Combining advanced NMR techniques with ultrahigh resolution mass spectrometry: A new strategy for molecular scale characterization of macromolecular components of soil and sedimentary organic matter

Zhong, Junyan; Sleighter, Rachel L.; Salmon, Élodie; McKee, Georgina A.; Hatcher, Patrick G.

doi:10.1016/j.orggeochem.2011.04.007

Cited by 37 publications

(23 citation statements)

References 46 publications

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“…The sorption of three different dissolved OM samples that were isolated from Peat humic acid (PHA), a forest soil and Leonardite humic acid (LHA) to Ca 2þ enriched kaolinite and montmorillonite was studied using 1 H high-resolution magic-angle-spinning (HR-MAS) NMR spectroscopy which enables the analysis of semisolid phase compounds that are in contact with the NMR solvent. [21,28,29] 1 H HR-MAS NMR spectroscopy has been used successfully in the past to study dissolved OM sorption to clay mineral surfaces [15,21] and OM at the solvent-solid interface in whole soils and sediments. [28,29] We also examined the structural composition of the dissolved OM samples before sorption using solution-state 1 H NMR spectroscopy.…”

Section: Introductionmentioning

confidence: 99%

Analysis of soil organic matter at the solid–water interface by nuclear magnetic resonance spectroscopy

Genest

Simpson

et al. 2014

Environ. Chem.

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Environmental context. Structural and conformational information on organic matter-clay complexes and whole soils was obtained using different NMR methods. The results show that organic matter interactions with clay mineral surfaces determine the accessibility of specific organic matter components at the soil-water interface. This physical conformation may also play a role in soil biogeochemical processes and binding to pollutants in terrestrial environments.Abstract. Organic matter (OM)-mineral interactions play an important role in OM preservation, global carbon cycling and contaminant transport. Studies have indicated that preferential sorption of OM is dependent on mineral type and solution conditions. In this study, 1 H high resolution-magic angle spinning nuclear magnetic resonance (HR-MAS NMR) spectroscopy was employed to examine OM chemistry in organo-clay complexes. Dissolved OM from a forest soil, Leonardite humic acid and Peat humic acid were sorbed to Ca 2þ enriched kaolinite and montmorillonite. As observed using 1 H HR-MAS NMR spectroscopy, kaolinite sorbed mainly long-chain aliphatic compounds such as those from plant cuticles whereas montmorillonite sorbed a mixture of aliphatic components and proteins. These results show the preferential sorption of specific dissolved OM components on clay surfaces. This was tested further using solid-state 13 C and 1 H HR-MAS NMR analysis of whole soils containing kaolinite and montmorillonite as well as a Peat soil for contrast. The species present at the soil-water interface were mainly aliphatic components, carbohydrates and amino acids. Aromatic constituents were present in the soils (observed by solid-state 13 C NMR and by 1 H HR-MAS NMR spectroscopy when a more penetrating solvent was used) which signifies that these compounds likely exist in more hydrophobic domains that are buried and surface inaccessible. This study highlights the important role of OM interactions with clay minerals in the preservation of OM in soils and suggests that OM-OM associations may also play a role in the protection of specific OM components in soil.

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Section: Introductionmentioning

confidence: 99%

Analysis of soil organic matter at the solid–water interface by nuclear magnetic resonance spectroscopy

Genest

Simpson

et al. 2014

Environ. Chem.

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“…Interestingly, this work showed that HRMAS applied to the whole NOM samples was superior to the traditional liquid-state NMR measurements of extracts from the same NOM materials [24]. Another study combined HRMAS and DRIFT (Diffuse reflectance infrared Fourier transform spectroscopy) techniques to identify the relationship between the structure of soil humic substances and long-term (40 years) soil management practices, including organic and/or mineral fertilizations [25].…”

Section: Hrmas Applications In Agriculturementioning

confidence: 98%

“…A variety of natural organic matters (NOM) (wood, kerogen, bitumen, and whole sediments) were subjected to both Fourier transform ion cyclotron resonance mass spectrometry (FTICR-MS) and NMR techniques [24]. Interestingly, this work showed that HRMAS applied to the whole NOM samples was superior to the traditional liquid-state NMR measurements of extracts from the same NOM materials [24].…”

Section: Hrmas Applications In Agriculturementioning

confidence: 99%

HRMAS NMR spectroscopy applications in agriculture

Mazzei¹,

Piccolo²

2017

Chem. Biol. Technol. Agric.

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The relatively recent and advanced high-resolution magic angle spinning (HRMAS) NMR technique enables the direct application of NMR spectroscopy to semi-solid and gel-like samples. It combines the advantages of both solid-and liquid-state NMR by allowing to concomitantly measure intact and non-manipulated samples. Based on both 1D and 2D homo-and heteronuclear NMR spectra, HRMAS evaluates the composition of fresh semi-solid samples with a similar resolution as that of classical liquid-state NMR techniques. The enhanced spectral quality still obtained for semi-solid samples is mainly due to the MAS system, whose rapid spinning and sample orientation minimize the anisotropic processes that prevent the acquisition of meaningful NMR spectra for non-liquid materials. Moreover, HRMAS allows us to use edited pulse sequences which, especially in the case of biological tissues or agrofood products, may provide a simultaneous information on polar and non-polar components without the need of preliminary sample extraction. Additionally, this technique may differentiate molecular species according to their degree of mobility in hydrated matrices. The evident versatile potential of the HRMAS NMR makes this technique particularly useful for life science molecular studies. Despite the focus of HRMAS has been greatly devoted on clinical biomedicine, materials chemistry, and metabolomics, there are already enough studies that show useful applications on agricultural issues. This report reviews the latest representative studies that employ HRMAS NMR on systems related to agricultural chemistry, requiring the characterization and dynamics of soil components, plant tissues, agrofood products, and in vivo organisms.

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“…It is well known that shale is multiphase material, composed of organic matters [5][6][7][8][9][10] scattered in inorganic matrix encompass of clay, quartz and calcite [11]. Kerogen is always defined as insoluble macromolecular organic matter in sedimentary rock [12]. As kerogen is tightly connected with the generation of shale gas [13], extensive attention has been paid to its evolution.…”

Section: Introductionmentioning

confidence: 99%

Methane adsorption on the surface of a model of shale: A density functional theory study

Zhu

Jing

et al. 2016

Applied Surface Science

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Combining advanced NMR techniques with ultrahigh resolution mass spectrometry: A new strategy for molecular scale characterization of macromolecular components of soil and sedimentary organic matter

Cited by 37 publications

References 46 publications

Analysis of soil organic matter at the solid–water interface by nuclear magnetic resonance spectroscopy

Analysis of soil organic matter at the solid–water interface by nuclear magnetic resonance spectroscopy

HRMAS NMR spectroscopy applications in agriculture

Methane adsorption on the surface of a model of shale: A density functional theory study

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