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Development of a method for determination of pharmaceutical residues in surface sea water using bag-SPE and UPLC-QToF
Stockholm University, Faculty of Science, Department of Applied Environmental Science (ITM).ORCID iD: 0000-0002-2131-4418
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]

In the present study, a multi-residue method based on a bag –solid phase extraction (bag-SPE) technique was applied to determine the occurrence of ten pharmaceuticals in surface water close to the effluent of a sewage treatment plant (STP) and along a coastal gradient from a STP effluent.

The ten compounds selected were caffeine, atenolol, metoprolol, oxazepam, carbamazepine, ketoprofen, naproxen, ibuprofen, diclofenac and gemfibrozil, i.e. a mixture of pharmaceuticals of different therapeutic classes having logarithmic octanol/water partitioning coefficients (Log KOW) ranging from -0.13 to 4.39.

All analyses were performed using ultra performance liquid chromatography (UPLC) combined with quadrupole time-of-flight (QToF) mass spectrometry.

The detection limit (LOD) of the pharmaceuticals in water ranged from 1.0-13 ng/L. The method showed consistent linear concentration ranges from 25-800 ng/L with regression coefficients (R2) better than 0.9801. The recoveries of the selected analytes ranged from 10.6-64.5 % with relative standard deviations (RSD) of < 16.4 % and inter-day variations of less than 17.7 %.

Although the detection limits (LOD) of the analytes were low, only four of the selected ten pharmaceuticals (caffeine, metoprolol, oxazepam and carbamazepine) showed concentrations in surface water higher than the detection levels. The concentrations of the four pharmaceuticals in sea water range from 4-210 ng/L.

Keyword [en]
Bag-SPE, Solid phase extraction, Pharmaceuticals, Sea water, UPLC-QToF
National Category
Analytical Chemistry
Research subject
Applied Environmental Science
Identifiers
URN: urn:nbn:se:su:diva-35549OAI: oai:DiVA.org:su-35549DiVA: diva2:287476
Projects
This research was financially supported by European Union (European Commission, FP6 Contract No. 003956) “Novel Methods for Integrated Risk Assessment of Cumulative Stressors in the Environment” (NoMiracle) and by the Swedish research council Formas.
Available from: 2010-01-18 Created: 2010-01-18 Last updated: 2016-01-29Bibliographically approved
In thesis
1. Methodologies to assess the fate of polar organic compounds in aquatic environments
Open this publication in new window or tab >>Methodologies to assess the fate of polar organic compounds in aquatic environments
2010 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

Polar organic compounds (POCs) are chemicals with polar functional groups in their structure. The functional groups make the compounds hydrophilic and less prone to partition with biota. However, the knowledge of their fate is limited due to difficulties associated with their measurements. Although, the persistence of POCs in the environment is generally low, they are considered to be semi-persistent compounds due to their continuous introduction to the environment via wastewater. Studies have shown that complex mixtures of POCs of different classes may have synergistic toxic effects on biota at environmental concentration levels. Therefore, it is important to develop analytical methods in order to establish the occurrence and fate of POCs in aquatic environments.

In Study I, a positive correlation between the sorption of a novel poly(ethylene-co-vinyl acetate-co-carbon monoxide) (PEVAC) material and the theoretical logarithmic dissociation partition coefficient (Log D) for seven POCs was observed. The PEVAC material showed an enhanced sorption of the POCs compared to the silicone material. Study II, demonstrated that the PEVAC sampler assess the freely dissolved concentration of POCs in aquatic environments. The results showed that the PEVAC polymer is an attractive alternative to silicone for mimicing the biological uptake of POCs in aquatic environments. Additionally, Study II showed that total extraction is appropriate for determination of the freely dissolved concentration of uncharged POCs with Log KOW < 2.67 in natural water.

In study III, a novel bag-solid phase extraction (bag-SPE) technique was compared to a conventional SPE-technique. Despite that the extraction efficiencies for POCs in wastewater were lower using the bag-SPE method, the two methods showed similar detection limits due to the lower ion-suppression experienced with the bag-SPE.

In study IV the bag-SPE method was further developed with the aim of lowering the detection limits for POCs. Detection limits (LOD) below 13 ng/L showed that the bag-SPE method was suitable for determination of POCs in surface sea water.

 

Place, publisher, year, edition, pages
Stockholm: Department of Applied Environmental Science (ITM), Stockholm University, 2010. 25 p.
Keyword
Passive equilibrium sampler, Absorbent, Polar organic compounds, Liquid chromatography-mass spectrometry, Partitioning coefficient, Fulvic acid, Sediment, PEVAC, Bag-SPE, Solid phase extraction, Pharmaceuticals, Wastewater, Sea water, UPLC-QToF
National Category
Environmental Sciences Analytical Chemistry
Research subject
Applied Environmental Science
Identifiers
urn:nbn:se:su:diva-35552 (URN)978-91-7447-003-1 (ISBN)
Public defence
2010-02-12, Nordenskiöldsalen, Geovetenskapens hus, Svante Arrhenius väg 12, Stockholm, 10:00 (Swedish)
Opponent
Supervisors
Projects
This research was financially supported by European Union (European Commission, FP6 Contract No. 003956) “Novel Methods for Integrated Risk Assessment of Cumulative Stressors in the Environment” (NoMiracle) and by the Swedish research council Formas.
Available from: 2010-01-21 Created: 2010-01-18 Last updated: 2010-01-18Bibliographically approved

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