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Analysis of hydroxamate siderophores in soil solution using liquid chromatography with mass spectrometry and tandem mass spectrometry with on-line sample preconcentration
Mid Sweden University, Faculty of Science, Technology and Media, Department of Natural Sciences. (Analytisk kemi - Skog och Miljö)ORCID iD: 0000-0002-0893-7071
Mid Sweden University, Faculty of Science, Technology and Media, Department of Natural Sciences. (Analytisk kemi - Skog och Miljö)ORCID iD: 0000-0002-3646-294X
2015 (English)In: Journal of Separation Science, ISSN 1615-9306, E-ISSN 1615-9314, Vol. 38, no 19, p. 3305-3312Article in journal (Refereed) Published
Abstract [en]

A liquid chromatography-electrospray ionization-mass spectrometry method was developed to quantitatively and qualitatively analyze thirteen hydroxamate siderophores (ferrichrome, ferrirubin, ferrirhodin, ferrichrysin, ferricrocin, ferrioxamine B, D1, E and G, neocoprogen I and II, coprogen and triacetylfusarinine C). Samples were pre-concentrated on-line via switch-valve setup prior to analyte separation on a Kinetex C18 column. Gradient elution was performed using a mixture of an ammonium formate buffer and acetonitrile. Total analysis time including column conditioning was 20.5 minutes. Analyte were fragmented by applying collision induced dissociation, enabling structural identification via tandem mass spectrometry. Limit of detection values for the selected ion monitoring method ranged from 71 pM to 1.5 nM with corresponding values of two to nine times higher for the multiple reaction monitoring method. The liquid chromatography-mass spectrometry method resulted in a robust and sensitive quantification of hydroxamate siderophores as indicated by retention time stability, linearity, sensitivity, precision and recovery. The analytical error of the methods, assessed trough random-order, duplicate analysis of soil samples extracted with a mixture of 10 mM phosphate buffer and methanol, appears negligible in relation to between-sample variations. 

Place, publisher, year, edition, pages
Weinheim: Wiley-VCH Verlagsgesellschaft, 2015. Vol. 38, no 19, p. 3305-3312
Keywords [en]
Collision induces dissociation, column-switching, coprogens/fusigens, ferrichromes, ferrioxamines
National Category
Analytical Chemistry
Identifiers
URN: urn:nbn:se:miun:diva-25990DOI: 10.1002/jssc.201500509ISI: 000362553600001Scopus ID: 2-s2.0-84942828265OAI: oai:DiVA.org:miun-25990DiVA, id: diva2:857146
Projects
FOREAvailable from: 2015-09-28 Created: 2015-09-28 Last updated: 2017-12-01Bibliographically approved
In thesis
1. On the investigation of chemical parameters reflecting microbial activity linked to nutrient availability in forest soil
Open this publication in new window or tab >>On the investigation of chemical parameters reflecting microbial activity linked to nutrient availability in forest soil
2015 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

As agrarian society developed, the most fertile soils able to sustain the nutritional requirements needed for high crop yield were assigned to farming, while the more penurious soils were left to uphold the forest ecosystems. Some temperate forests are developed on acidic soils considered to be nutrient poor, as much of the inorganic nutrients are entrapped in poorly weatherable soil minerals and not easily accessed by plant roots. In an undisturbed ecosystem, the largest contribution of available nutrients comes from the recycling of organically bound nutrients via the decomposition of dead plant material. If biomass is removed, for instance with a more intensified exploitation of the forest ecosystems including whole tree harvesting, this source of nutrients is consequently decreased. The importance of soil mineral weathering as a source of nutrients, and especially that promoted by soil biota, is thereby emphasized.

This thesis addresses biotic parameters associated with mineral weathering. Different aspects of soil solution sampling strategies and analysis of different organic ligands as well as biomarkers for the estimation of fungal biomass were investigated. These chemical parameters were also evaluated as indicators of microbial activity in relation to mineral nutrient availability in soil.

With the assumption that the current nutrient status of a soil will affect the microbial interest of certain minerals as sources of inorganic nutrients, a mineral amendment trial was performed in a Swedish boreal forest soil. Overall, the amended soil presented good nutrient status, but with a possible shortage of iron. Due to this, it was hypothesized that the amended mineral with the highest iron content i.e. biotite would cause an elevation of microbial activity in its vicinity when compared to the bulk soil.

The level of microbial activity in the vicinity of the amended minerals was evaluated via quantification of organic acids and siderophores, as well as estimation of fungal biomass and enzymatic activity.

The highest microbial activity was measured for the O horizon of the investigated podzol, although nothing indicated an elevated association with the amended minerals. In the E horizon, however, elevation in microbial activity was observed in the vicinity of the biotite mineral when compared with bulk soil, although only a few of the investigated parameters differed significantly when evaluated separately.  

To enable this study, a highly sensitive analytical method employing liquid chromatography and mass spectrometry was developed to quantify a number of hydroxamate siderophores. On-line pre-concentration enabled detection of these organic ligands in the pico-molar range – a necessity when analyzing natural samples.

Furthermore, an analytical method was developed for the estimation of fungal biomass via quantification of chitin-derived glucosamine, which also employed liquid chromatography and tandem mass spectrometry. Unlike currently available methods, the one presented in this thesis did not involve analyte derivatization, which resulted in high sample throughput while simultaneously avoiding complications involved with the additional derivatization procedure.

The distribution of a group of organic ligands known as aromatic low molecular mass organic acids was also studied in a boreal forest podzol soil. Different sampling and samples preparation techniques, namely tension-lysimeters, soil centrifugation and liquid-soil extraction, were compared when analyzing soil solution components. Significant differences in analyte amount and species type were found between these sampling techniques. Some of the differences could be accounted for by variation in soil composition at different depths of the investigated podzol, but others could be attributed to structural differences within the studied analyte group. This clearly illustrated the intricacy of sampling and analysis when working with a sample matrix as complex and diverse as soil.

As previously, liquid chromatography and mass spectrometry was used to quantify the analytes of interest. A highly sensitive analytical method was developed that was able to detect eleven aromatic low molecular mass organic acids in the nano-molar range. High selectivity was ensured by applying multiple reaction monitoring enabled by collision induced fragmentation of the analytes.

 

Place, publisher, year, edition, pages
Sundsvall: Mid Sweden University, 2015. p. 62
Series
Mid Sweden University doctoral thesis, ISSN 1652-893X ; 230
Keywords
Boreal forest, electrospray ionization, fungal biomass, hydrophilic interaction chromatography, hydroxamate siderophores, liquid chromatography-mass spectrometry, mineral amendment, aromatic acids, podzol soil
National Category
Analytical Chemistry Other Chemistry Topics
Identifiers
urn:nbn:se:miun:diva-25994 (URN)978-91-88025-40-1 (ISBN)
Public defence
2015-10-23, O102, Holmgatan 10, Sundsvall, 10:15 (English)
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Available from: 2015-09-28 Created: 2015-09-28 Last updated: 2015-09-28Bibliographically approved

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Olofsson, MadelenBylund, Dan

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