scholarly journals Discrimination of GalNAc (4S/6S) sulfation sites in chondroitin sulfate disaccharides by chip-based nanoelectrospray multistage mass spectrometry

2009 ◽  
Vol 7 (4) ◽  
pp. 752-759 ◽  
Author(s):  
Corina Flangea ◽  
Alina Serb ◽  
Catalin Schiopu ◽  
Sorin Tudor ◽  
Eugen Sisu ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Chondroitin Sulfate ◽  
Ion Trap ◽  
High Capacity ◽  
Ester Group ◽  
Negative Ion ◽  
Post Translational Modification ◽  
Spectrometric Data ◽  
Group Position ◽  
Fragmentation Patterns

AbstractSulfation pattern within chondroitin sulfate (CS) glycosaminoglycan (GAG) chains is an important post-translational modification that regulates their interaction with proteins. In this context, development of highly efficient and reproducible analytical methods for the investigation of CS sulfation patterns is of high necessity. In this study we report a novel method for straightforward determination of N-acetylgalactosamine (GalNAc) sulfation sites in chondroitin sulfate disaccharides. Our protocol involves combining fully automated chip-based nanoelectrospray (nanoESI) for analyte infusion and ionization in negative ion mode with multistage (MSn) collision-induced dissociation (CID) high capacity ion trap (HCT) mass spectrometry for generation of sequence ions diagnostic for identification of sulfate ester group position within GalNAc residues. The feasibility of this approach is here demonstrated on chondroitin 6-O-sulfate and chondroitin 4-O-sulfate disaccharides. Fragmentation patterns obtained by MS2 and MS3 sequencing stages provided first mass spectrometric data from which sulfation site(s) within GalNAc monosaccharide ring could be unequivocally deciphered. Hence, the method allowed discriminating 4S/6S sulfation sites solely on the basis of MS and multistage MS evidence.

Identification of Phosphorylcholine-Substituted Peptides by Their Characteristic Mass Spectrometric Fragmentation

2005 ◽  
Vol 11 (3) ◽  
pp. 335-344 ◽  
Author(s):  
Julia Grabitzki ◽  
Volker Sauerland ◽  
Rudolf Geyer ◽  
Günter Lochnit
Keyword(s):  
Mass Spectrometry ◽  
Ion Trap ◽  
Neutral Loss ◽  
Structural Data ◽  
Mass Spectrometric ◽  
Peptide Backbone ◽  
Fragmentation Behavior ◽  
Flight Mass Spectrometry ◽  
Characteristic Fragmentation ◽  
Fragmentation Patterns

Phosphorylcholine (PC)-substituted biomolecules are wide-spread, highly relevant antigens of parasites, since this small hapten has been found to be a potent immunomodulatory component which allows the establishment of long lasting infections of the host. Structural data, especially of protein bound PC-substituents, are still rare due to the observation that mass spectrometric analyses are mostly hampered by this zwitterionic substituent resulting in low sensitivities and unusual but characteristic fragmentation patterns. Here, we investigated the fragmentation behavior of synthetic PC-substituted peptides by matrix-assisted laser desorption/ionization time-of-flight mass spectrometry and electrospray ionization ion-trap mass spectrometry. We could show that the predominant neutral loss of a trimethylamine unit (Hoffmann elimination) leads to cyclic phosphate derivatives which prevent further fragmentation of the peptide backbone by stabilizing the positive charge at this particular side chain. Knowledge of this PC-specific fragmentation might help to identify PC-substituted biomolecules and facilitate their structural analysis.

scholarly journals Isolation and Identification of Chemical Constituents from Zhideke Granules by Ultra-Performance Liquid Chromatography Coupled with Mass Spectrometry

2020 ◽  
Vol 2020 ◽  
pp. 1-16
Author(s):  
Guangqiang Huang ◽  
Jie Liang ◽  
Xiaosi Chen ◽  
Jing Lin ◽  
Jinyu Wei ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Chemical Constituents ◽  
Relevant Literature ◽  
Ultra Performance Liquid Chromatography ◽  
Negative Ion ◽  
Volatile Components ◽  
Isolation And Identification ◽  
Fragmentation Patterns ◽  
Nitrogen Containing Compounds

Chemical constituents from Zhideke granules were rapidly isolated and identified by ultra-performance liquid chromatography (UPLC) coupled with hybrid quadrupole-orbitrap mass spectrometry (MS) in positive and negative ion modes using both full scan and two-stage threshold-triggered mass modes. The secondary fragment ion information of the target compound was selected and compared with the compound reported in databases and related literatures to further confirm the possible compounds. A total of 47 chemical constituents were identified from the ethyl acetate extract of Zhideke granules, including 21 flavonoids and glycosides, 9 organic acids, 4 volatile components, 3 nitrogen-containing compounds, and 10 other compounds according to the fragmentation patterns, relevant literature, and MS data. The result provides a new method for the analysis of chemical constituents of Zhideke granules which laid the foundation for quality control and the study of pharmacodynamic materials of Zhideke granules.

scholarly journals Characterization of Flavonoid and Naphthopyranone Derivatives from Eriocaulon ligulatum using Liquid Chromatography Tandem Mass Spectrometry

2009 ◽  
Vol 4 (12) ◽  
pp. 1934578X0900401 ◽  
Author(s):  
Lourdes Campaner dos Santos ◽  
Marcelo Aparecido da Silva ◽  
Clenilson Martins Rodrigues ◽  
Virginia Carbone ◽  
Assunta Napolitano ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Methanol Extract ◽  
Ion Trap ◽  
Ion Trap Mass Spectrometry ◽  
Chromatography Tandem Mass Spectrometry ◽  
Liquid Chromatography Tandem Mass ◽  
Fragmentation Patterns

Liquid chromatography-electrospray ionization multistage ion trap mass spectrometry (LC-ESI-IT-MSn) was used to analyze the secondary metabolites in the methanol extract of the capitulae of Eriocaulon ligulatum. The major components were mono-and diglycosides of flavonoids and naphthopyranones. Eleven compounds, including four new flavonol glycosides, were identified based on their fragmentation patterns in MS experiments and on NMR analysis of the isolated compounds. The described data may contribute to a better understanding of the taxonomic classification of the Eriocaulaceae family.

scholarly journals Capillary Gas Chromatography/Mass Spectrometry with Chemical Ionization and Negative Ion Detection for Confirmation of Identity of Patulin in Apple Juice

2000 ◽  
Vol 83 (1) ◽  
pp. 104-112 ◽  
Author(s):  
John A G Roach ◽  
Kevin D White ◽  
Mary W Trucksess ◽  
Frederick S Thomas
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Chemical Ionization ◽  
Apple Juice ◽  
Ion Trap ◽  
Quadrupole Ion Trap ◽  
Capillary Columns ◽  
Negative Ion ◽  
Gas Chromatography Mass Spectrometry ◽  
Chromatography Mass Spectrometry

Abstract Gas chromatography/mass spectrometry (GC/MS) with negative ion chemical ionization permits detection of underivatized patulin in apple juice extracts while minimizing co-extractive responses. The technique has been used with a variety of capillary columns in quadrupole, ion trap, and magnetic sector GC/MS instruments to confirm presumptive findings of patulin in apple juice at concentrations ranging from 68 to 3700 μg/L. The demonstrated ability to use any of these 3 mass spectrometers and several capillary columns to confirm the identity of patulin are significant strengths of the technique.

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