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Simultaneous determination of several natural steroids in blood plasma from perch (Perca fluviatilis) by GC-HRMS
Stockholm University, Faculty of Science, Department of Applied Environmental Science (ITM).
Stockholm University, Faculty of Science, Department of Applied Environmental Science (ITM).
Stockholm University, Faculty of Science, Department of Applied Environmental Science (ITM).
(English)Manuscript (preprint) (Other academic)
Abstract [en]

A gas chromatography–high resolution mass spectrometry (GC-HRMS) procedure for the simultaneous determination of 18 endogenous steroid hormones in blood plasma from teleost fish has been developed. Proteins were removed by precipitation in methanol and lipids were removed by a liquid-liquid extraction. The protein and lipid free extract was further purified by using two successive solid phase extraction (SPE) methods (C18 and NH2). The isolated steroid hormones were silylated with a mixture of N-methyl-N-(trimethylsilyl)trifluoroacetamide (MSTFA): iodotrimethylsilane (TMSI ):dithioerythritol (DTE) prior to determination with GC-HRMS working in selective ion recording mode. A volume of 200 mL blood plasma was sufficient for accurate determination of the steroid hormone levels, which enabled determination in individual fish. The detection limits ranged from 0.0003 to 0.2 ng/g blood plasma from perch (Perca fluviatilis), approximately 10 to 100 times lower then previously reported in this field. The recoveries for the entire procedure were in the range 58 to 150% with a variation, expressed as standard deviation (SD), below 10% with some exceptions. Despite the multi-step clean-up procedure, the intra-assay coefficient of variation, i.e. the within-day variation, for most steroid hormones was well below 14%. Finally, the procedure has been successfully applied to the determination of steroid hormones in blood plasma from female perch caught in two Swedish lakes.

Keyword [en]
endocrine disruption, testosterone, GC-HRMS, silylation
National Category
Environmental Sciences
Research subject
Applied Environmental Science
Identifiers
URN: urn:nbn:se:su:diva-29472OAI: oai:DiVA.org:su-29472DiVA: diva2:233450
Available from: 2009-09-01 Created: 2009-09-01 Last updated: 2010-01-14Bibliographically approved
In thesis
1. Development of GC-HRMS procedures for determination of naturally occuring polar compounds in various environmental applications 
Open this publication in new window or tab >>Development of GC-HRMS procedures for determination of naturally occuring polar compounds in various environmental applications 
2009 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

The overall objectives of this dissertation were to gain further understanding of the two following environmentally significant issues: (i) Determination of natural steroid hormones in blood plasma from perch (Perca fluviatilis) during a reproductive cycle and to evaluate the possibility of using the steroid composition as a biomarker for early signs of endocrine disruptive effects. (ii) Determination of dissolved free amino acids in size resolved airborne particles collected over the Arctic pack ice area (>80°N) in summer and to study their overall relationship with the ocean surface microlayer as a potential source.

 This was made possible by the development of two separate gas chromatographic–high resolution mass spectrometry methods. To enable separation with gas chromatography both steroids and amino acids had to be chemically modified to increase their volatility. The small sample volumes available and low concentrations of analytes required a multi-step clean-up procedure to enable determination.

 The results showed that the circulating levels of steroids in perch varied over the year and that the levels of some androgens were lower in female perch exposed to leachate from a refuse dump compare to unexposed perch, which may explain the decline in fertility observed for the former group. This also indicated that the steroid composition in the blood plasma may function as a sensitive biomarker.

 The levels of dissolved free amino acids were enriched in the submicrometer aerosol, peaking in sizes around 100nm aerodynamic diameter. These findings do support a previous assumption that the most likely source for these particles is the surface microlayer of the open water between the ice floes. The most likely exchange mechanism of biogenic matter between ocean and atmosphere is the bursting of bubbles at the surface of the leads. This mechanism would provide a very important and poorly understood link between cloud radiative properties and marine biochemistry in the summer high Arctic (>80°N) through the production of cloud condensation nuclei.

Place, publisher, year, edition, pages
Stockholm: Department of Applied Environmental Science (ITM), Stockholm University, 2009. 57 p.
Keyword
GC-HRMS, steroid hormones, amino acids, perch, size-resolved aerosol, Arctic
National Category
Natural Sciences
Research subject
Applied Environmental Science
Identifiers
urn:nbn:se:su:diva-29283 (URN)978-91-7155-907-4 (ISBN)
Public defence
2009-09-25, De Geer salen, Geovetenskapens hus, Svante Arrhenius väg 14, Stockholm, 10:00 (English)
Opponent
Supervisors
Note
At the time of the doctoral defense, the following papers were unpublished and had a status as follows: Paper 1: Accepted. Paper 4: In progress. Paper 5: In progress.Available from: 2009-09-03 Created: 2009-08-20 Last updated: 2009-09-01Bibliographically approved

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