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Sediment extraction and clean-up for organic phosphorus analysis by electrospray ionization tandem mass spectrometry
Uppsala University, Disciplinary Domain of Science and Technology, Chemistry, Department of Physical and Analytical Chemistry, Analytical Chemistry.
Uppsala University, Disciplinary Domain of Science and Technology, Chemistry, Department of Physical and Analytical Chemistry, Analytical Chemistry.
Uppsala University, Disciplinary Domain of Science and Technology, Chemistry, Department of Physical and Analytical Chemistry, Analytical Chemistry.
Uppsala University, Disciplinary Domain of Science and Technology, Chemistry, Department of Physical and Analytical Chemistry, Analytical Chemistry.
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2008 (English)In: Talanta: The International Journal of Pure and Applied Analytical Chemistry, ISSN 0039-9140, E-ISSN 1873-3573, Vol. 74, no 5, 1175-1183 p.Article in journal (Refereed) Published
Abstract [en]

A method to prepare NaOH sediment extracts for organic P compound analysis with electrospray ionization tandem mass spectrometry (ESI-MS-MS) was developed on natural samples. Ion exchange, rotary evaporation and mass cut-off filtering proved to be suitable for sample preparation. Samples were analyzed with ESI-MS-MS, and reproducibility and repeatability of the method was calculated. In addition, 31P-nuclear magnetic resonance spectroscopy (31P NMR) was used to measure recovery of different P compound groups such as orthophosphate (Ortho-P), orthophosphate monoesters (Monoester-P), orthophosphate diesters (Diester-P) and pyrophosphates (Pyro-P).

The developed sample preparation method resulted in an easy-to-spray liquid for the ESI-MS-MS instrumentation. The overall P recovery was 65% and 31P NMR showed that Diester-P, possibly in the form of DNA, was apparently lost through the filtering step most likely due to their size. Variances in the total intensities of the MS scans (relative standard deviation (R.S.D.) 35–54%) were for about 50% due to repeated MS runs. Covariances of the peaks in the MS spectra were calculated to be for about 30% due to the sample preparation procedure. Finally, with the ESI-MS-MS approach, 11 peaks in the mass spectra were found likely to represent phosphate containing compounds.

Place, publisher, year, edition, pages
2008. Vol. 74, no 5, 1175-1183 p.
Keyword [en]
Organic phosphorus, Sediment, Sample preparation, ESI-MS-MS, 31P NMR
National Category
Analytical Chemistry
Identifiers
URN: urn:nbn:se:uu:diva-97625DOI: 10.1016/j.talanta.2007.08.030ISI: 000253514700013OAI: oai:DiVA.org:uu-97625DiVA: diva2:172643
Available from: 2008-10-15 Created: 2008-10-15 Last updated: 2017-12-14Bibliographically approved
In thesis
1. Organic Phosphorus Compounds in Aquatic Sediments: Towards Molecular Identification with Mass Spectrometry
Open this publication in new window or tab >>Organic Phosphorus Compounds in Aquatic Sediments: Towards Molecular Identification with Mass Spectrometry
2008 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

Phosphorus (P) regulates trophic status in most aquatic systems. However, only bioavailable P contributes to primary production. In most lakes and shallow seas, mineralisation of sediment P into its bioavailable form and its release to the water column is important for maintaining primary production. Sediment organic P forms a substantial proportion of this P to be mineralised and can originate from different sources on land (farmland, forests, etc.) or from primary production in the lake. These organic P forms can thus be expected to have differing composition, degradability and recyclable P content.

Knowledge of the chemical structure of sediment organic P compounds is scarce, mainly due to lack of appropriate analytical techniques. The commonly used 31P-nuclear magnetic resonance (31P-NMR) technique, only identifies P binding groups, so a mass spectrometric (MS) analysis method was developed that allows individual sediment organic P compounds to be identified.

EDTA as pre-extractant resulted in the highest P yield in subsequent NaOH extraction. Extracted organic P compound groups were identified using 31P-NMR. For identification of specific P compounds with MS, a sample preparation method prior to electrospray tandem mass spectrometry (ESI-MS/MS) analysis was developed. Liquid chromatography (LC) with porous graphitic carbon prior to ESI-MS/MS enhanced sensitivity and selectivity, enabling several of the ions detected to be identified as nucleotides. 31P-NMR analysis showed P monoesters to be the most stabile P compounds throughout a lake sediment profile. The developed LC-ESI-MS/MS analysis method revealed that some monoester-P (nucleotides) were labile, while other P compounds increased in concentration with Baltic Sea sediment depth and were therefore considered stabile. Differences in patterns of P compounds detected were also shown depending on catchment characteristics in relation to Baltic Sea sediment age.

For cost-effective management of eutrophication, knowledge of the sources of degradable organic P forms, contributing to internal loading, is needed. This thesis showed the developed LC-ESI-MS/MS analysis method to be a powerful analytical tool for this purpose.

Place, publisher, year, edition, pages
Uppsala: Universitetsbiblioteket, 2008. 58 p.
Series
Digital Comprehensive Summaries of Uppsala Dissertations from the Faculty of Science and Technology, ISSN 1651-6214 ; 560
Keyword
electrospray ionisation, mass spectrometry, liquid chromatography, organic phosphorus, aquatic sediment, eutrophication, sample preparation, extraction
National Category
Analytical Chemistry
Identifiers
urn:nbn:se:uu:diva-9319 (URN)978-91-554-7306-8 (ISBN)
Public defence
2008-11-07, B42, BMC, Husargatan 3, Uppsala, Sweden, 10:15
Opponent
Supervisors
Available from: 2008-10-15 Created: 2008-10-15 Last updated: 2010-08-16Bibliographically approved

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Sjöberg, Per J. R.

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