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On the investigation of chemical parameters reflecting microbial activity linked to nutrient availability in forest soil
Mid Sweden University, Faculty of Science, Technology and Media, Department of Natural Sciences. (Analytisk kemi - Skog och Miljö)ORCID iD: 0000-0002-0893-7071
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. , 62 p.
Series
Mid Sweden University doctoral thesis, ISSN 1652-893X ; 230
Keyword [en]
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: urn:nbn:se:miun:diva-25994ISBN: 978-91-88025-40-1 (print)OAI: oai:DiVA.org:miun-25994DiVA: diva2:857185
Public defence
2015-10-23, O102, Holmgatan 10, Sundsvall, 10:15 (English)
Opponent
Supervisors
Projects
FORE
Available from: 2015-09-28 Created: 2015-09-28 Last updated: 2015-09-28Bibliographically approved
List of papers
1. Evaluation of sampling and sample preparation procedures for the determination of aromatic acids and their distribution in a podzol soil using liquid chromatography-tandem mass spectrometry
Open this publication in new window or tab >>Evaluation of sampling and sample preparation procedures for the determination of aromatic acids and their distribution in a podzol soil using liquid chromatography-tandem mass spectrometry
2014 (English)In: Geoderma, ISSN 0016-7061, E-ISSN 1872-6259, Vol. 232-234, 373-380 p.Article in journal (Refereed) Published
Abstract [en]

In this work the distribution of free and weekly adsorbed aromatic acids (phthalic acid and ten phenolicacids; gallic, p-hydroxybenzoic, salicylic, vanillic, protocatechuic, p-coumaric, syringic, sinapic, ferulic and caffeicacid), which could participate in weathering and soil formation processes, were studied for O, E and Bhorizons in a podzol soil in central Sweden. For the analysis a simple and rapid quantitative and qualitative liquidchromatography–tandem mass spectrometry method (using gradient elution) was developed with LODs rangingfrom 5 to 25 nM. Different soil solution sampling techniques (tension-lysimeter and soil centrifugation) and soilextraction with either 10 mM phosphate buffer (pH 7.2) or 50:50 (v/v) 10 mM phosphate buffer:MeOHwere compared. All eleven acids were found in detectable or trace concentrations. The most abundant aromaticacids were vanillic and phthalic acid with concentrations around 1 μM for O and E horizon respectively.Lysimeter samples resulted in the lowest concentrations followed by centrifugation samples. Ingeneral, buffer:MeOH extraction resulted in the highest concentrations for the O horizon, likely due toMeOH's ability to compete for hydrophobic sites on soil organic matter (SOM). Then again, pure bufferwith its higher ion strength, interfering with the acids electrostatic interactions with clay particles, leads tohigher extracted concentrations for the E and B horizons. Since the efficiency of the extraction solutions, to alarge extent, depends on the sample properties, a general approach is hard to appoint. However, the extractionof substituted cinnamic acids is in general facilitated by adding MeOH to the extraction solution. The use of statisticalmethods for the evaluation of the results showed a large and significant difference in aromatic acid concentrationsreceived using different sampling techniques and sample preparations. In fact, sampling methodsresulted in higher variations in aromatic acid concentrations than sampled horizon.

Place, publisher, year, edition, pages
Amsterdam: Elsevier, 2014
Keyword
phenolic acids, phthalic acid, soil extraction, soil centrifugation, tension-lysimeter
National Category
Analytical Chemistry
Identifiers
urn:nbn:se:miun:diva-23171 (URN)10.1016/j.geoderma.2014.06.005 (DOI)000340315700036 ()2-s2.0-84902330801 (Scopus ID)
Projects
FORE
Available from: 2014-10-08 Created: 2014-10-08 Last updated: 2015-09-28Bibliographically approved
2. Effects of mineral amendment on soil chemistry parameters reflecting microbial activity in a Swedish boreal forest soil
Open this publication in new window or tab >>Effects of mineral amendment on soil chemistry parameters reflecting microbial activity in a Swedish boreal forest soil
(English)Manuscript (preprint) (Other academic)
Abstract [en]

Samples of apatite, biotite and oligoclase were incubated in different soil horizons of a boreal forest podzol in central Sweden. After four years, soil from the bulk and the surfaces of the minerals were extracted and analyzed in regard to fungal biomass, enzymatic activity, low molecular mass organic acids and hydroxamate siderophores.  The nutrient status of the study area was evaluated using historical data from foliar and soil solution analysis. Soil solution indicated a possible shortage of P in the mineral soil even though foliar content was above target levels. The foliar analysis instead revealed possible shortage of Fe. Apatite is the primary source of inorganic P in soil and biotite is rich in Fe compared to the soil at the site, and it was hypothesized that both minerals could be attractive sources of weatherable mineral nutrients, hence associated with higher microbial activity. Parameters measured as indicators of microbial activity revealed few significant (p<0.05) differences between the minerals and bulk soil in the O horizon, probably due to large variations among replicates, although an overall higher microbial activity was found in the bulk soil. In the E horizon a distinct trend appeared indicating higher levels of low molecular mass organic acids, enzymatic activity and fungal biomass associated with the biotite mineral, although this observation was only found to be significant for some of the parameters when analyzed individually. No clear trends were observed in the B horizon.

Keyword
Low molecular mass organic acids, hydroxamate siderophores, enzymatic activity, fungal biomass, podzol soil
National Category
Other Chemistry Topics
Identifiers
urn:nbn:se:miun:diva-25993 (URN)
Projects
FORE
Available from: 2015-09-28 Created: 2015-09-28 Last updated: 2015-09-28Bibliographically approved
3. Liquid Chromatography with Electrospray Ionization and Tandem Mass Spectrometry Applied in the Quantitative Analysis of Chitin-Derived Glucosamine for a Rapid Estimation of Fungal Biomass in Soil
Open this publication in new window or tab >>Liquid Chromatography with Electrospray Ionization and Tandem Mass Spectrometry Applied in the Quantitative Analysis of Chitin-Derived Glucosamine for a Rapid Estimation of Fungal Biomass in Soil
2016 (English)In: International Journal of Analytical Chemistry, ISSN 1687-8760, E-ISSN 1687-8779, 9269357Article in journal (Refereed) Published
Abstract [en]

This method employs liquid chromatography-tandem mass spectrometry to rapidly quantify chitin-derived glucosamine for estimating fungal biomass. Analyte retention was achieved using hydrophilic interaction liquid chromatography, with a zwitter-ionic stationary phase (ZIC-HILIC), and isocratic elution using 60 % 5 mM ammonium formate buffer (pH 3.0) and 40 % ACN. Inclusion of muramic acid, and its chromatographic separation from glucosamine, enabled calculation of the bacterial contribution to the latter. Galactosamine, an isobaric isomer to glucosamine, found in significant amounts in soil samples, was also investigated. The two isomers form the same precursor and product ions, and could not be chromatographically separated using this rapid method. Instead, glucosamine and galactosamine were distinguished mathematically, using the linear relationships describing the differences in product ion intensities for the two analytes. The m/z transitions of 180→72 and 180→84 were applied for the detection of glucosamine and galactosamine and that of 252→126 for muramic acid. Limits of detection were in the pico-molar range for all included analytes. The total analysis time was 6 min, providing a high sample through-put method.

Place, publisher, year, edition, pages
Hindawi Publishing Corporation, 2016
Keyword
Amino sugars, galactosamine, hydrophilic interaction liquid chromatography, muramic acid
National Category
Analytical Chemistry
Identifiers
urn:nbn:se:miun:diva-25992 (URN)10.1155/2016/9269357 (DOI)000370708500001 ()2-s2.0-84959156661 (Scopus ID)
Projects
FORE
Available from: 2015-09-28 Created: 2015-09-28 Last updated: 2016-12-15Bibliographically approved
4. Analysis of hydroxamate siderophores in soil solution using liquid chromatography with mass spectrometry and tandem mass spectrometry with on-line sample preconcentration
Open this publication in new window or tab >>Analysis of hydroxamate siderophores in soil solution using liquid chromatography with mass spectrometry and tandem mass spectrometry with on-line sample preconcentration
2015 (English)In: Journal of Separation Science, ISSN 1615-9306, E-ISSN 1615-9314, Vol. 38, no 19, 3305-3312 p.Article 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
Keyword
Collision induces dissociation, column-switching, coprogens/fusigens, ferrichromes, ferrioxamines
National Category
Analytical Chemistry
Identifiers
urn:nbn:se:miun:diva-25990 (URN)10.1002/jssc.201500509 (DOI)000362553600001 ()2-s2.0-84942828265 (Scopus ID)
Projects
FORE
Available from: 2015-09-28 Created: 2015-09-28 Last updated: 2016-01-13Bibliographically approved

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