scholarly journals Multiplexed Single Ion Mass Spectrometry Improves Measurement of Proteoforms and Their Complexes

2019 ◽  
Author(s):  
Jared O. Kafader ◽  
Rafael D. Melani ◽  
Kenneth R. Durbin ◽  
Bon Ikwuagwu ◽  
Bryan P. Early ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Mass Spectra ◽  
Analysis Procedure ◽  
Modes Of Operation ◽  
Charge Detection ◽  
Individual Protein ◽  
Protein Ions ◽  
True Mass ◽  
Ion Analysis

AbstractA new Orbitrap-based single ion analysis procedure is shown to be possible by determining the direct charge on numerous measurements of individual protein ions to generate true mass spectra. The deployment of an Orbitrap system for charge detection enables the characterization of highly complicated mixtures of proteoforms and their complexes in both denatured and native modes of operation, revealing information not obtainable by traditional measurement of an ensemble of ions.

scholarly journals MASS SPECTROMETRIC CHARACTERIZATION OF PLASMA MEBEVERINE METABOLITES AND ITS SYNTHESIS

2019 ◽  
Vol 16 (32) ◽  
pp. 633-646
Author(s):  
Natalia E. MOSKALEVA ◽  
Roman M. KUZNETZOV ◽  
Pavel A. MARKIN ◽  
Svetlana A. APPOLONOVA
Keyword(s):  
Mass Spectrometry ◽  
Blood Plasma ◽  
Mass Spectra ◽  
Human Blood Plasma ◽  
Veratric Acid ◽  
First Order ◽  
Flight Mass Spectrometry ◽  
Before And After ◽  
Irritable Bowel

Mebeverine is a musculotropic antispasmodic drug that is widely used in the treatment of irritable bowel syndrome. As an ester of mebeverine alcohol and veratric acid, mebeverin is quickly metabolized and is practically undetectable in blood plasma. The main goal of this work was establishing the structure of the main metabolites of mebeverin in human blood plasma. The study was conducted by time-of-flight mass spectrometry (LC-IT-TOF MS), metabolites of mebeverine were extracted from plasma with acetonitrile. When comparing chromatograms of blood plasma obtained before and after drug administration, four main peaks of metabolites were detected. To establish the structure of the compounds, mass spectra of the first and second order were taken. The first-order spectra were used to calculate the metabolite formula and the structure was determined from the fragmentation spectra, as well as by comparing the fragmentation spectra of mebeverine and its proposed metabolites. The proposed compounds were synthesized, and their structure was confirmed using NMR and chromatography-mass spectrometry. Four main metabolites were found in this study: desmethylmebeverine acid (DMAC), glucuronide product of DMAC (DMAC-Glu), mebeverine acid (MAC) and mebeverine alcohol (MAL). The results complement the available literature data about the veratric acid metabolism, urine, and microsomal studies. According to the data obtained, the main metabolite of mebeverine in the blood is DMAC. The concentration of MAC after mebeverine administration is almost ten times less than DMAC, the content of MAL and DMAC-Glu is insignificant, and probably does not affect the pharmacological effect of mebeverine. Therefore, the concentration of DMAC is the main parameter to be monitored in pharmacokinetics studies.

Characterization of Classical Vaccines by Charge Detection Mass Spectrometry

2021 ◽  
Vol 93 (35) ◽  
pp. 11965-11972 ◽  
Author(s):  
Lohra M. Miller ◽  
Kevin M. Bond ◽  
Benjamin E. Draper ◽  
Martin F. Jarrold
Keyword(s):  
Mass Spectrometry ◽  
Charge Detection Mass Spectrometry ◽  
Charge Detection

scholarly journals Characterization of aliphatic hyperbranched polyesters by MALDI-TOF mass spectrometry

2007 ◽  
Vol 61 (6) ◽  
pp. 333-341
Author(s):  
Jasna Vukovic ◽  
Slobodan Jovanovic ◽  
Manfred Lechner
Keyword(s):  
Mass Spectrometry ◽  
Mass Spectra ◽  
Degree Of Polymerization ◽  
Side Reactions ◽  
Maldi Tof Ms ◽  
Hyperbranched Polyesters ◽  
Maldi Tof ◽  
Maldi Tof Mass Spectra ◽  
Tof Ms

In this work, MALDI-TOF mass spectrometry was used for the characterization of aliphatic hyperbranched polyesters (AHBP), synthesized from 2,2-bis(hydroxymethyl)propionic acid (bis-MPA) and di-trimethylolpropane. From the obtained results it was concluded that it was not possible to take complete advantages of MALDI-TOF MS in this particular case, since the AHBP used in this work were polydisperse. The intensity of the signals from the high mass tail of these samples (pseudo generation higher than four) was underestimated and insufficient to distinguish it from the baseline and to use it for the analysis of the spectra. As a consequence of that, lower values of the Mn were obtained. At the same time, Mw were also underestimated, which led to very low values of the polydispersity index. On the other hand, it was possible to obtain molar masses of individual molecules from the MALDI-TOF mass spectra of AHBP and to qualitatively determine the extent of cyclization (side reactions) at each degree of polymerization. Using the adequate set of equations and results obtained from MALDI-TOF mass spectra of AHBP, every signal from the spectra was identified. The obtained results show that formation of poly(bis-MPA), intramolecular esterification and intramolecular etherification occurred as side reactions during the synthesis of these polyesters. The relative amount of the cycles increases with the number of pseudo generation (from the second up to the fifth pseudo generation). It was also observed that the relative proportion of the signals which represent cyclic structures increases with the increasing degree of polymerization. In this work the basic principles of MALDI-TOF MS are also presented, as well as, a review of adequate published articles.

scholarly journals Dereplikace látek a de novo charakterizace malých molekul z hmotnostních spekter

2022 ◽  
Vol 116 (1) ◽  
pp. 11-19
Author(s):  
Jiří Novák ◽  
Vladimír Havlíček
Keyword(s):  
Mass Spectrometry ◽  
Small Molecules ◽  
Mass Spectra ◽  
De Novo ◽  
Imaging Mass Spectrometry ◽  
Mass Spectrometry Data ◽  
Data Sets ◽  
Liquid Chromatography Mass Spectrometry ◽  
Imaging Mass Spectrometry Data

We describe the molecular dereplication principles and de novo characterization of small molecules obtained from liquid-chromatography mass spectrometry and imaging mass spectrometry data sets. Our methodology aims at supporting chemists and computer programmers to understand the hidden computing algorithms used for metabolomics mass spectrometry data processing. The approaches have been made available in the open-source tool CycloBranch. The presented tutorial extends the interpretation of mass spectra portfolia described in a series of papers published in Chemicke Listy, issues 2/2020 and 3/2020.

Liquid Secondary Ion Mass Spectrometry and Collision-induced Dissociation Mass Spectrometry of Sulfonamide Derivatives of meso-Tetraphenylporphyrin

1999 ◽  
Vol 03 (03) ◽  
pp. 172-179 ◽  
Author(s):  
M. ROSÁRIO M. DOMINGUES ◽  
M. GRAÇA SANTANA-MARQUES ◽  
A. J. FERRRER-CORREIA ◽  
AUGUSTO C. TOMÉ ◽  
MARIA G. P. M. S. NEVES ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Mass Spectra ◽  
Secondary Ion Mass Spectrometry ◽  
Molecular Ions ◽  
Collision Induced Dissociation ◽  
Fragment Ions ◽  
Ion Mass Spectrometry ◽  
Derivatives Of ◽  
Secondary Ion

Liquid secondary ion mass spectrometry (LSIMS) and collision-induced dissociation (CID) were used for the characterization of sulfonamide derivatives of meso-tetraphenylporphyrin (TPP). The spectra obtained using LSIMS show abundant molecular ions and fragment ions from losses of the sulfonamide moieties. The main fragmentation observed in the LSI mass spectra and in the CID spectra of the protonated or cationized molecules involves the loss of one sulfonamide group. In addition, in the CID spectra of these compounds the fragment ions formed by the elimination of two, three and/or four sulfonamide groups are also observed. The CID spectra of the protonated or cationized molecules of these derivatives do not display the ions formed by the cleavage of the S - N bond which have been reported for other sulfonamide compounds. The LSI mass spectra and CID spectra of sulfonamide derivatives of meso-tetraphenylporphyrin provide an easy and reliable means of identification of the number and nature of sulfonamide groups in the porphyrinic ring.

Structural Characterization of Fucose-Containing Oligosaccharides by High-Performance Liquid Chromatography and Matrix-Assisted Laser Desorption/ Ionization Time-of-Flight Mass Spectrometry

2001 ◽  
Vol 382 (2) ◽  
pp. 251-257 ◽  
Author(s):  
Minoru Suzuki ◽  
Akemi Suzuki
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Structural Characterization ◽  
High Performance ◽  
Mass Spectra ◽  
Laser Desorption ◽  
Laser Desorption Ionization ◽  
Column Temperature ◽  
Desorption Ionization

Abstract Eight pyridylamino (PA) derivatives of fucosecontaining oligosaccharides, which occur as free oligosaccharides in human milk and also are derived from glycosphingolipids, have been analyzed by highperformance liquid chromatography (HPLC) on normalphase and reversedphase columns, and by matrixassisted laser desorption/ionization timeofflight MALDITOF) mass spectrometry. Six out of eight PAoligosaccharides were clearly separated by both normal and reversedphase HPLC at a column temperature of 40 C, but two PAoligosaccharides, lactoNfucopentaose II [Gal?1-3(Fuc?1-4)GlcNAc?1- 3Gal?1-4GlcPA] and lactoNfucopentaose III Gal?1-4(Fuc?1-3)GlcNAc?1-3Gal?1-4GlcPA], were not separated. The two unresolved PAoligosaccharides were finally separated by reversedphase HPLC at a column temperature of 11 C. MALDITOF mass spectra of PAoligosaccharides demonstrated pseudomolecular ions as the predominant signals, therefore information about the molecular mass of each PAoligosaccharide was easily obtained. Postsource decay (PSD) MALDITOF mass spectra of PAoligosaccharides gave information about the carbohydrate sequences and carbohydrate species of each PAoligosaccharide by detecting the ions responsible for the cleavage of the glycosidic bonds. The detection limits of the PAoligosaccharides by HPLC, MALDITOF mass spectrometry, and PSD MALDITOF mass spectrometry were 20 fmol, 20 fmol, and 2 pmol, respectively. These results suggest that a system including HPLC and MALDITOF mass spectrometry or HPLC and PSD MALDITOF mass spectrometry is quite useful for the structural characterization of subpmol or pmol levels of fucosecontaining oligosaccharides, and that these methods could be used for the analysis of various types of oligosaccharides derived from glycoproteins and glycosphingolipids.

Gas Chromatographic and Mass Spectrometric Characterization of Impurities in Technical Methoxychlor

1980 ◽  
Vol 63 (5) ◽  
pp. 1007-1037
Author(s):  
Carolejean H Lamoureux ◽  
Vernon J Feil
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Mass Spectra ◽  
Mass Spectrometric ◽  
Gas Chromatography Mass Spectrometry ◽  
Chromatography Mass Spectrometry

Abstract The impurities in technical methoxychlor were concentrated by removing most of the 1,1,1-trichloro-2,2-bis(4-methoxyphenyl)ethane by recrystallization. Analysis of the impurities by gas chromatography–mass spectrometry provided evidence for more than 50 compounds. Twenty-five of these were identified through interpretation of mass spectra and synthesis.

scholarly journals Assessment of genome packaging in AAVs using Orbitrap-based charge detection mass spectrometry

2021 ◽  
Author(s):  
Tobias P Woerner ◽  
Joost Snijder ◽  
Olga Friese ◽  
Thomas W Powers ◽  
Albert J.R. Heck
Keyword(s):  
Mass Spectrometry ◽  
High Demand ◽  
Genome Packaging ◽  
Charge Detection Mass Spectrometry ◽  
Charge Detection ◽  
Essential Step ◽  
Gene Therapy Vectors ◽  
Effective Drugs ◽  
Limited Sensitivity

Adeno-associated viruses (AAV) represent important gene therapy vectors with several approved clinical applications and numerous more in clinical trials. Genome packaging is an essential step in the bioprocessing of AAVs and needs to be tightly monitored to ensure the proper delivery of transgenes and the production of effective drugs. Current methods to monitor genome packaging have limited sensitivity, a high demand on labour, and struggle to distinguish between packaging of the intended genome or unwanted side-products. Here we show that Orbitrap based charge detection mass spectrometry allows the ultra-sensitive quantification of all these different AAV bioprocessing products. A protocol is presented that allows the quantification of genome packed AAV preparations in under half an hour, requiring only micro-liter quantities of typical AAV preparations with ~1013 viral genome copies per millilitre. The method quickly assesses the integrity and amount of genome packed AAV particles to support AAV bioprocessing and characterization of this rapidly emerging class of advanced drug therapies.

The Generation of Low-Valence Tin Derivatives, RSn(I), in the Gas-Phase by Neutralization—reionization Mass Spectrometry

2002 ◽  
Vol 8 (5) ◽  
pp. 351-357 ◽  
Author(s):  
Dmitri Zagorevskii ◽  
Yang Yuan ◽  
C. Michael Greenlief ◽  
Alexander A. Mommers
Keyword(s):  
Mass Spectrometry ◽  
Gas Phase ◽  
Quantum Chemical Calculations ◽  
Molecular Species ◽  
Quantum Chemical ◽  
Mass Spectra ◽  
Stable Species ◽  
The Stability ◽  
Franck Condon

Neutralization-reionization mass spectrometry (NRMS) was applied to the generation and characterization of low-valence Sn(I) derivatives. The observation of recovery signals in the NR mass spectra of RSn+ ions (R=H, Cl, Br, CH3, C2H, C6H5) demonstrated that their neutral counterparts are stable species in the gas-phase with a lifetime of at least 5 μs. According to quantum chemical calculations, a favorable Franck–Condon factor may contribute to the stability of RSn neutrals generated in the NR event. The experimental results for tin acetylide and phenyltin are the first examples of the generation of these previously unknown molecular species.

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