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Title: Chemical characterization of a chelator-treated soil humate by solution-state multinuclear two-dimensional NMR and FTIR and pyrolysis-GCMS

Abstract

A California forest soil used for contaminant bioavailability studies was extracted for humic substances (HS) and then treated with 4,5-dihydroxy-1,3-benzene disulfonate (Tiron) to remove exchangeable metal ions. This yielded HS that was readily water-soluble at neutral pH without residual Tiron contamination, and the gel electrophoretic pattern was very similar to an international reference HS. The improved solubility facilitated analysis of HS by solution-state 1-D and 2-D {sup 1}H, {sup 13}C, {sup 31}P, and {sup 13}C-{sup 1}H NMR. The amino acids Gly, Ala, Leu, lle, Val, Asp, Ser, Thr, Glu, and Pro were identified in intact HS as peptidic from scalar coupling in TOCSY and dipolar interactions in NOESY and then confirmed by acid digestion of HS with 2-D {sup 1}H NMR and GCMS analysis. The presence of peptides was also corroborated by FT-IR and pyrolysis-GCMS results. Carbohydrates containing {alpha}- and {beta}-pyranoses, methoxy-phenylpropanyl structures, phosphate mono/diesters, polyphosphates, plus phosphatidic acid esters were also evident. Furthermore, the {sup 1}H NOESY, TOCSY, and HSQC together indicated that the peptidic side chains were mobile, whereas aromatic groups were relatively rigid. Thus the peptidic moieties may be more readily accessible to aqueous contaminants than aromatic groups.

Authors:
; ;
Publication Date:
Research Org.:
Univ. of California, Davis (US)
Sponsoring Org.:
Environmental Protection Agency; USDOE
OSTI Identifier:
20080503
DOE Contract Number:  
FG07-96ER20255; FG03-97ER62349
Resource Type:
Journal Article
Journal Name:
Environmental Science and Technology
Additional Journal Information:
Journal Volume: 34; Journal Issue: 9; Other Information: PBD: 1 May 2000; Journal ID: ISSN 0013-936X
Country of Publication:
United States
Language:
English
Subject:
54 ENVIRONMENTAL SCIENCES; SOILS; HUMUS; NUCLEAR MAGNETIC RESONANCE; FOURIER TRANSFORMATION; INFRARED SPECTRA; GAS CHROMATOGRAPHY; MASS SPECTROSCOPY; CHELATING AGENTS

Citation Formats

Fan, T.W.M., Higashi, R.M., and Lane, A.N. Chemical characterization of a chelator-treated soil humate by solution-state multinuclear two-dimensional NMR and FTIR and pyrolysis-GCMS. United States: N. p., 2000. Web. doi:10.1021/es991127v.
Fan, T.W.M., Higashi, R.M., & Lane, A.N. Chemical characterization of a chelator-treated soil humate by solution-state multinuclear two-dimensional NMR and FTIR and pyrolysis-GCMS. United States. doi:10.1021/es991127v.
Fan, T.W.M., Higashi, R.M., and Lane, A.N. Mon . "Chemical characterization of a chelator-treated soil humate by solution-state multinuclear two-dimensional NMR and FTIR and pyrolysis-GCMS". United States. doi:10.1021/es991127v.
@article{osti_20080503,
title = {Chemical characterization of a chelator-treated soil humate by solution-state multinuclear two-dimensional NMR and FTIR and pyrolysis-GCMS},
author = {Fan, T.W.M. and Higashi, R.M. and Lane, A.N.},
abstractNote = {A California forest soil used for contaminant bioavailability studies was extracted for humic substances (HS) and then treated with 4,5-dihydroxy-1,3-benzene disulfonate (Tiron) to remove exchangeable metal ions. This yielded HS that was readily water-soluble at neutral pH without residual Tiron contamination, and the gel electrophoretic pattern was very similar to an international reference HS. The improved solubility facilitated analysis of HS by solution-state 1-D and 2-D {sup 1}H, {sup 13}C, {sup 31}P, and {sup 13}C-{sup 1}H NMR. The amino acids Gly, Ala, Leu, lle, Val, Asp, Ser, Thr, Glu, and Pro were identified in intact HS as peptidic from scalar coupling in TOCSY and dipolar interactions in NOESY and then confirmed by acid digestion of HS with 2-D {sup 1}H NMR and GCMS analysis. The presence of peptides was also corroborated by FT-IR and pyrolysis-GCMS results. Carbohydrates containing {alpha}- and {beta}-pyranoses, methoxy-phenylpropanyl structures, phosphate mono/diesters, polyphosphates, plus phosphatidic acid esters were also evident. Furthermore, the {sup 1}H NOESY, TOCSY, and HSQC together indicated that the peptidic side chains were mobile, whereas aromatic groups were relatively rigid. Thus the peptidic moieties may be more readily accessible to aqueous contaminants than aromatic groups.},
doi = {10.1021/es991127v},
journal = {Environmental Science and Technology},
issn = {0013-936X},
number = 9,
volume = 34,
place = {United States},
year = {2000},
month = {5}
}