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Open AccessArticle

Multiple-stage Precursor Ion Separation and High Resolution Mass Spectrometry toward Structural Characterization of 2,3-Diacyltrehalose Family from Mycobacterium tuberculosis

1
Department of Medicine, Washington University School of Medicine, St. Louis, MO 63110, USA
2
Department of Microbiology and Molecular Genetics, Michigan State University, East Lansing, MI 48824, USA
3
Department of Molecular Microbiology and Immunology, Oregon Health & Science University, Portland, OR 97239, USA
4
Univ Rennes, Ecole Nationale Supérieure de Chimie de Rennes, CNRS, ISCR–UMR 6226, F-35000 Rennes, France
*
Author to whom correspondence should be addressed.
These authors contributed equally as co-first author.
Separations 2019, 6(1), 4; https://doi.org/10.3390/separations6010004
Received: 1 December 2018 / Revised: 2 January 2019 / Accepted: 7 January 2019 / Published: 15 January 2019
(This article belongs to the Special Issue Five Years of Separations: Feature Paper 2018)
Mass spectrometry (MS)-based precursor ion isolation, collision-induced dissociation (CID) fragmentation, and detection using linear ion-trap multiple-stage mass spectrometry (LIT MSn) in combination with high resolution mass spectrometry (HRMS) provides a unique tool for structural characterization of complex mixture without chromatographic separation. This approach permits not only separation of various lipid families and their subfamilies, but also stereoisomers, thereby, revealing the structural details. In this report, we describe the LIT MSn approach to unveil the structures of a 2,3-diacyl trehalose (DAT) family isolated from the cell envelope of Mycobacterium tuberculosis, in which more than 30 molecular species, and each species consisting of up to six isomeric structures were found. LIT MSn performed on both [M + Na]+ and [M + HCO2] ions of DAT yield complimentary structural information for near complete characterization of the molecules, including the location of the fatty acyl substituents on the trehalose backbone. This latter information is based on the findings of the differential losses of the two fatty acyl chains in the MS2 and MS3 spectra; while the product ion spectra from higher stage LIT MSn permit confirmation of the structural assignment. View Full-Text
Keywords: tandem mass spectrometry; linear ion trap; glycolipid; diacyltrehalose; Mycobacterium tuberculosis tandem mass spectrometry; linear ion trap; glycolipid; diacyltrehalose; Mycobacterium tuberculosis
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MDPI and ACS Style

Frankfater, C.; Abramovitch, R.B.; Purdy, G.E.; Turk, J.; Legentil, L.; Lemiègre, L.; Hsu, F.-F. Multiple-stage Precursor Ion Separation and High Resolution Mass Spectrometry toward Structural Characterization of 2,3-Diacyltrehalose Family from Mycobacterium tuberculosis. Separations 2019, 6, 4.

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