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J. Lipid Res.
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A more recent version of this article appeared on July 1, 2009

Papers In Press, published online ahead of print March 2, 2009
J. Lipid Res., doi:10.1194/jlr.M800478-JLR200
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Submitted on September 8, 2008
Revised on March 2, 2009
Accepted on March 2, 2009

Positive- and negative-tandem mass spectrometric fingerprints of lipids from the halophilic Archaea Haloarcula marismortui

Lauro M. de Souza, Marcelo Müller-Santos, Marcello Iacomini, Philip A. J. Gorin, and Guilherme L. Sassaki

Biochemistry and Molecular Biology, Universidade Federal do Paraná, Curitiba, Paraná 81531-980

Corresponding Author: sassaki{at}ufpr.br

Lipids from the extremely halophilic Archaea, Haloarcula marismortui, contain abundant phytanyl diether phospholipids, namely archaetidic acid (AA), archaetidylglycerol (AG), archaetidylglycerosulfate (AGS), with mainly archaetidylglycerophosphate methyl ester (AGP-Me). These were accompanied by a triglycosyl archaeol (TGA), lacking characteristic sulfate groups. Tandem-mass spectrometry was employed to provide fingerprints for identifying these known lipids, as well as small amounts of unsaturated phospholipids. These contained 3 and 6 double bonds in their archaeol moiety, suggested by negative tandem-MS of intact phospholipids, as indicated by differences between their pseudo-molecular ion and specific fragment ions designated as pi 2. The core ether lipids were confirmed by ESI-MS/MS as 2,3-di-O-phytanyl-sn-glycerol (C20, C20), which gave rise to a precursor-ion at m/z 660 [M+Li]+, and its fragment-ion at m/z 379 [M+Li]+, consistent with mono-O-phytanyl-glycerol. Furthermore, lithiated ions at m/z 654 (MS1), 379 (MS2) and m/z 648 (MS1), 373 (MS2), combined with 1H/13C NMR chemical shifts at delta 5.31-121.6 (C2/2’-H2/2’), 5.08-124.9 (C6/6’-H6/6’) and 5.10-126.0 (10/10’-H10/10’) confirmed the presence of unsaturated homologues of archaeol.


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