Quantitation of partial structures of aquatic humic substances by one- and two-dimensional solution 13C nuclear magnetic resonance spectroscopy

Buddrus, Joachim; Burba, P.; Lambert, Jörg; Herzog, H.

doi:10.1021/ac00181a027

Cited by 41 publications

(34 citation statements)

References 14 publications

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“…The most obvious choices for studies of NOM are DMSO -d 6 or D 2 O (or D 2 O/NaOD, depending on the solubility of the NOM). D 2 O and D 2 O/NaOD have been employed in numerous NOM studies (Buddrus et al, 1989 ;Larive et al, 1996 ;Dixon et al, 1999 ;Fan et al, 2000 ;Simpson et al, 2001c ;Wang et al, 2003 ;Hertkorn et al, 2004 ;Peuravuori, 2005 ) while others utilize DMSO -d 6 (Wais et al, 1996 ;Simpson, 2001 ;Simpson et al, 2003a ;Uyguner et al, 2004 ;Hertkorn et al, 2006 ;. D 2 O and D 2 O/NaOD have advantages in that the solution conformation adopted by the solute are likely to be more predictable than those adopted in DMSO.…”

Section: Sample Preparation For Solution -State Nmrmentioning

confidence: 99%

“…This section simply aims to provide the reader with an Barton and Schnitzer, 1963 ). Since then, NMR studies of NOM has progressed rapidly, with the fi rst applications of multidimensional solution -state NMR to study NOM occurring in 1989 (Buddrus et al, 1989 ). In the last 10 years the development of NMR experiments to study complex systems has expanded exponentially, mainly as a result of advances in the biomedical arena.…”

Section: Structural Studies Of Nommentioning

confidence: 99%

“…Thus, it is not surprising that in the last decade the application of multidimensional NMR has grown exponentially (Simpson et al, 1997(Simpson et al, , 2001a(Simpson et al, ,c, 2002a(Simpson et al, , 2003aHaiber et al, 1999Haiber et al, , 2001aFan et al, 2000 ;Kingery et al, 2000 ;Knicker, 2000a ;Simpson, 2001 ;Hertkorn et al, 2002bHertkorn et al, , 2006Cook et al, 2003 ;Kaiser et al, 2003 ;Kim et al, 2003 ;Cardoza et al, 2004 ;Mao and Schmidt -Rohr, 2006 ). In 1989, the fi rst applications of multidimensional NMR were applied to humic substances (Buddrus et al, 1989 ). This study involved the application of 13 C detected J -resolved (J -Res) spectroscopy.…”

Section: Structural Studies Of Nommentioning

confidence: 99%

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Nuclear Magnetic Resonance Analysis of Natural Organic Matter

Simpson

2009

Biophysico‐Chemical Processes Involving Natural Nonliving Organic Matter in Environmental Systems

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Section: Sample Preparation For Solution -State Nmrmentioning

confidence: 99%

Section: Structural Studies Of Nommentioning

confidence: 99%

Section: Structural Studies Of Nommentioning

confidence: 99%

See 1 more Smart Citation

Nuclear Magnetic Resonance Analysis of Natural Organic Matter

Simpson

2009

Biophysico‐Chemical Processes Involving Natural Nonliving Organic Matter in Environmental Systems

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“…The linkage points of the reserve glucan of the prymnesiophyte Emiliania huxleyi have been investigated using 13 C-NMR , and the structure of sulfated galactans isolated from the macrophyte Furcellaria lumbricalis was studied using both 13 C-and 1 H-NMR (Knutsen et al, 1990). Carbon-13 NMR has also been used for gross characterization of humic materials isolated from groundwater (Buddrus et al, 1989;Lambert et al, 1992) and soils (Wershaw et al, 1990). Solid-state 13 C-NMR has been used to characterize green algae Saito et al, 1991) and decaying mangrove leaves (Benner et al, 1990).…”

Section: Thesis Goal: a New Approach To Early Diagenesismentioning

confidence: 99%

Structural characterization and bacterial degradation of marine carbohydrates

Arnosti¹

1993

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The goal of this thesis was to develop and apply an integrated chemical and microbial approach to study the effects of chemical structure on the rates and patterns of carbohydrate degradation by anaerobic marine bacteria.Polysaccharides produced by five species of marine plankton, Dunaliella tertiolecta, Emiliania huxleyi, Stephanopixis palmeri, a Phaeocystis sp., and Synechococcus WH7335, were surveyed using one-and two-dimensional nuclear magnetic resonance spectroscopy (NMR). Two carbohydrates from Synechococcus WH7335 were characterized in detail. Synechococcus produced an a(1,4) glucose polysaccharide with a(1,6) branches, which probably functions as an energy reserve. The nominal molecular weight of the polysaccharide was -5000 daltons. Large quantities of a glycerolpolysaccharide, which was tentatively identified as a teichoic acid similar in structure to teichoic acids found in cell walls of gram-positive bacteria, were also produced by Synechococcus WH7335. This is the first report of teichoic acids in cyanobacteria.Enrichment of bacteria from anoxic marine sediments on specific carbohydrates yielded reproducible model systems with which to study the degradation of chemically well-defined substrates. Headspace gases (CO 2 , H 2 , CH4, H 2 S) were monitored by gas chromatography, and carbohydrate substrates and intermediates were separated and quantified via gel-permeation chromatography and high-pressure liquid chromatography. The transfer of carbon from substrates through to end products was followed quantitatively. Nuclear magnetic resonance spectroscopy was used to check for selective structural alterations (such as preferential cleavage of specific linkage types or positions) of the substrates.A series of enrichment experiments showed that mixed cultures of marine bacteria distinguish even between small, very closely-related substrates which do not require extracellular hydrolysis prior to uptake. A galactose-13(1,3)-arabinose dimer was degraded at half the rate of seven other similar disaccharides and three larger oligosaccharides. A further series of degradation experiments with polysaccharides (pullulan, laminarin) showed that they are degraded by bacteria at virtually the same rate as structurally related substrates in the molecular weight range of 300-600 daltons. Degradation of the branched glucan and the teichoic acid-type polysaccharide from Synechococcus WH7335 was also very rapid.The time-course of bacterial hydrolysis of pullulan was examined with gel permeation chromatography and NMR to provide the first molecular-level evidence in marine systems of the bacterial extracellular transformation of high molecular weight organic matter to lower molecular weight organic matter. NMR spectra provided evidence that the pullulan was hydrolyzed by pullulanase, an endo-acting extracellular enzyme which preferentially hydrolyzes a(1,6) linkages. This is the first experimental evidence of pullulanase activity among marine mesophilic bacteria.The culture results suggest that enzymatic hydrolysi...

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“…Unfortunately, polarisation transfer and 2D NMR techniques have had limited application in the characterisation of SOM. The spectra obtained to date have been at relatively low magnetic¯elds ranging up to 9 T [4,5,6,7], allowing low dispersion.…”

Section: Introductionmentioning

confidence: 99%

13C NMR and mass spectrometry of soil organic matter

Ivanova

Randall

2003

Open Chemistry

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Liquid state, high resolution 13 C NMR spectroscopy and mass spectrometry were used to study the composition and structure of soil organic matter (SOM) using soil extracts from two long-term experiments at the Rothamsted Experimental Station. Both one-and two-dimensional NMR techniques were applied. 13 C NMR sub-spectra of the CH n (n = 0 : : : 3) groups, obtained by the Distortionless Enhancement by Polarisation Transfer (DEPT) technique, were used for the elucidation of the qualitative and quantitative composition of humic and fulvic acids in the soils. The chemical structure of SOM was further analysed at the molecular level through Fast Atom Bombardment Mass Spectrometry (FABMS) and Gas Chromatography-Mass Spectrometry (GC/MS). Humic and fulvic extract results were not only compared to each other, but also to the solid state 13 C NMR results for the complete soil sample.

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Quantitation of partial structures of aquatic humic substances by one- and two-dimensional solution 13C nuclear magnetic resonance spectroscopy

Cited by 41 publications

References 14 publications

Nuclear Magnetic Resonance Analysis of Natural Organic Matter

Nuclear Magnetic Resonance Analysis of Natural Organic Matter

Structural characterization and bacterial degradation of marine carbohydrates

13C NMR and mass spectrometry of soil organic matter

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