No Cover Image

Journal article 775 views

Investigation of uremic analytes in hemodialysate and their structural elucidation from accurate mass maps generated by a multi-dimensional liquid chromatography/mass spectrometry approach / Ruth Godfrey, C. M Williams, Ed Dudley, R. P Newton, Peter Willshaw, A Mikhail, L Bastin, Anthony Brenton

Rapid Communications in Mass Spectrometry, Volume: 23, Issue: 19, Pages: 3194 - 3204

Swansea University Authors: Ruth Godfrey, Ed Dudley, Peter Willshaw, Anthony Brenton

Full text not available from this repository: check for access using links below.

Check full text

DOI (Published version): 10.1002/rcm.4235

Abstract

Historically, structural elucidation of unknown analytes by mass spectrometry alone has involved tandem mass spectrometry experiments using electron ionization. Most target molecules for bioanalysis in the metabolome are unsuitable for detection by this previous methodology. Recent publications have...

Full description

Published in: Rapid Communications in Mass Spectrometry
ISSN: 0951-4198 1097-0231
Published: Wiley 2009
Online Access: Check full text

URI: https://cronfa.swan.ac.uk/Record/cronfa6117
Tags: Add Tag
No Tags, Be the first to tag this record!
Abstract: Historically, structural elucidation of unknown analytes by mass spectrometry alone has involved tandem mass spectrometry experiments using electron ionization. Most target molecules for bioanalysis in the metabolome are unsuitable for detection by this previous methodology. Recent publications have used high-resolution accurate mass analysis using a LTQ-Orbitrap with the more modern approach of electrospray ionization to identify new metabolites of known metabolic pathways. We have investigated the use of this methodology to build accurate mass fragmentation maps for the structural elucidation of unknown compounds. This has included the development and validation of a novel multi-dimensional LC-MS/MS methodology to identify known uremic analytes in a clinical hemodialysate sample. Good inter and intra-day reproducibility of both chromatographic stages with a high degree of mass accuracy and precision was achieved with the multi-dimensional LC-MS/MS system. Fragmentation maps were generated most successfully using collision induced dissociation (CID) as unlike high energy CID (HCD), ions formed by this technique could be fragmented further. Structural elucidation is more challenging for large analytes >270 Da and distinguishing between isomers where their initial fragmentation pattern is insufficiently different. For small molecules (<200 Da), where fragmentation data may be obtained without loss of signal intensity, complete structures can be proposed from just the accurate mass fragmentation data. This methodology has led to the discovery of a selection of known uremic analytes and two completely novel moieties with chemical structural assignments made.
College: Swansea University Medical School
Issue: 19
Start Page: 3194
End Page: 3204