector a distance `d` away. The flight time `t` of the photoions is then related to their mass by `d` {radical}m / {radical} 2E{sub o} so measurement of `t` allows mass spectra to be obtained. It is found that LSNMS is an emerging technique of great sensitivity and flexibility, useful for both applied analysis and to investigate basic sputtering processes. 4 refs., 3 figs.

Laser sputter neutral mass spectrometry

Energy Technology Data Exchange (ETDEWEB)

King, B V; Clarke, M; Hu, H; Betz, [Newcastle Univ., NSW (Australia). Dept. of Physics

1994-12-31

Laser sputter neutral mass spectrometry (LSNMS) is an emerging technique for highly sensitive surface analysis. In this technique a target is bombarded with a pulsed beam of keV ions. The sputtered particles are intercepted by a high intensity pulsed laser beam above the surface and ionised with almost 100% efficiency. The photions may then be mass analysed using a quadrupole or, more commonly, using time of flight (TOF) techniques. In this method photoions are extracted from the ionisation region, accelerated to a known energy E{sub o} and strike a channelplate detector a distance `d` away. The flight time `t` of the photoions is then related to their mass by `d` {radical}m / {radical} 2E{sub o} so measurement of `t` allows mass spectra to be obtained. It is found that LSNMS is an emerging technique of great sensitivity and flexibility, useful for both applied analysis and to investigate basic sputtering processes. 4 refs., 3 figs.

Inductively coupled plasma-mass spectrometry: an initial assessment of the VG isotopes Plasmaquad

International Nuclear Information System (INIS)

Brown, R.M.; Pickford, C.J.

1985-04-01

The Chemical Analysis Group has been approached by a British Scientific instrument maker regarding the possibility of the group participating in a Department of Trade and Industry sponsored scheme whereby we would have a 12 month period to assess the advantages and disadvantages of a new analytical technique, Inductively Coupled Plasma-Mass Spectrometry. This report details our initial assessment of the instrument, carried out in order to decide whether to participate in the scheme. We have attempted to discover whether the instrument meets the claims made of it in advertising literature, and have attempted to compare the technique with another, proven technique, Inductively Coupled Plasma - Optical Emission Spectroscopy. The Plasmaquad offers excellent sensitivity for almost all of the elements of the periodic table, giving a distinct improvement over the Chemical Analysis Group's present capabilities for many elements. The isotope ratio measuring ability is important, as the Group has no such capability at the moment and a demand for this type of measurement is foreseen. Our conclusions, while inevitably somewhat subjective, form the basis for recommending Harwell to participate in the scheme. (author)

Radiocarbon accelerator mass spectrometry: background and contamination

International Nuclear Information System (INIS)

Beukens, R.P.

1993-01-01

Since the advent of radiocarbon accelerator mass spectrometry (AMS) many studies have been conducted to understand the background from mass spectrometric processes and the origins of contamination associated with the ion source and sample preparation. By studying the individual contributions a better understanding of these processes has been obtained and it has been demonstrated that it is possible to date samples reliably up to 60 000 BP. (orig.)

Quantitative Clinical Chemistry Proteomics (qCCP) using mass spectrometry: general characteristics and application.

Science.gov (United States)

Lehmann, Sylvain; Hoofnagle, Andrew; Hochstrasser, Denis; Brede, Cato; Glueckmann, Matthias; Cocho, José A; Ceglarek, Uta; Lenz, Christof; Vialaret, Jérôme; Scherl, Alexander; Hirtz, Christophe

2013-05-01

Proteomics studies typically aim to exhaustively detect peptides/proteins in a given biological sample. Over the past decade, the number of publications using proteomics methodologies has exploded. This was made possible due to the availability of high-quality genomic data and many technological advances in the fields of microfluidics and mass spectrometry. Proteomics in biomedical research was initially used in 'functional' studies for the identification of proteins involved in pathophysiological processes, complexes and networks. Improved sensitivity of instrumentation facilitated the analysis of even more complex sample types, including human biological fluids. It is at that point the field of clinical proteomics was born, and its fundamental aim was the discovery and (ideally) validation of biomarkers for the diagnosis, prognosis, or therapeutic monitoring of disease. Eventually, it was recognized that the technologies used in clinical proteomics studies [particularly liquid chromatography-tandem mass spectrometry (LC-MS/MS)] could represent an alternative to classical immunochemical assays. Prior to deploying MS in the measurement of peptides/proteins in the clinical laboratory, it seems likely that traditional proteomics workflows and data management systems will need to adapt to the clinical environment and meet in vitro diagnostic (IVD) regulatory constraints. This defines a new field, as reviewed in this article, that we have termed quantitative Clinical Chemistry Proteomics (qCCP).

Surface analysis of lipids by mass spectrometry: more than just imaging.

Science.gov (United States)

Ellis, Shane R; Brown, Simon H; In Het Panhuis, Marc; Blanksby, Stephen J; Mitchell, Todd W

2013-10-01

Mass spectrometry is now an indispensable tool for lipid analysis and is arguably the driving force in the renaissance of lipid research. In its various forms, mass spectrometry is uniquely capable of resolving the extensive compositional and structural diversity of lipids in biological systems. Furthermore, it provides the ability to accurately quantify molecular-level changes in lipid populations associated with changes in metabolism and environment; bringing lipid science to the "omics" age. The recent explosion of mass spectrometry-based surface analysis techniques is fuelling further expansion of the lipidomics field. This is evidenced by the numerous papers published on the subject of mass spectrometric imaging of lipids in recent years. While imaging mass spectrometry provides new and exciting possibilities, it is but one of the many opportunities direct surface analysis offers the lipid researcher. In this review we describe the current state-of-the-art in the direct surface analysis of lipids with a focus on tissue sections, intact cells and thin-layer chromatography substrates. The suitability of these different approaches towards analysis of the major lipid classes along with their current and potential applications in the field of lipid analysis are evaluated. Copyright © 2013 Elsevier Ltd. All rights reserved.

Mass Spectrometry Imaging Can Distinguish on a Proteomic Level Between Proliferative Nodules Within a Benign Congenital Nevus and Malignant Melanoma.

Science.gov (United States)

Lazova, Rossitza; Yang, Zhe; El Habr, Constantin; Lim, Young; Choate, Keith Adam; Seeley, Erin H; Caprioli, Richard M; Yangqun, Li

2017-09-01

Histopathological interpretation of proliferative nodules occurring in association with congenital melanocytic nevi can be very challenging due to their similarities with congenital malignant melanoma and malignant melanoma arising in association with congenital nevi. We hereby report a diagnostically challenging case of congenital melanocytic nevus with proliferative nodules and ulcerations, which was originally misdiagnosed as congenital malignant melanoma. Subsequent histopathological examination in consultation by one of the authors (R.L.) and mass spectrometry imaging analysis rendered a diagnosis of congenital melanocytic nevus with proliferative nodules. In this case, mass spectrometry imaging, a novel method capable of distinguishing benign from malignant melanocytic lesions on a proteomic level, was instrumental in making the diagnosis of a benign nevus. We emphasize the importance of this method as an ancillary tool in the diagnosis of difficult melanocytic lesions.

Simultaneous drug identification in urine of sexual assault victims by using liquid chromatography tandem mass spectrometry.

Science.gov (United States)

Lee, Hei Hwa; Chen, Suen Chi; Lee, Jong Feng; Lin, Hsin Yu; Chen, Bai Hsiun

2018-01-01

According to domestic and international epidemiological investigation, the proportion of substance involved sexual assault has the trend of ascent. In the past, laboratory methods that investigated urine sample of the sexual assault victims was to screen with enzyme immunoassay and then confirmed with mass spectrometry. The objective of the study is to simultaneously identify abused drugs in 126 decoded urine samples of sexual assault victims by liquid chromatography tandem mass spectrometry. The instrument was operated in multiple-reaction monitoring with an electro-spray positive ionization mode. Chromatograms were separated with ACE5 C18 column on a gradient of acetonitrile. After liquid-liquid extraction, samples were passed through a 0.22μm PVDF filter before injection into the system. The limits of quantitation ranged from 0.2 to 10ng/mL. The precision (CV) results were below 12.9% (intraday) and 15.0% (interday). The intraday accuracy ranged from 84.8 to 121.0%, interday accuracy ranged from 72.0 to 117.3%. We found that 29 (23.0%) were positive for drugs. The most common drug identified is flunitrazepam (11.1%), followed by nimetazepam and ketamine (7.9%), some new psychoactive substances, such as 2C-B, mephedrone, methylone, PMA and PMMA were also identified. We identified abused drugs, benzodiazepines, and new psychoactive substances in urine of sexual assault victims by using liquid chromatography tandem mass spectrometry. Copyright © 2017 Elsevier B.V. All rights reserved.

Microbial metabolomics with gas chromatography/mass spectrometry

NARCIS (Netherlands)

Koek, M.M.; Muilwijk, B.; Werf, M.J. van der; Hankemeier, T.

2006-01-01

An analytical method was set up suitable for the analysis of microbial metabolomes, consisting of an oximation and silylation derivatization reaction and subsequent analysis by gas chromatography coupled to mass spectrometry. Microbial matrixes contain many compounds that potentially interfere with

Analytical strategies in mass spectrometry-based phosphoproteomics

DEFF Research Database (Denmark)

Rosenqvist, Heidi; Ye, Juanying; Jensen, Ole N

2011-01-01

then discuss various tandem mass spectrometry approaches for phosphopeptide sequencing and quantification, and we consider aspects of phosphoproteome data analysis and interpretation. Efficient integration of these stages of phosphoproteome analysis is highly important to ensure a successful outcome of large...

Multi-Reflection Time-of-Flight Mass Separation and Spectrometry

CERN Document Server

Kreim, Susanne; Wolf, R N

2014-01-01

The mass of a nucleus is one of its most fundamental ground-state properties and reveals the strength of nuclear binding. Investigating the binding energy of nuclei with respect to the number of protons and neutrons in a nucleus is important for advancing nuclear theory and increases our understanding of nucleosynthesis in supernovae and neutron stars. Precision mass measurements on radioactive nuclides belong to the state-of-the-art techniques [1, 2]. Presently, four complementary techniques are applied: isochronous and Schottky mass spectrometry in storage rings (IMS and SMS, respectively), magnetic-rigidity time-of-flight (TOF-ρ) measurements, and Penning-trap mass spectrometry (PTMS). With measurement cycles in the sub-ms range, IMS and TOF-Bρ MS are well suited for very short-lived species while offering moderate relative precision on the level of 10−6. A higher precision is achieved by SMS but with the need for measurement times on the order of several seconds. As soon as masses with a relative prec...

High efficiency nebulization for helium inductively coupled plasma mass spectrometry

International Nuclear Information System (INIS)

Jorabchi, Kaveh; McCormick, Ryan; Levine, Jonathan A.; Liu Huiying; Nam, S.-H.; Montaser, Akbar

2006-01-01

A pneumatically-driven, high efficiency nebulizer is explored for helium inductively coupled plasma mass spectrometry. The aerosol characteristics and analyte transport efficiencies of the high efficiency nebulizer for nebulization with helium are measured and compared to the results obtained with argon. Analytical performance indices of the helium inductively coupled plasma mass spectrometry are evaluated in terms of detection limits and precision. The helium inductively coupled plasma mass spectrometry detection limits obtained with the high efficiency nebulizer at 200 μL/min are higher than those achieved with the ultrasonic nebulizer consuming 2 mL/min solution, however, precision is generally better with high efficiency nebulizer (1-4% vs. 3-8% with ultrasonic nebulizer). Detection limits with the high efficiency nebulizer at 200 μL/min solution uptake rate approach those using ultrasonic nebulizer upon efficient desolvation with a heated spray chamber followed by a Peltier-cooled multipass condenser

Multi photon ionization mass spectrometry of carbamate pesticides, herbicides and fungicides

International Nuclear Information System (INIS)

Grun, Carsten; Koenig, Marcelle; Grotemeyer, Juergen

2001-01-01

Pesticides and herbicides are useful for a wide range of applications today. The determination of these substances either in the pure form or in complex matrices is of high analytical interest. Especially since these substances can by found in every day products. The combination of multi photon ionization (MUPI) and time of flight laser mass spectrometry may be a powerful tool for achieving fast well interpretable mass spectra for analytical purposes. In this paper we will discuss the mass spectra of several pesticides and herbicides accessed by MUPI-time-of-flight mass spectrometry. The influence of the laser pulse duration on the mass spectra are discussed

Plutonium bioassay by inductively coupled plasma mass spectrometry ICP/MS

International Nuclear Information System (INIS)

Wyse, E.J.; Fisher, D.R.

1993-04-01

The determination of plutonium in urine poses several analytical challenges, e.g., detectability, matrix, etc. We have investigated the feasibility of analyzing plutonium in processed urine by inductively coupled plasma mass spectrometry (ICP/MS). The urine samples are first spiked with 244 Pu as a tracer and internal standard, then processed by co-precipitation and column chromatography using TRU-Spec trademark, an extraction resin. By enhancing ICP/MS detection capabilities via improved sample introduction and data acquisition efficiencies, an instrumental detection limit of 5 to 50 fg (0.3 to 3 fCi for 239 pu) is typically obtained, depending on the desired degree of quantitation. A brief summary of the analytical method as well as the basis for measuring radionuclides by ICP/MS are submitted; the separation procedure, methods of sample introduction, and data acquisition techniques are then highlighted

Current medical research with the application of coupled techniques with mass spectrometry

OpenAIRE

Ka?u?na-Czapli?ska, Joanna

2011-01-01

Summary The most effective methods of analysis of organic compounds in biological fluids are coupled chromatographic techniques. Capillary gas chromatography/mass spectrometry (GC-MS) allows the most efficient separation, identification and quantification of volatile metabolites in biological fluids. Liquid chromatography-mass spectrometry (LC-MS) is especially suitable for the analysis of non-volatile and/or thermally unstable compounds. A major drawback of liquid chromatography-mass spectro...

Mass Spectrometry Applications for Toxicology

OpenAIRE

Mbughuni, Michael M.; Jannetto, Paul J.; Langman, Loralie J.

2016-01-01

Toxicology is a multidisciplinary study of poisons, aimed to correlate the quantitative and qualitative relationships between poisons and their physiological and behavioural effects in living systems. Other key aspects of toxicology focus on elucidation of the mechanisms of action of poisons and development of remedies and treatment plans for associated toxic effects. In these endeavours, Mass spectrometry (MS) has become a powerful analytical technique with a wide range of application used i...

Analytical chemistry instrumentation

International Nuclear Information System (INIS)

Laing, W.R.

1986-01-01

In nine sections, 48 chapters cover 1) analytical chemistry and the environment 2) environmental radiochemistry 3) automated instrumentation 4) advances in analytical mass spectrometry 5) fourier transform spectroscopy 6) analytical chemistry of plutonium 7) nuclear analytical chemistry 8) chemometrics and 9) nuclear fuel technology

multiplierz v2.0: A Python-based ecosystem for shared access and analysis of native mass spectrometry data.

Science.gov (United States)

Alexander, William M; Ficarro, Scott B; Adelmant, Guillaume; Marto, Jarrod A

2017-08-01

The continued evolution of modern mass spectrometry instrumentation and associated methods represents a critical component in efforts to decipher the molecular mechanisms which underlie normal physiology and understand how dysregulation of biological pathways contributes to human disease. The increasing scale of these experiments combined with the technological diversity of mass spectrometers presents several challenges for community-wide data access, analysis, and distribution. Here we detail a redesigned version of multiplierz, our Python software library which leverages our common application programming interface (mzAPI) for analysis and distribution of proteomic data. New features include support for a wider range of native mass spectrometry file types, interfaces to additional database search engines, compatibility with new reporting formats, and high-level tools to perform post-search proteomic analyses. A GUI desktop environment, mzDesktop, provides access to multiplierz functionality through a user friendly interface. multiplierz is available for download from: https://github.com/BlaisProteomics/multiplierz; and mzDesktop is available for download from: https://sourceforge.net/projects/multiplierz/. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Identification of bacteria using mass spectrometry techniques

Czech Academy of Sciences Publication Activity Database

Krásný, Lukáš; Hynek, R.; Hochel, I.

2013-01-01

Roč. 353, NOV 2013 (2013), s. 67-79 ISSN 1387-3806 R&D Projects: GA ČR GAP503/10/0664 Institutional support: RVO:61388971 Keywords : Mass spectrometry * Bacteria * Identification Subject RIV: EE - Microbiology, Virology Impact factor: 2.227, year: 2013

Mass spectrometry in structural biology and biophysics architecture, dynamics, and interaction of biomolecules

CERN Document Server

Kaltashov, Igor A; Desiderio, Dominic M; Nibbering, Nico M

2012-01-01

The definitive guide to mass spectrometry techniques in biology and biophysics The use of mass spectrometry (MS) to study the architecture and dynamics of proteins is increasingly common within the biophysical community, and Mass Spectrometry in Structural Biology and Biophysics: Architecture, Dynamics, and Interaction of Biomolecules, Second Edition provides readers with detailed, systematic coverage of the current state of the art. Offering an unrivalled overview of modern MS-based armamentarium that can be used to solve the most challenging problems in biophysics, structural biol

Study of the matrix specific mass discrimination effects during inductively coupled plasma mass spectrometry isotope ratio measurements

International Nuclear Information System (INIS)

Vassileva, E.; Quetel, Ch.R.

2004-01-01

Sample matrix related effects on mass discrimination during inductively coupled plasma mass spectrometry (ICP-MS) isotope ratio measurements have only been rarely reported. However, they can lead to errors larger than the uncertainty claimed on the ratio results when not properly taken into account or corrected for. These matrix specific affects were experienced during an Isotope Dilution Mass Spectrometry (IDMS) campaign we carried out for the certification of the Cd amount content in some food digest samples (7% acidity and salts content around 450μg g -1 ). Dilution was not possible for Cd only present at the low ng g -1 level. Up to 1% difference was observed on Cd isotope ratio results between measurements performed directly or after matrix separation. This was a significant difference considering that less than 1.5% relative combined uncertainty was eventually estimated for these IDMS measurements. Similar results could be obtained either way after the implementation of necessary corrections. The direct measurement approach associated to a correction for mass discrimination effects using the food digest sample itself (and the IUPAC table values as reference for the natural Cd isotopic composition) was preferred as it was the easiest. Consequently, the impact of matrix effects on mass discrimination during isotope ratio measurements with two types of ICP- MS (quadrupole and magnetic sector instruments) was studied for 4 elements (Li, Cu, Cd and Tl). Samples of varying salinity (up to 0.25%) and acidity (up to 7%) characteristics were prepared using isotopic certified reference materials of these elements. The long term and short-term stability, respectively reproducibility and repeatability, of the results, as well as the evolution of the difference to certified ratio values were monitored. As expected the 13 investigated isotopic ratios were all sensitive to variations in salt and acid concentrations. Our experiments also showed that simultaneous variation

Mass Determination of Entire Amyloid Fibrils by Using Mass Spectrometry.

Science.gov (United States)

Doussineau, Tristan; Mathevon, Carole; Altamura, Lucie; Vendrely, Charlotte; Dugourd, Philippe; Forge, Vincent; Antoine, Rodolphe

2016-02-12

Amyloid fibrils are self-assembled protein structures with important roles in biology (either pathogenic or physiological), and are attracting increasing interest in nanotechnology. However, because of their high aspect ratio and the presence of some polymorphism, that is, the possibility to adopt various structures, their characterization is challenging and basic information such as their mass is unknown. Here we show that charge-detection mass spectrometry, recently developed for large self-assembled systems such as viruses, provides such information in a straightforward manner. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

[Sample preparation and bioanalysis in mass spectrometry].

Science.gov (United States)

Bourgogne, Emmanuel; Wagner, Michel

2015-01-01

The quantitative analysis of compounds of clinical interest of low molecular weight (sample preparation. Sample preparation is a crucial part of chemical/biological analysis and in a sense is considered the bottleneck of the whole analytical process. The main objectives of sample preparation are the removal of potential interferences, analyte preconcentration, and converting (if needed) the analyte into a more suitable form for detection or separation. Without chromatographic separation, endogenous compounds, co-eluted products may affect a quantitative method in mass spectrometry performance. This work focuses on three distinct parts. First, quantitative bioanalysis will be defined, different matrices and sample preparation techniques currently used in bioanalysis by mass spectrometry of/for small molecules of clinical interest in biological fluids. In a second step the goals of sample preparation will be described. Finally, in a third step, sample preparation strategies will be made either directly ("dilute and shoot") or after precipitation.

Quantitation of stable isotopic tracers of calcium by fast atom bombardment mass spectrometry

International Nuclear Information System (INIS)

Jiang, X.; Smith, D.L.

1987-01-01

Instrumentation and methodology developed for quantitation of stable isotopic traces in urine are described. Calcium is isolated from urine as the insoluble oxalate salt which is subsequently dissolved in hydrochloric acid. The isotopic content of the acid solution is determined by use of a conventional mass spectrometer equipped with a fast atom bombardment ion source. Calcium ions are desorbed from the sample surface by a beam of high-energy xenon atoms and detected with a high-resolution mass spectrometer. A data acquisition system has been developed to control the mass spectrometer and record the ion signals. Detailed analysis of potential sources of error indicates that the precision of the method is presently limited primarily by an isotope effect that occurs during ion desorption. Results presented here demonstrate that the relative abundances of calcium isotopes in urine can be determined with high precision (coefficient of variation < 0.2%) and that the method is a viable alternative to conventional thermal ionization mass spectrometry. The method is especially attractive because it uses a conventional high-resolution mass spectrometer which is routinely used for analysis of organic substances

Simulation of Two Dimensional Electrophoresis and Tandem Mass Spectrometry for Teaching Proteomics

Science.gov (United States)

Fisher, Amanda; Sekera, Emily; Payne, Jill; Craig, Paul

2012-01-01

In proteomics, complex mixtures of proteins are separated (usually by chromatography or electrophoresis) and identified by mass spectrometry. We have created 2DE Tandem MS, a computer program designed for use in the biochemistry, proteomics, or bioinformatics classroom. It contains two simulations--2D electrophoresis and tandem mass spectrometry.…

Mapping posttranscriptional modifications in 5S ribosomal RNA by MALDI mass spectrometry.

OpenAIRE

Kirpekar, F; Douthwaite, S; Roepstorff, P

2000-01-01

We present a method to screen RNA for posttranscriptional modifications based on Matrix Assisted Laser Desorption/Ionization mass spectrometry (MALDI-MS). After the RNA is digested to completion with a nucleotide-specific RNase, the fragments are analyzed by mass spectrometry. A comparison of the observed mass data with the data predicted from the gene sequence identifies fragments harboring modified nucleotides. Fragments larger than dinucleotides were valuable for the identification of post...

Direct Analysis of Large Living Organism by Megavolt Electrostatic Ionization Mass Spectrometry

Science.gov (United States)

Ng, Kwan-Ming; Tang, Ho-Wai; Man, Sin-Heng; Mak, Pui-Yuk; Choi, Yi-Ching; Wong, Melody Yee-Man

2014-09-01

A new ambient ionization method allowing the direct chemical analysis of living human body by mass spectrometry (MS) was developed. This MS method, namely Megavolt Electrostatic Ionization Mass Spectrometry, is based on electrostatic charging of a living individual to megavolt (MV) potential, illicit drugs, and explosives on skin/glove, flammable solvent on cloth/tissue paper, and volatile food substances in breath were readily ionized and detected by a mass spectrometer.

The mass spectral density in quantitative time-of-flight mass spectrometry of polymers

Science.gov (United States)

Tate, Ranjeet S.; Ebeling, Dan; Smith, Lloyd M.

2001-03-01

Time-of-flight mass spectrometry (TOF-MS) is being increasingly used for the study of polymers, for example to obtain the distribution of molecular masses for polymer samples. Serious efforts have also been underway to use TOF-MS for DNA sequencing. In TOF-MS the data is obtained in the form of a time-series that represents the distribution in arrival times of ions of various m/z ratios. This time-series data is then converted to a "mass-spectrum" via a coordinate transformation from the arrival time (t) to the corresponding mass-to-charge ratio (m/z = const. t^2). In this transformation, it is important to keep in mind that spectra are distributions, or densities of weight +1, and thus do not transform as functions. To obtain the mass-spectral density, it is necessary to include a multiplicative factor of √m/z. Common commercial instruments do not take this factor into account. Dropping this factor has no effect on qualitative analysis (detection) or local quantitative measurements, since S/N or signal-to-baseline ratios are unaffected for peaks with small dispersions. However, there are serious consequences for general quantitative analyses. In DNA sequencing applications, loss of signal intensity is in part attributed to multiple charging; however, since the √m/z factor is not taken into account, this conclusion is based on an overestimate (by a factor of √z) of the relative amount of the multiply charged species. In the study of polymers, the normalized dispersion is underestimated by approximately (M_w/Mn -1)/2. In terms of M_w/Mn itself, for example, a M_w/M_n=1.5 calculated without the √m factor corresponds in fact to a M_w/M_n=1.88.

Design of software platform based on linux operating system for γ-spectrometry instrument

International Nuclear Information System (INIS)

Hong Tianqi; Zhou Chen; Zhang Yongjin

2008-01-01

This paper described the design of γ-spectrometry instrument software platform based on s3c2410a processor with arm920t core, emphases are focused on analyzing the integrated application of embedded linux operating system, yaffs file system and qt/embedded GUI development library. It presented a new software platform in portable instrument for γ measurement. (authors)

Collisional Activation of Peptide Ions in FT-ICR Mass Spectrometry

International Nuclear Information System (INIS)

Laskin, Julia; Futrell, Jean H.

2003-01-01

In the last decade characterization of complex molecules, particularly biomolecules became a focus of both fundamental and applied research in mass spectrometry. Most of these studies utilize tandem mass spectrometry (MS/MS) for obtaining structural information for complex molecules. . Tandem mass spectrometry (MS/MS) typically involves the mass selection of a primary ion, its activation by collision or photon excitation, unimolecular decay into fragment ions characteristic of the ion structure and its internal excitation, and mass analysis of the fragment ions. Although the fundamental principles of tandem mass spectrometry of relatively small molecules are fairly well understood, our understanding of the activation and fragmentation of large molecules is much more primitive. For small ions a single energetic collision is sufficient to dissociate the ion but this is not the case for complex molecules. For large ions two fundamental limits severely constrain fragmentation in tandem mass spectrometry. First the center-of-mass collision energy?the absolute upper limit of energy transfer in a collision process?decreases with increasing mass of the projectile ion for fixed ion kinetic energy and neutral mass. Secondly, the dramatic increase in density of states with increasing internal degrees of freedom of the ion decreases the rate of dissociation by many orders of magnitude at a given internal energy. Consequently most practical MS/MS experiments with complex ions involve multiple collision activation (MCA-CID), multi-photon activation or surface-induced dissociation (SID). This review is focused on what has been learned in recent research studies concerned with fundamental aspects of MCA-CID and SID of model peptides with emphasis on experiments carried out using Fourier transform ion cyclotron resonance mass spectrometers (FT-ICR MS). These studies provide the first quantitative comparison of gas-phase multiple-collision activation and SID of peptide ions

'Collisional Activation of Peptide Ions in FT-ICR Mass Spectrometry'

International Nuclear Information System (INIS)

Laskin, Julia; Futrell, Jean H.

2003-01-01

In the last decade characterization of complex molecules, particularly biomolecules became a focus of both fundamental and applied research in mass spectrometry. Most of these studies utilize tandem mass spectrometry (MS/MS) for obtaining structural information for complex molecules. . Tandem mass spectrometry (MS/MS) typically involves the mass selection of a primary ion, its activation by collision or photon excitation, unimolecular decay into fragment ions characteristic of the ion structure and its internal excitation, and mass analysis of the fragment ions. Although the fundamental principles of tandem mass spectrometry of relatively small molecules are fairly well understood, our understanding of the activation and fragmentation of large molecules is much more primitive. For small ions a single energetic collision is sufficient to dissociate the ion but this is not the case for complex molecules. For large ions two fundamental limits severely constrain fragmentation in tandem mass spectrometry. First the center-of-mass collision energy?the absolute upper limit of energy transfer in a collision process?decreases with increasing mass of the projectile ion for fixed ion kinetic energy and neutral mass. Secondly, the dramatic increase in density of states with increasing internal degrees of freedom of the ion decreases the rate of dissociation by many orders of magnitude at a given internal energy. Consequently most practical MS/MS experiments with complex ions involve multiple collision activation (MCA-CID), multi-photon activation or surface-induced dissociation (SID). This review is focused on what has been learned in recent research studies concerned with fundamental aspects of MCA-CID and SID of model peptides with emphasis on experiments carried out using Fourier transform ion cyclotron resonance mass spectrometers (FT-ICR MS). These studies provide the first quantitative comparison of gas-phase multiple-collision activation and SID of peptide ions

Inductively coupled plasma- mass spectrometry. Chapter 13

International Nuclear Information System (INIS)

Mahalingam, T.R.

1997-01-01

Inductively Coupled Plasma - Mass Spectrometry (ICP-MS) is a new technique for elemental and isotopic analysis which is currently attracting a great deal of interest. This relatively new technique has found wide applications in different fields of research viz., nuclear, geological, biological and environmental sciences

Determination of {sup 135}Cs by accelerator mass spectrometry

Energy Technology Data Exchange (ETDEWEB)

MacDonald, C.M.; Charles, C.R.J. [Andre. E. Lalonde AMS Laboratory, University of Ottawa, 150 Louis Pasteur, Ottawa, ON K1N 6N5 (Canada); Department of Earth Sciences, University of Ottawa, 150 Louis Pasteur, Ottawa, ON K1N 6N5 (Canada); Zhao, X.-L.; Kieser, W.E. [Andre. E. Lalonde AMS Laboratory, University of Ottawa, 150 Louis Pasteur, Ottawa, ON K1N 6N5 (Canada); Department of Physics, University of Ottawa, 150 Louis Pasteur, Ottawa, ON K1N 6N5 (Canada); Cornett, R.J. [Andre. E. Lalonde AMS Laboratory, University of Ottawa, 150 Louis Pasteur, Ottawa, ON K1N 6N5 (Canada); Department of Earth Sciences, University of Ottawa, 150 Louis Pasteur, Ottawa, ON K1N 6N5 (Canada); Litherland, A.E. [IsoTrace Laboratory, University of Toronto, 60 St. George St., Toronto, ON M5S 1A7 (Canada)

2015-10-15

The ratio of anthropogenic {sup 135}Cs and {sup 137}Cs isotopes is characteristic of a uranium fission source. This research evaluates the technique of isotope dilution (yield tracing) for the purpose of quantifying {sup 135}Cs by accelerator mass spectrometry with on-line isobar separation. Interferences from Ba, Zn{sub 2}, and isotopes of equal mass to charge ratios were successfully suppressed. However, some sample crosstalk from source contamination remains. The transmission and di-fluoride ionization efficiencies of Cs isotopes were found to be 8 × 10{sup −3} and 1.7 × 10{sup −7} respectively. This quantification of {sup 135}Cs using yield tracing by accelerator mass spectrometry shows promise for future environmental sample analysis once the issues of sample crosstalk and low efficiency can be resolved.

Mass cytometry: technique for real time single cell multitarget immunoassay based on inductively coupled plasma time-of-flight mass spectrometry.

Science.gov (United States)

Bandura, Dmitry R; Baranov, Vladimir I; Ornatsky, Olga I; Antonov, Alexei; Kinach, Robert; Lou, Xudong; Pavlov, Serguei; Vorobiev, Sergey; Dick, John E; Tanner, Scott D

2009-08-15

A novel instrument for real time analysis of individual biological cells or other microparticles is described. The instrument is based on inductively coupled plasma time-of-flight mass spectrometry and comprises a three-aperture plasma-vacuum interface, a dc quadrupole turning optics for decoupling ions from neutral components, an rf quadrupole ion guide discriminating against low-mass dominant plasma ions, a point-to-parallel focusing dc quadrupole doublet, an orthogonal acceleration reflectron analyzer, a discrete dynode fast ion detector, and an 8-bit 1 GHz digitizer. A high spectrum generation frequency of 76.8 kHz provides capability for collecting multiple spectra from each particle-induced transient ion cloud, typically of 200-300 micros duration. It is shown that the transients can be resolved and characterized individually at a peak frequency of 1100 particles per second. Design considerations and optimization data are presented. The figures of merit of the instrument are measured under standard inductively coupled plasma (ICP) operating conditions ( 900 for m/z = 159, the sensitivity with a standard sample introduction system of >1.4 x 10(8) ion counts per second per mg L(-1) of Tb and an abundance sensitivity of (6 x 10(-4))-(1.4 x 10(-3)) (trailing and leading masses, respectively) are shown. The mass range (m/z = 125-215) and abundance sensitivity are sufficient for elemental immunoassay with up to 60 distinct available elemental tags. When 500) can be used, which provides >2.4 x 10(8) cps per mg L(-1) of Tb, at (1.5 x 10(-3))-(5.0 x 10(-3)) abundance sensitivity. The real-time simultaneous detection of multiple isotopes from individual 1.8 microm polystyrene beads labeled with lanthanides is shown. A real time single cell 20 antigen expression assay of model cell lines and leukemia patient samples immuno-labeled with lanthanide-tagged antibodies is presented.

Laser mass spectrometry of chemical warfare agents using ultrashort laser pulses

International Nuclear Information System (INIS)

Weickhardt, C.; Grun, C.; Grotemeyer, J.

1998-01-01

Fast relaxation processes in excited molecules such as IC, ISC, and fragmentation are observed in many environmentally and technically relevant substances. They cause severe problems to resonance ionization mass spectrometry because they reduce the ionization yield and lead to mass spectra which do not allow the identification of the compound. By the use of ultrashort laser pulses these problems can be overcome and the advantages of REMPI over conventional ionization techniques in mass spectrometry can be regained. This is demonstrated using soil samples contaminated with a chemical warfare agent

Mass spectrometry in nuclear technology - a review of application of thermal ionization mass spectrometry in fuel reprocessing plants. PD-7-1

International Nuclear Information System (INIS)

Dakshinamoorthy, A.

2007-01-01

Mass spectrometry finds the widespread application in nuclear science and technology due to the fact that it can be employed for isotope composition measurements of different elements of interest and also concentration measurements of these elements using isotope dilution techniques. Thermal ionization mass spectrometer (TIMS), Inductively coupled plasma mass spectrometer (ICP-MS) and gas chromatography mass spectrometer (GC-MS) are the different types of mass spectrometers used in nuclear industry for the analyses of isotope composition of special nuclear material, trace impurities in nuclear fuels and components and characterization of various solvents respectively. Among them, TIMS plays a vital role in the nuclear fuel cycle in determining precisely the isotope composition of uranium, plutonium, D/H ratio in heavy water etc. TIMS is an indispensable analytical tool for nuclear material accounting at the input stage of a reprocessing plant by carrying out precise and accurate concentration measurement of plutonium and uranium by isotope dilution mass spectrometry (IDMS). It is the only accepted measurement technique for the purpose because of its high precision, better sensitivity and no quantitative separation is needed. The isotope abundance measurements of uranium and plutonium at this point are also useful for burn-up studies and isotope correlations. Mass spectrometric analysis of uranium and plutonium is also required for nuclear data measurements and calibrating other chemical methods

Polymer and Additive Mass Spectrometry Literature Review

Energy Technology Data Exchange (ETDEWEB)

Shear, Trevor Allan [Los Alamos National Lab. (LANL), Los Alamos, NM (United States)

2017-06-06

The use of mass spectrometry in fields related to polymers has increased significantly over the past three decades and will be explored in this literature review. The importance of this technique is highlighted when exploring how polymers degrade, verifying purchased materials, and as internal requirements change. The primary focus will be on four ionization techniques and the triple quadrupole and quadrupole / time-of-flight mass spectrometers. The advantages and limitations of each will also be explored.

Recent applications of mass spectrometry in forensic toxicology

Science.gov (United States)

Foltz, Rodger L.

1992-09-01

This review encompasses applications of mass spectrometry reported during the years 1989, 1990 and 1991 for the analysis of cannabinoids, cocaine, opiates, amphetamines, lysergic acid diethylamide (LSD), and their metabolites in physiological specimens.

Variability of matrix effects in liquid and gas chromatography - mass spectrometry analysis of pesticide residues after QuEChERS sample preparation of different food crops

Science.gov (United States)

Gas and liquid chromatography (GC and LC) coupled to sophisticated mass spectrometry (MS) instruments are among the most powerful analytical tools currently available to monitor pesticide residues in food, among other applications. However, both GC-MS and LC-MS are susceptible to matrix effects whi...

Determining Double Bond Position in Lipids Using Online Ozonolysis Coupled to Liquid Chromatography and Ion Mobility-Mass Spectrometry.

Science.gov (United States)

Harris, Rachel A; May, Jody C; Stinson, Craig A; Xia, Yu; McLean, John A

2018-02-06

The increasing focus on lipid metabolism has revealed a need for analytical techniques capable of structurally characterizing lipids with a high degree of specificity. Lipids can exist as any one of a large number of double bond positional isomers, which are indistinguishable by single-stage mass spectrometry alone. Ozonolysis reactions coupled to mass spectrometry have previously been demonstrated as a means for localizing double bonds in unsaturated lipids. Here we describe an online, solution-phase reactor using ozone produced via a low-pressure mercury lamp, which generates aldehyde products diagnostic of cleavage at a particular double bond position. This flow-cell device is utilized in conjunction with structurally selective ion mobility-mass spectrometry. The lamp-mediated reaction was found to be effective for multiple lipid species in both positive and negative ionization modes, and the conversion efficiency from precursor to product ions was tunable across a wide range (20-95%) by varying the flow rate through the ozonolysis device. Ion mobility separation of the ozonolysis products generated additional structural information and revealed the presence of saturated species in a complex mixture. The method presented here is simple, robust, and readily coupled to existing instrument platforms with minimal modifications necessary. For these reasons, application to standard lipidomic workflows is possible and aids in more comprehensive structural characterization of a myriad of lipid species.

Monoterpene separation by coupling proton transfer reaction time-of-flight mass spectrometry with fastGC.

Science.gov (United States)

Materić, Dušan; Lanza, Matteo; Sulzer, Philipp; Herbig, Jens; Bruhn, Dan; Turner, Claire; Mason, Nigel; Gauci, Vincent

2015-10-01

Proton transfer reaction mass spectrometry (PTR-MS) is a well-established technique for real-time analysis of volatile organic compounds (VOCs). Although it is extremely sensitive (with sensitivities of up to 4500 cps/ppbv, limits of detection monoterpenes, which belong to the most important plant VOCs, still cannot be distinguished so more traditional technologies, such as gas chromatography mass spectrometry (GC-MS), have to be utilised. GC-MS is very time consuming (up to 1 h) and cannot be used for real-time analysis. Here, we introduce a sensitive, near-to-real-time method for plant monoterpene research-PTR-MS coupled with fastGC. We successfully separated and identified six of the most abundant monoterpenes in plant studies (α- and β-pinenes, limonene, 3-carene, camphene and myrcene) in less than 80 s, using both standards and conifer branch enclosures (Norway spruce, Scots pine and black pine). Five monoterpenes usually present in Norway spruce samples with a high abundance were separated even when the compound concentrations were diluted to 20 ppbv. Thus, fastGC-PTR-ToF-MS was shown to be an adequate one-instrument solution for plant monoterpene research.

Real-time measurement of plutonium in air by direct-inlet surface ionization mass spectrometry. Status report

International Nuclear Information System (INIS)

Stoffels, J.J.

1980-04-01

A new technique is being developed for monitoring low-level airborne plutonium on a real-time basis. The technique is based on surface ionization mass spectrometry of airborne particles. It will be capable of measuring plutonium concentrations below the maximum permissible concentration (MPC) level. A complete mass spectrometer was designed and constructed for this purpose. Major components which were developed and made operational for the instrument include an efficient inlet for directly sampling particles in air, a wide dynamic range ion detector and a minicomputer-based ion-burst measurement system. Calibration of the direct-inlet mass spectrometer (DIMS) was initiated to establish the instrument's response to plutonium dioxide as a function of concentration and particle size. This work revealed an important problem - bouncing of particles upon impact with the ionizing filament. Particle bounce results in a significant loss of measurement sensitivity. The feasibility of using an oven ionizer to overcome the particle bounce problem has been demonstrated. A rhenium oven ionizer was designed and constructed for the purpose of trapping particles which enter via the direct inlet. High-speed particles were trapped in the oven yielding a measurement sensitivity comparable to that for particles which are preloaded. Development of the Pu DIMS can now be completed by optimizing the oven design and calibrating the instrument's performance with UO 2 and CeO 2 particles as analogs to PuO 2 particles

Can laser-ionisation time-of-flight mass spectrometry be a promising alternative to laser ablation/inductively-coupled plasma mass spectrometry and glow discharge mass spectrometry for the elemental analysis of solids?

NARCIS (Netherlands)

Sysoev, AA; Sysoev, AA

2002-01-01

At the beginning of the age of laser-ionisation mass spectrometry (LIMS) increasing numbers of publications were observed. However, later the method began to run into obstacles associated with poor reproducibility of analysis and large variations in elemental sensitivities so that the wide interest

Cortisol production rates measured by liquid chromatography/mass spectrometry

International Nuclear Information System (INIS)

Esteban, N.V.; Yergey, A.L.

1990-01-01

Cortisol production rates (FPRs) in physiologic and pathologic states in humans have been investigated over the past 30 years. However, there has been conflicting evidence concerning the validity of the currently accepted value of FPRs in humans (12 to 15 mg/m2/d) as determined by radiotracer methodology. The present study reviews previous methods proposed for the measurement of FPRs in humans and discusses the applications of the first method for the direct determination of 24-hour plasma FPRs during continuous administration of a stable isotope, using a thermospray high-pressure liquid chromatography-mass spectrometry technique. The technique is fast, sensitive, and, unlike gas chromatography-mass spectrometry methods, does not require derivatization, allowing on-line detection and quantification of plasma cortisol after a simple extraction procedure. The results of determination of plasma FPRs by stable tracer/mass spectrometry are directly in units of mass/time and, unlike radiotracer methods, are independent of any determination of volume of distribution or cortisol concentration. Our methodology offers distinct advantages over radiotracer techniques in simplicity and reliability since only single measurements of isotope ratios are required. The technique was validated in adrenalectomized patients. Circadian variations in daily FRPs were observed in normal volunteers, and, to date, results suggest a lower FRP in normal children and adults than previously believed. 88 references

A theory of stable-isotope dilution mass spectrometry

International Nuclear Information System (INIS)

Pickup, J.F.; McPherson, C.K.

1977-01-01

In order to perform quantitative analysis using stable isotope dilution with mass spectrometry, an equation is derived which describes the relationship between the relative proportions of natural and labelled material and measured isotope ratios

Detection and quantification of neurotensin in human brain tissue by matrix-assisted laser desorption/ionization time-of-flight mass spectrometry

DEFF Research Database (Denmark)

Gobom, J; Kraeuter, K O; Persson, R

2000-01-01

A method was developed for mass spectrometric detection of neurotensin (NT)-like immunoreactivity and quantification of NT in human brain tissue. The method is based on immunoprecipitation followed by analysis using matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF......-MS). The identity of the major component of the immunoprecipitates as neurotensin was confirmed by fragment ion analysis on an electrospray ionization quadrupole time-of-flight instrument. MALDI-TOF-MS quantification of NT was achieved using stable-isotope-labeled NT as the internal standard, yielding an error...

Analysis of hydroxamate siderophores in soil solution using liquid chromatography with mass spectrometry and tandem mass spectrometry with on-line sample preconcentration.

Science.gov (United States)

Olofsson, Madelen A; Bylund, Dan

2015-10-01

A liquid chromatography with electrospray ionization mass spectrometry method was developed to quantitatively and qualitatively analyze 13 hydroxamate siderophores (ferrichrome, ferrirubin, ferrirhodin, ferrichrysin, ferricrocin, ferrioxamine B, D1 , E and G, neocoprogen I and II, coprogen and triacetylfusarinine C). Samples were preconcentrated on-line by a switch-valve setup prior to analyte separation on a Kinetex C18 column. Gradient elution was performed using a mixture of an ammonium formate buffer and acetonitrile. Total analysis time including column conditioning was 20.5 min. Analytes were fragmented by applying collision-induced dissociation, enabling structural identification by tandem mass spectrometry. Limit of detection values for the selected ion monitoring method ranged from 71 pM to 1.5 nM with corresponding values of two to nine times higher for the multiple reaction monitoring method. The liquid chromatography with mass spectrometry method resulted in a robust and sensitive quantification of hydroxamate siderophores as indicated by retention time stability, linearity, sensitivity, precision and recovery. The analytical error of the methods, assessed through random-order, duplicate analysis of soil samples extracted with a mixture of 10 mM phosphate buffer and methanol, appears negligible in relation to between-sample variations. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Resonance ionization mass spectrometry system for measurement of environmental samples

International Nuclear Information System (INIS)

Pibida, L.; McMahon, C.A.; Noertershaeuser, W.; Bushaw, B.A.

2002-01-01

A resonance ionization mass spectrometry (RIMS) system has been developed at the National Institute of Standards and Technology (NIST) for sensitive and selective determination of radio-cesium in the environment. The overall efficiency was determined to be 4x10-7 with a combined (laser and mass spectrometer) selectivity of 108 for both 135Cs and 137Cs with respect to 133Cs. RIMS isotopic ratio measurements of 135Cs/ 137Cs were performed on a nuclear fuel burn-up sample and compared to measurements on a similar system at Pacific Northwest National Laboratory (PNNL) and to conventional thermal ionization mass spectrometry (TIMS). Results of preliminary RIMS investigations on a freshwater lake sediment sample are also discussed

Structural characterization of suppressor lipids by high-resolution mass spectrometry

DEFF Research Database (Denmark)

Rovillos, Mary Joy; Pauling, Josch Konstantin; Hannibal-Bach, Hans Kristian

2016-01-01

RATIONALE: Suppressor lipids were originally identified in 1993 and reported to encompass six lipid classes that enable Saccharomyces cerevisiae to live without sphingolipids. Structural characterization, using non-mass spectrometric approaches, revealed that these suppressor lipids are very long...... chain fatty acid (VLCFA)-containing glycerophospholipids with polar head groups that are typically incorporated into sphingolipids. Here we report, for the first time, the structural characterization of the yeast suppressor lipids using high-resolution mass spectrometry. METHODS: Suppressor lipids were...... isolated by preparative chromatography and subjected to structural characterization using hybrid quadrupole time-of-flight and ion trap-orbitrap mass spectrometry. RESULTS: Our investigation recapitulates the overall structural features of the suppressor lipids and provides an in-depth characterization...

Negative ion electrospray ionization mass spectrometry of nucleoside phosphoramidate monoesters: elucidation of novel rearrangement mechanisms by multistage mass spectrometry incorporating in-source deuterium labelling.

Science.gov (United States)

Xu, Peng-Xiang; Hu, An-Fu; Hu, Dan; Gao, Xiang; Zhao, Yu-Fen

2008-10-01

Several O-2',3'-isopropylideneuridine-O-5'-phosphoramidate monoesters were synthesized and analyzed by negative ion electrospray ionization tandem mass spectrometry (ESI-MS(n)). Two kinds of novel rearrangement reactions were observed due to the difference in the amino acid in the nucleoside phosphoramidate monoesters, and possible mechanisms were proposed. One involves a five-membered cyclic transition state. The other is formation of a stable five-membered ring intermediate by Michael addition. Results were confirmed by tandem mass spectrometry and isotopically labeled hydrogen atoms. Furthermore, the internal hydrogen exchange between active hydrogen and methyl acrylate in the heated capillary of the mass spectrometer was found. The characteristic fragmentation behavior in ESI-MS may be used to monitor this kind of compounds in the biological metabolism.

Advancements in mass spectrometry for biological samples: Protein chemical cross-linking and metabolite analysis of plant tissues

Energy Technology Data Exchange (ETDEWEB)

Klein, Adam [Iowa State Univ., Ames, IA (United States)

2015-01-01

This thesis presents work on advancements and applications of methodology for the analysis of biological samples using mass spectrometry. Included in this work are improvements to chemical cross-linking mass spectrometry (CXMS) for the study of protein structures and mass spectrometry imaging and quantitative analysis to study plant metabolites. Applications include using matrix-assisted laser desorption/ionization-mass spectrometry imaging (MALDI-MSI) to further explore metabolic heterogeneity in plant tissues and chemical interactions at the interface between plants and pests. Additional work was focused on developing liquid chromatography-mass spectrometry (LC-MS) methods to investigate metabolites associated with plant-pest interactions.

Major roles for minor bacterial lipids identified by mass spectrometry.

Science.gov (United States)

Garrett, Teresa A

2017-11-01

Mass spectrometry of lipids, especially those isolated from bacteria, has ballooned over the past two decades, affirming in the process the complexity of the lipidome. With this has come the identification of new and interesting lipid structures. Here is an overview of several novel lipids, from both Gram-negative and Gram-positive bacteria with roles in health and disease, whose structural identification was facilitated using mass spectrometry. This article is part of a Special Issue entitled: Bacterial Lipids edited by Russell E. Bishop. Copyright © 2016 Elsevier B.V. All rights reserved.

Liquid chromatography-mass spectrometry for metabolic footprinting of co-cultures of lactic and propionic acid bacteria

DEFF Research Database (Denmark)

Honore, Anders H.; Thorsen, Michael; Skov, Thomas

2013-01-01

(UPLC) coupled to high-resolution mass spectrometry (MS) via electrospray ionisation (ESI) operated in both positive and negative modes is regarded as the optimum instrumental technique. The applicability of a range of liquid chromatographic techniques ranging from ion-pair (IPC) and hydrophilic...... could be a potent approach to elucidation of the mechanism. The purpose of this review is to discuss the two pre-requisites for such a study-the compound classes expected in the co-cultures, and on the basis of these, the most suitable analytical technique(s). Ultrahigh-performance liquid chromatography...

Improving mass measurement accuracy in mass spectrometry based proteomics by combining open source tools for chromatographic alignment and internal calibration.

Science.gov (United States)

Palmblad, Magnus; van der Burgt, Yuri E M; Dalebout, Hans; Derks, Rico J E; Schoenmaker, Bart; Deelder, André M

2009-05-02

Accurate mass determination enhances peptide identification in mass spectrometry based proteomics. We here describe the combination of two previously published open source software tools to improve mass measurement accuracy in Fourier transform ion cyclotron resonance mass spectrometry (FTICRMS). The first program, msalign, aligns one MS/MS dataset with one FTICRMS dataset. The second software, recal2, uses peptides identified from the MS/MS data for automated internal calibration of the FTICR spectra, resulting in sub-ppm mass measurement errors.

Mass spectrometry-based metabolomics: Targeting the crosstalk between gut microbiota and brain in neurodegenerative disorders.

Science.gov (United States)

Luan, Hemi; Wang, Xian; Cai, Zongwei

2017-11-12

Metabolomics seeks to take a "snapshot" in a time of the levels, activities, regulation and interactions of all small molecule metabolites in response to a biological system with genetic or environmental changes. The emerging development in mass spectrometry technologies has shown promise in the discovery and quantitation of neuroactive small molecule metabolites associated with gut microbiota and brain. Significant progress has been made recently in the characterization of intermediate role of small molecule metabolites linked to neural development and neurodegenerative disorder, showing its potential in understanding the crosstalk between gut microbiota and the host brain. More evidence reveals that small molecule metabolites may play a critical role in mediating microbial effects on neurotransmission and disease development. Mass spectrometry-based metabolomics is uniquely suitable for obtaining the metabolic signals in bidirectional communication between gut microbiota and brain. In this review, we summarized major mass spectrometry technologies including liquid chromatography-mass spectrometry, gas chromatography-mass spectrometry, and imaging mass spectrometry for metabolomics studies of neurodegenerative disorders. We also reviewed the recent advances in the identification of new metabolites by mass spectrometry and metabolic pathways involved in the connection of intestinal microbiota and brain. These metabolic pathways allowed the microbiota to impact the regular function of the brain, which can in turn affect the composition of microbiota via the neurotransmitter substances. The dysfunctional interaction of this crosstalk connects neurodegenerative diseases, including Parkinson's disease, Alzheimer's disease and Huntington's disease. The mass spectrometry-based metabolomics analysis provides information for targeting dysfunctional pathways of small molecule metabolites in the development of the neurodegenerative diseases, which may be valuable for the

Quantitation of mycotoxins using direct analysis in real time (DART)-mass spectrometry (MS)

Science.gov (United States)

Ambient ionization represents a new generation of mass spectrometry ion sources which is used for rapid ionization of small molecules under ambient conditions. The combination of ambient ionization and mass spectrometry allows analyzing multiple food samples with simple or no sample treatment, or in...

The Application of Resonance-Enhanced Multiphoton Ionization Technique in Gas Chromatography Mass Spectrometry

Directory of Open Access Journals (Sweden)

Adan Li

2014-01-01

Full Text Available Gas chromatography resonance-enhanced multiphoton ionization time-of-flight mass spectrometry (GC/REMPI-TOFMS using a nanosecond laser has been applied to analyze the 16 polycyclic aromatic hydrocarbons (PAHs. The excited-state lifetime, absorption characters, and energy of electronic states of the 16 PAHs were investigated to optimize the ionization yield. A river water sample pretreated by means of solid phase extraction was analyzed to evaluate the performance of the analytical instrument. The results suggested that REMPI is superior to electron impact ionization method for soft ionization and suppresses the background signal due to aliphatic hydrocarbons. Thus, GC/REMPI-TOFMS is a more reliable method for the determination of PAHs present in the environment.

Fusion of mass spectrometry-based metabolomics data

NARCIS (Netherlands)

Smilde, Age K.; van der Werf, Mariët J.; Bijlsma, Sabina; van der Werff-van der Vat, Bianca J. C.; Jellema, Renger H.

2005-01-01

A general method is presented for combining mass spectrometry-based metabolomics data. Such data are becoming more and more abundant, and proper tools for fusing these types of data sets are needed. Fusion of metabolomics data leads to a comprehensive view on the metabolome of an organism or

Radiocarbon detection by ion charge exchange mass spectrometry

International Nuclear Information System (INIS)

Hotchkis, Michael; Wei, Tao

2007-01-01

A method for detection of radiocarbon at low levels is described and the results of tests are presented. We refer to this method as ion charge exchange mass spectrometry (ICE-MS). The ICE-MS instrument is a two stage mass spectrometer. In the first stage, molecular interferences which would otherwise affect radiocarbon detection at mass 14 are eliminated by producing high charge state ions directly in the ion source (charge state ≥2). 14 N interference is eliminated in the second stage by converting the beam to negative ions in a charge exchange cell. The beam is mass-analysed at each stage. We have built a test apparatus consisting of an electron cyclotron resonance ion source and a pair of analysing magnets with a charge exchange cell in between, followed by an electrostatic analyser to improve the signal to background ratio. With this apparatus we have measured charge exchange probabilities for (C n+ → C - ) from 4.5 to 40.5 keV (n = 1-3). We have studied the sources of background including assessment of limits for nitrogen interference by searching for negative ions from charge exchange of 14 N ions. Our system has been used to detect 14 C in enriched samples of CO 2 gas with 14 C/ 12 C isotopic ratio down to the 10 -9 level. Combined with a measured sample consumption rate of 4 ng/s, this corresponds to a capability to detect transient signals containing only a few μBq of 14 C activity, such as may be obtained from chromatographic separation. The method will require further development to match the sensitivity of AMS with a gas ion source; however, even in its present state its sensitivity is well suited to tracer studies in biomedical research and drug development

Gas Chromatography Mass Spectrometry of Quassia undulata Seed ...

African Journals Online (AJOL)

Prof. Ogunji

The use of gas chromatography mass spectrometry (GC MS) as a sensitive and specific technique ... cold flow properties and stability of the fuel to oxidation, peroxidation and polymerization .... determinants of both the physical and chemical ...

ICP magnetic sector multiple collector mass spectrometry and the precise measurement of isotopic compositions using nebulization of solutions and laser ablation of solids

International Nuclear Information System (INIS)

Halliday, A.N.; Lee, D-C.; Christensen, J.N.; Yi, W.; Hall, C.M.; Jones, C.E.; Teagle, D.A.H.; Freedman, P.A.

1996-01-01

Inductively-coupled plasma (ICP) sources offer considerable advantages over thermal sources because the high ionization efficiency facilitates measurements of relatively high sensitivity for elements such as Hf or Sn, which can be difficult to measure precisely with thermal ionization mass spectrometry (TIMS). The mass discrimination (bias) is larger than for TIMS, favours the heavier ions, and decreases in magnitude with increasing mass. However, in contrast to TIMS, this discrimination is largely independent of the chemical or physical properties of the element or the duration of the analysis. This has been demonstrated to high precision with a double focussing multiple collector magnetic sector mass spectrometer with an ICP source. The principle of this instrument is briefly described. The potential of the instrument for high precision isotopic measurements of a very broad range of elements, using solution aspiration or laser ablation, is indicated. 15 refs

Determination of long-lived actinides in soil leachates by inductively coupled plasma: Mass spectrometry

International Nuclear Information System (INIS)

Crain, J.S.; Smith, L.L.; Yaeger, J.S.; Alvarado, J.A.

1994-01-01

Inductively coupled plasma -- mass spectrometry (ICP-MS) was used to concurrently determine multiple long-lived (t 1/2 > 10 4 y) actinide isotopes in soil samples. Ultrasonic nebulization was found to maximize instrument sensitivity. Instrument detection limits for actinides in solution ranged from 50 mBq L -1 ( 239 Pu) to 2 μBq L -1 ( 235 U) Hydride adducts of 232 Th and 238 U interfered with the determinations of 233 U and 239 Pu; thus, extraction chromatography was, used to eliminate the sample matrix, concentrate the analytes, and separate uranium from the other actinides. Alpha spectrometric determinations of 230 Th, 239 Pu, and the 234 U/ 238 U activity ratio in soil leachates compared well with ICP-MS determinations; however, there were some small systematic differences (ca. 10%) between ICP-MS and a-spectrometric determinations of 234 U and 238 U activities

Simulation of the oxidative metabolism of diclofenac by electrochemistry/(liquid chromatography/)mass spectrometry.

Science.gov (United States)

Faber, Helene; Melles, Daniel; Brauckmann, Christine; Wehe, Christoph Alexander; Wentker, Kristina; Karst, Uwe

2012-04-01

Diclofenac is a frequently prescribed drug for rheumatic diseases and muscle pain. In rare cases, it may be associated with a severe hepatotoxicity. In literature, it is discussed whether this toxicity is related to the oxidative phase I metabolism, resulting in electrophilic quinone imines, which can subsequently react with nucleophiles present in the liver in form of glutathione or proteins. In this work, electrochemistry coupled to mass spectrometry is used as a tool for the simulation of the oxidative pathway of diclofenac. Using this purely instrumental approach, diclofenac was oxidized in a thin layer cell equipped with a boron doped diamond working electrode. Sum formulae of generated oxidation products were calculated based on accurate mass measurements with deviations below 2 ppm. Quinone imines from diclofenac were detected using this approach. It could be shown for the first time that these quinone imines do not react with glutathione exclusively but also with larger molecules such as the model protein β-lactoglobulin A. A tryptic digest of the generated drug-protein adduct confirms that the protein is modified at the only free thiol-containing peptide. This simple and purely instrumental set-up offers the possibility of generating reactive metabolites of diclofenac and to assess their reactivity rapidly and easily.

Optimization of the combination micro-high-performance liquid-chromatography/mass spectrometry

International Nuclear Information System (INIS)

Haider, K.

1997-03-01

The coupling of liquid chromatography and mass spectrometry is still growing in significance. In this thesis, a particle beam interface has been investigated for combining ion chromatography with mass spectrometric detection. To introduce the eluent directly (without membrane suppressor) into the spectrometer, only methods with low flow rates like microcolumn chromatography can be used. For the preparation of the columns, reversed-phase and silica-based anion exchange materials were packed into PEEK, steel and fused-silica capillaries with i.d. from 130 to 1000 μm using different methods. The performance of the particle beam interface (modified with a new miniaturized aerosol generator) and the mass spectrometric detection has been studied for a series of inorganic anions as well as aminopolycarboxylic acids and the metal-EDTA complexes. Detection limits between 10 and 100 ng injected could be achieved in the multiple ion detection mode of the mass spectrometer for the investigated solutes. A second type of interface, the direct liquid introduction (DLI) has been used to analyze the priority pollutant phenols. This interface is based on a modified GC-interface into the MS. Separation columns used so far include packed fused-silica capillaries with inner diameter of 75 μm and polystyrene-divinylbenzene (functionalized with tert. butyl groups) as stationary phase. Aspects of instrumentation and effects of chemical ionization in the direct liquid introduction mode are discussed. (author)

Dehydrodimerization of pterostilbene during electrospray ionization mass spectrometry

KAUST Repository

Raji, Misjudeen; Amad, Maan H.; Emwas, Abdul-Hamid M.

2013-01-01

RATIONALE Pterostilbene is a member of the hydroxystilbene family of compounds commonly found in plants such as blueberry and grapes. During the analysis of this compound by electrospray ionization mass spectrometry (ESI-MS), an ion was observed

Mass Spectrometry in Clinical Laboratory: Applications in Therapeutic Drug Monitoring and Toxicology.

Science.gov (United States)

Garg, Uttam; Zhang, Yan Victoria

2016-01-01

Mass spectrometry (MS) has been used in research and specialized clinical laboratories for decades as a very powerful technology to identify and quantify compounds. In recent years, application of MS in routine clinical laboratories has increased significantly. This is mainly due to the ability of MS to provide very specific identification, high sensitivity, and simultaneous analysis of multiple analytes (>100). The coupling of tandem mass spectrometry with gas chromatography (GC) or liquid chromatography (LC) has enabled the rapid expansion of this technology. While applications of MS are used in many clinical areas, therapeutic drug monitoring, drugs of abuse, and clinical toxicology are still the primary focuses of the field. It is not uncommon to see mass spectrometry being used in routine clinical practices for those applications.

Proton transfer reaction time-of-flight mass spectrometry advancement in detection of hazardous substances

International Nuclear Information System (INIS)

Agarwal, B.

2012-01-01

Proton Transfer Reaction Mass Spectrometry (PTR-MS) is a mass spectrometric technique based on chemical ionization, which provides very rapid measurements (within seconds) of volatile organic compounds in air, usually without special sample preparation, and with a very low detection limit. The detection and study of product ion patterns of threat agents such as explosives and drugs and some major environmental pollutants (isocyanates and polychlorinated biphenyls (PCBs)) is explored in detail here using PTR-MS, specifically Proton Transfer Reaction Time-of-Flight Mass Spectrometry (PTR-TOF-MS). The proton transfer reaction (PTR) principle works on the detection of the compound in the vapor phase. For some compounds, which have extremely low vapor pressures, both sample and inlet line heating were needed. Generally, the protonated parent molecule (MH+) is found to be the dominant product ion, which therefore provides us with a higher level of confidence in the assignment of a trace compound. However, for several compounds, dissociative proton transfer can occur at various degrees resulting in other product ions. Analysis of other compounds, such as the presence of taggants and impurities were carried out, and in certain compounds unusual E/N anomalies were discovered (E/N is an instrumental set of parameters, where E is the electric field strength and N is the number density). Head space measurements above four different drinks (plain water, tea, red wine and white wine) spiked with four different 'date rape' drugs were also conducted. (author)

Differentiating Fragmentation Pathways of Cholesterol by Two-Dimensional Fourier Transform Ion Cyclotron Resonance Mass Spectrometry.

Science.gov (United States)

van Agthoven, Maria A; Barrow, Mark P; Chiron, Lionel; Coutouly, Marie-Aude; Kilgour, David; Wootton, Christopher A; Wei, Juan; Soulby, Andrew; Delsuc, Marc-André; Rolando, Christian; O'Connor, Peter B

2015-12-01

Two-dimensional Fourier transform ion cyclotron resonance mass spectrometry is a data-independent analytical method that records the fragmentation patterns of all the compounds in a sample. This study shows the implementation of atmospheric pressure photoionization with two-dimensional (2D) Fourier transform ion cyclotron resonance mass spectrometry. In the resulting 2D mass spectrum, the fragmentation patterns of the radical and protonated species from cholesterol are differentiated. This study shows the use of fragment ion lines, precursor ion lines, and neutral loss lines in the 2D mass spectrum to determine fragmentation mechanisms of known compounds and to gain information on unknown ion species in the spectrum. In concert with high resolution mass spectrometry, 2D Fourier transform ion cyclotron resonance mass spectrometry can be a useful tool for the structural analysis of small molecules. Graphical Abstract ᅟ.

New developments in glow discharge optical emission and mass spectrometry

International Nuclear Information System (INIS)

Hoffmann, Volker; Dorka, Roland; Wilken, Ludger; Wetzig, Klaus

2000-01-01

This paper describes new developments in flow discharge optical emission (GD-OES) and mass spectrometry (GD-MS) at IFW and presents corresponding new applications (analysis of microelectronic multi-layer system by radio frequency glow discharge optical emission spectrometry (RF-GD-OES) and analysis of pure iron by a new Grimm-type GD-MS source)

Mass Spectrometry-Based N-Glycomics of Colorectal Cancer

Directory of Open Access Journals (Sweden)

Manveen K. Sethi

2015-12-01

Full Text Available Colorectal cancer (CRC is one of the most prevalent cancers worldwide. An increased molecular understanding of the CRC pathology is warranted to gain insights into the underlying molecular and cellular mechanisms of the disease. Altered protein glycosylation patterns are associated with most diseases including malignant transformation. Recent advances in mass spectrometry and bioinformatics have accelerated glycomics research and present a new paradigm for cancer biomarker discovery. Mass spectrometry (MS-based glycoproteomics and glycomics, therefore, hold considerable promise to improve the discovery of novel biomarkers with utility in disease diagnosis and therapy. This review focuses on the emerging field of glycomics to present a comprehensive review of advances in technologies and their application in studies aimed at discovering novel glycan-based biomarkers. We will also discuss some of the challenges associated with using glycans as biomarkers.

Mass spectrometry imaging: Towards a lipid microscope?

Science.gov (United States)

Touboul, David; Brunelle, Alain; Laprévote, Olivier

2011-01-01

Biological imaging techniques are the most efficient way to locally measure the variation of different parameters on tissue sections. These analyses are gaining increasing interest since 20 years and allow observing extremely complex biological phenomena at lower and lower time and resolution scale. Nevertheless, most of them only target very few compounds of interest, which are chosen a priori, due to their low resolution power and sensitivity. New chemical imaging technique has to be introduced in order to overcome these limitations, leading to more informative and sensitive analyses for biologists and physicians. Two major mass spectrometry methods can be efficiently used to generate the distribution of biological compounds over a tissue section. Matrix-Assisted Laser Desorption/Ionisation-Mass Spectrometry (MALDI-MS) needs the co-crystallization of the sample with a matrix before to be irradiated by a laser, whereas the analyte is directly desorbed by a primary ion bombardment for Secondary Ion Mass Spectrometry (SIMS) experiments. In both cases, energy used for desorption/ionization is locally deposited -some tens of microns for the laser and some hundreds of nanometers for the ion beam- meaning that small areas over the surface sample can be separately analyzed. Step by step analysis allows spectrum acquisitions over the tissue sections and the data are treated by modern informatics software in order to create ion density maps, i.e., the intensity plot of one specific ion versus the (x,y) position. Main advantages of SIMS and MALDI compared to other chemical imaging techniques lie in the simultaneous acquisition of a large number of biological compounds in mixture with an excellent sensitivity obtained by Time-of-Flight (ToF) mass analyzer. Moreover, data treatment is done a posteriori, due to the fact that no compound is selectively marked, and let us access to the localization of different lipid classes in only one complete acquisition. Copyright © 2010

Chiral recognition and determination of enantiomeric excess by mass spectrometry: A review

International Nuclear Information System (INIS)

Yu, Xiangying; Yao, Zhong-Ping

2017-01-01

Chiral analysis is of great importance to fundamental and applied research in chemical, biological and pharmaceutical sciences. Due to the superiority of mass spectrometry (MS) over other analytical methods in terms of speed, specificity and sensitivity, chiral analysis by MS has attracted much interest in recent years. Chiral analysis by MS typically involves introduction of a chiral selector to form diastereomers with analyte enantiomers, and comparison of the behaviors of diastereomers in MS. Chiral differentiation can be achieved by comparing the relative abundances of diastereomers, the thermodynamic or kinetic constants of ion-molecule reactions of diastereomers in the gas phase, the dissociation of diastereomers in MS/MS, or the mobility of diastereomers in ion mobility mass spectrometry. In this review, chiral recognition and determination of enantiomeric excess by these chiral MS methods were summarized, and the prospects of chiral analysis by MS were discussed. - Highlights: • Both chiral recognition and determination of enantiomeric excess by mass spectrometry are systematically reviewed. • Classification is based on the behavioral differences of diastereomers formed between chiral analytes and chiral selectors. • Development of ion mobility mass spectrometry for chiral differentiation is covered. • Various methods are highlighted and compared.

Chiral recognition and determination of enantiomeric excess by mass spectrometry: A review

Energy Technology Data Exchange (ETDEWEB)

Yu, Xiangying [College of Pharmacy, Jinan University, Guangzhou 510632, Guangdong (China); State Key Laboratory of Chinese Medicine and Molecular Pharmacology (Incubation) and Shenzhen Key Laboratory of Food Biological Safety Control, Shenzhen Research Institute of Hong Kong Polytechnic University, Shenzhen 518057 (China); Yao, Zhong-Ping, E-mail: zhongping.yao@polyu.edu.hk [State Key Laboratory of Chinese Medicine and Molecular Pharmacology (Incubation) and Shenzhen Key Laboratory of Food Biological Safety Control, Shenzhen Research Institute of Hong Kong Polytechnic University, Shenzhen 518057 (China); Key Laboratory of Natural Resources of Changbai Mountain and Functional Molecules (Yanbian University), Ministry of Education, Yanji 133002, Jilin (China); State Key Laboratory of Chirosciences, Food Safety and Technology Research Centre and Department of Applied Biology and Chemical Technology, The Hong Kong Polytechnic University, Hung Hom, Kowloon, Hong Kong Special Administrative Region (China)

2017-05-22

Chiral analysis is of great importance to fundamental and applied research in chemical, biological and pharmaceutical sciences. Due to the superiority of mass spectrometry (MS) over other analytical methods in terms of speed, specificity and sensitivity, chiral analysis by MS has attracted much interest in recent years. Chiral analysis by MS typically involves introduction of a chiral selector to form diastereomers with analyte enantiomers, and comparison of the behaviors of diastereomers in MS. Chiral differentiation can be achieved by comparing the relative abundances of diastereomers, the thermodynamic or kinetic constants of ion-molecule reactions of diastereomers in the gas phase, the dissociation of diastereomers in MS/MS, or the mobility of diastereomers in ion mobility mass spectrometry. In this review, chiral recognition and determination of enantiomeric excess by these chiral MS methods were summarized, and the prospects of chiral analysis by MS were discussed. - Highlights: • Both chiral recognition and determination of enantiomeric excess by mass spectrometry are systematically reviewed. • Classification is based on the behavioral differences of diastereomers formed between chiral analytes and chiral selectors. • Development of ion mobility mass spectrometry for chiral differentiation is covered. • Various methods are highlighted and compared.

Accelerated identification of proteins by mass spectrometry by employing covalent pre-gel staining with Uniblue A.

Directory of Open Access Journals (Sweden)

Marco A Mata-Gómez

Full Text Available BACKGROUND: The identification of proteins by mass spectrometry is a standard method in biopharmaceutical quality control and biochemical research. Prior to identification by mass spectrometry, proteins are usually pre-separated by electrophoresis. However, current protein staining and de-staining protocols are tedious and time consuming, and therefore prolong the sample preparation time for mass spectrometry. METHODOLOGY AND PRINCIPAL FINDINGS: We developed a 1-minute covalent pre-gel staining protocol for proteins, which does not require de-staining before the mass spectrometry analysis. We investigated the electrophoretic properties of derivatized proteins and peptides and studied their behavior in mass spectrometry. Further, we elucidated the preferred reaction of proteins with Uniblue A and demonstrate the integration of the peptide derivatization into typical informatics tools. CONCLUSIONS AND SIGNIFICANCE: The Uniblue A staining method drastically speeds up the sample preparation for the mass spectrometry based identification of proteins. The application of this chemo-proteomic strategy will be advantageous for routine quality control of proteins and for time-critical tasks in protein analysis.

A new generation of x-ray spectrometry UHV instruments at the SR facilities BESSY II, ELETTRA and SOLEIL

Energy Technology Data Exchange (ETDEWEB)

Lubeck, J., E-mail: janin.lubeck@ptb.de; Fliegauf, R.; Holfelder, I.; Hönicke, P.; Müller, M.; Pollakowski, B.; Ulm, G.; Weser, J.; Beckhoff, B. [Physikalisch-Technische Bundesanstalt (PTB), Abbestr. 2-12, 10587 Berlin (Germany); Bogovac, M.; Kaiser, R. B.; Karydas, A. G.; Leani, J. J.; Migliori, A.; Sghaier, H. [Nuclear Science and Instrumentation Laboratory, IAEA Laboratories, A-2444, Seibersdorf (Austria); Boyer, B.; Lépy, M. C.; Ménesguen, Y. [CEA, LIST, Laboratoire National Henri Becquerel, Bât. 602 PC 111, CEA-Saclay 91191 Gif-sur-Yvette c. (France); Detlefs, B. [CEA-LETI, Minatec Campus, 17 rue des Martyrs, 38054 Grenoble (France); Eichert, D. [Elettra - Sincrotrone Trieste (EST) S.C.p.A., 34149 Basovizza, Trieste (Italy); and others

2016-07-27

A novel type of ultra-high vacuum instrument for X-ray reflectometry and spectrometry-related techniques for nanoanalytics by means of synchrotron radiation (SR) has been constructed and commissioned at BESSY II. This versa-tile instrument was developed by the PTB, Germany’s national metrology institute, and includes a 9-axis manipulator that allows for an independent alignment of the samples with respect to all degrees of freedom. In addition, it integrates a rotational and translational movement of several photodiodes as well as a translational movement of a beam-geometry-defining aperture system. Thus, the new instrument enables various analytical techniques based on energy dispersive X-ray detectors such as reference-free X-Ray Fluorescence (XRF) analysis, total-reflection XRF, grazing-incidence XRF, in addition to optional X-Ray Reflectometry (XRR) measurements or polarization-dependent X-ray absorption fine structure analyses (XAFS). Samples having a size of up to (100 × 100) mm{sup 2}; can be analyzed with respect to their mass deposition, elemental, spatial or species composition. Surface contamination, nanolayer composition and thickness, depth pro-file of matrix elements or implants, nanoparticles or buried interfaces as well as molecular orientation of bonds can be accessed. Three technology transfer projects of adapted instruments have enhanced X-Ray Spectrometry (XRS) research activities within Europe at the synchrotron radiation facilities ELETTRA (IAEA) and SOLEIL (CEA/LNE-LNHB) as well as at the X-ray innovation laboratory BLiX (TU Berlin) where different laboratory sources are used. Here, smaller chamber requirements led PTB in cooperation with TU Berlin to develop a modified instrument equipped with a 7-axis manipulator: reduced freedom in the choice of experimental geometry modifications (absence of out-of-SR-plane and reference-free XRS options) has been compensated by encoder-enhanced angular accuracy for GIXRF and XRR.

Rocket-borne time-of-flight mass spectrometry

Science.gov (United States)

Reiter, R. F.

1976-01-01

Theoretical and numerical analyses are made of planar, cylindrical and spherical-electrode two-field time-of-flight mass spectrometers in order to optimize their operating conditions. A method is introduced which can improve the resolving power of these instruments by a factor of 7.5. Potential barrier gating in time-of-flight mass spectrometers is also analyzed. Experimental studies of a miniature cylindrical-electrode and a hemispherical-electrode time-of-flight mass spectrometer are presented. Their sensitivity and ability to operate at D-region pressures with an open source make them ideal instruments for D-region ion composition measurements. A sounding rocket experiment package carrying a cylindrical electrode time-of-flight mass spectrometer was launched. The data indicate that essentially 100% of the positive electric charge on positive ions is carried by ions with mass-to-charge ratios greater than 500 below an altitude of 92 km. These heavy charge carriers were present at altitudes up to about 100 km.

Rocket-borne time-of-flight mass spectrometry

International Nuclear Information System (INIS)

Reiter, R.F.

1976-08-01

Theoretical and numerical analyses are made of planar-, cylindrical- and spherical-electrode two-field time-of-flight mass spectrometers in order to optimize their operating conditions. A method is introduced which can improve the resolving power of these instruments by a factor of 7.5. Potential barrier gating in time-of-flight mass spectrometers is also analyzed. Experimental studies of a miniature cylindrical-electrode and a hemispherical-electrode time-of-flight mass spectrometer are presented. Their sensitivity and ability to operate at D-region pressures with an open source make them ideal instruments for D-region ion composition measurements. A sounding rocket experiment package carrying a cylindrical electrode time-of-flight mass spectrometer was launched. The data indicate that essentially 100% of the positive electric charge on positive ions is carried by ions with mass-to-charge ratios greater than 500 below an altitude of 92 km. These heavy charge carriers were present at altitudes up to about 100 km

Instrument development in support of Falcon and Phebus-FP

International Nuclear Information System (INIS)

Bowsher, B.R.; Brunning, J.

1992-12-01

This review has been undertaken to identify various on-line instruments and post-test analytical techniques that may improve the quality of data from both the Falcon Integral Test Programme and Phebus-FP. Particular emphasis is placed on the use of in-situ techniques to provide mass-based data on the aerodynamic properties of the aerosol and fission product-surface interactions. The principles of the following techniques are reviewed: cascade impactors, tapered element oscillating microbalance, condensation nucleus counter, Knudsen cell mass spectrometry, diffuse reflectance infrared Fourier transform spectrometry and secondary-ion mass spectrometry. These methods are currently being used in the Falcon experimental programme. (author)

Bayesian Integration and Characterization of Composition C-4 Plastic Explosives Based on Time-of-Flight Secondary Ion Mass Spectrometry and Laser Ablation-Inductively Coupled Plasma Mass Spectrometry

Energy Technology Data Exchange (ETDEWEB)

Mahoney, Christine M.; Kelly, Ryan T.; Alexander, M. L.; Newburn, Matthew K.; Bader, Sydney P.; Ewing, Robert G.; Fahey, Albert J.; Atkinson, David A.; Beagley, Nathaniel

2016-02-25

Key elements regarding the use of non-radioactive ionization sources will be presented as related to explosives detection by mass spectrometry and ion mobility spectrometry. Various non-radioactive ionization sources will be discussed along with associated ionization mechanisms pertaining to specific sample types.

Mass spectrometry. Environment, biology, oenology, medicine, geology, chemistry, archaeology, mechanisms; Spectrometrie de masse. Environnement, biologie, oenologie, medecine, geologie, chimie, archeologie, mecanismes

Energy Technology Data Exchange (ETDEWEB)

NONE

1999-07-01

This document provides the papers (communications and posters) presented at the 16. French days of mass spectrometry, held September 6-9, 1999 in Nancy, France. 7 papers are interesting for the ETDE database and are analyzed separately. (O.M.)

Mass spectrometry. Environment, biology, oenology, medicine, geology, chemistry, archaeology, mechanisms; Spectrometrie de masse. Environnement, biologie, oenologie, medecine, geologie, chimie, archeologie, mecanismes

Energy Technology Data Exchange (ETDEWEB)

NONE

1999-07-01

This document provides the papers (communications and posters) presented at the 16. French days of mass spectrometry, held September 6-9, 1999 in Nancy, France. 5 papers are interesting for the INIS database and are analyzed separately. (O.M.)

Next generation offline approaches to trace organic compound speciation: Approaching comprehensive speciation with soft ionization and very high resolution tandem mass spectrometry

Science.gov (United States)

Khare, P.; Marcotte, A.; Sheu, R.; Ditto, J.; Gentner, D. R.

2017-12-01

Intermediate- and semi-volatile organic compounds (IVOCs and SVOCs) have high secondary organic aerosol (SOA) yields, as well as significant ozone formation potentials. Yet, their emission sources and oxidation pathways remain largely understudied due to limitations in current analytical capabilities. Online mass spectrometers are able to collect real time data but their limited mass resolving power renders molecular level characterization of IVOCs and SVOCs from the unresolved complex mixture unfeasible. With proper sampling techniques and powerful analytical instrumentation, our offline tandem mass spectrometry (i.e. MS×MS) techniques provide molecular-level and structural identification over wide polarity and volatility ranges. We have designed a novel analytical system for offline analysis of gas-phase SOA precursors collected on custom-made multi-bed adsorbent tubes. Samples are desorbed into helium via a gradual temperature ramp and sample flow is split equally for direct-MS×MS analysis and separation via gas chromatography (GC). The effluent from GC separation is split again for analysis via atmospheric pressure chemical ionization quadrupole time-of-flight mass spectrometry (APCI-Q×TOF) and traditional electron ionization mass spectrometry (EI-MS). The compounds for direct-MS×MS analysis are delivered via a transfer line maintained at 70ºC directly to APCI-Q×TOF, thus preserving the molecular integrity of thermally-labile, or other highly-reactive, organic compounds. Both our GC-MS×MS and direct-MS×MS analyses report high accuracy parent ion masses as well as information on molecular structure via MS×MS, which together increase the resolution of unidentified complex mixtures. We demonstrate instrument performance and present preliminary results from urban atmospheric samples collected from New York City with a wide range of compounds including highly-functionalized organic compounds previously understudied in outdoor air. Our work offers new