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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
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)
Mid Sweden University, Faculty of Science, Technology and Media, Department of Natural Sciences. (Analytisk kemi - Skog och Miljö)ORCID iD: 0000-0002-3646-294X
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. Vol. 232-234, 373-380 p.
Keyword [en]
phenolic acids, phthalic acid, soil extraction, soil centrifugation, tension-lysimeter
National Category
Analytical Chemistry
Identifiers
URN: urn:nbn:se:miun:diva-23171DOI: 10.1016/j.geoderma.2014.06.005ISI: 000340315700036Scopus ID: 2-s2.0-84902330801OAI: oai:DiVA.org:miun-23171DiVA: diva2:753673
Projects
FORE
Available from: 2014-10-08 Created: 2014-10-08 Last updated: 2015-09-28Bibliographically 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. 62 p.
Series
Mid Sweden University doctoral thesis, ISSN 1652-893X ; 230
Keyword
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)
Opponent
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Projects
FORE
Available from: 2015-09-28 Created: 2015-09-28 Last updated: 2015-09-28Bibliographically approved

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