Skip to content

Development of Alditol Acetate Derivatives for the Determination of 15 N-Enriched Amino Sugars by Gas Chromatography-Combustion-Isotope Ratio Mass Spectrometry

Research output: Contribution to journalArticle

Original languageEnglish
Pages (from-to)3397-3404
Number of pages8
JournalAnalytical Chemistry
Volume91
Issue number5
Early online date11 Feb 2019
DOIs
DateAccepted/In press - 11 Feb 2019
DateE-pub ahead of print - 11 Feb 2019
DatePublished (current) - 5 Mar 2019

Abstract

Amino sugars can be used as indices to evaluate the role of soil microorganisms in active nitrogen (N) cycling in soil. This paper details the assessment of the suitability of gas chromatography-combustion-isotope ratio mass spectrometry (GC-C-IRMS) for the analysis of 15 N-enriched amino sugars as alditol acetate derivatives prior to application of a novel 15 N stable isotope probing (SIP) approach to amino sugars. The efficient derivatization and cleanup of alditol acetate derivatives for GC was achieved using commercially available amino sugars, including glucosamine, mannosamine, galactosamine, and muramic acid, as laboratory standards. A VF-23ms stationary phase was found to produce optimal separations of all four compounds. The structure of the alditol acetate derivatives was confirmed using gas chromatography/mass spectrometry (GC/MS). For GC-C-IRMS determinations, implementation of a two-point normalization confirmed the optimal carrier gas flow rate to be 1.7 mL min -1 . Linearity of δ 15 N value determinations up to δ 15 N t of 469 ± 3.1‰ (where δ 15 N t is the independently measured δ 15 N value) was confirmed when 30 nmol N was injected on-column, with the direction of deviation from δ 15 N t at low sample amount dependent on the 15 N abundance of the analyte. Observed between- and within-run memory effects were significant (P < 0.007) when a highly enriched standard (469 ± 3.1‰) was run; therefore, analytical run order and variation in 15 N enrichment of analytes within the same sample must be considered. The investigated parameters have confirmed the isotopic robustness of alditol acetate derivatives of amino sugars for the GC-C-IRMS analysis of 15 N-enriched amino sugars in terms of linearity over an enrichment range (natural abundance to 469 ± 3.1‰) with on-column analyte amount over 30 nmol N.

Download statistics

No data available

Documents

Documents

  • Full-text PDF (accepted author manuscript)

    Rights statement: This is the author accepted manuscript (AAM). The final published version (version of record) is available online via ACS at https://pubs.acs.org/doi/10.1021/acs.analchem.8b04838. Please refer to any applicable terms of use of the publisher.

    Accepted author manuscript, 705 KB, PDF document

DOI

View research connections

Related faculties, schools or groups