Journal
ORGANIC GEOCHEMISTRY
Volume 85, Issue -, Pages 22-31Publisher
PERGAMON-ELSEVIER SCIENCE LTD
DOI: 10.1016/j.orggeochem.2015.04.007
Keywords
Sediment organic matter; H-1 liquid state nuclear magnetic resonance (NMR) spectroscopy; Fourier transform ion cyclotron resonance mass spectrometry; Electrospray ionisation; Extraction solvent; Pyridine
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Funding
- Batten Endowment Fund at Old Dominion University
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Fourier transform ion cyclotron resonance mass spectrometry (FTICRMS) can begin to tease apart the molecular character of sedimentary organic matter (SOM). We therefore tested five different solvents (aqueous base, CHCl3, MeOH, pyridine and water) for their ability to extract a representative fraction from two organic rich lacustrine sediments, Mangrove Lake, Bermuda (MLB) and Mud Lake, Florida (MLF). Following comparison using liquid state nuclear magnetic resonance spectroscopy (NMR) and negative ion mode electrospray ionization mass spectrometry (FTICRMS) we found that pyridine was the optimal solvent, extracting a more diverse (10-100 x greater integration for carbonyl, amide and amine groups) and a larger number of peaks on average (1375-1450 vs. 380-1450). Comparison of the pyridine extracts between MLB, MLF and two organic poor sediments from the Mississippi River Delta and Bayou Grande (Pensacola, FL) showed that only 4.9% of the molecular formulae were common to all four and that unique formulae made up the highest proportion of the assignments. The use of pyridine for extracting immature (Holocene) SOM for FTICRMS analysis can therefore be widely applied to immature sediments and produce representative spectra. (C) 2015 Elsevier Ltd. All rights reserved.
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