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Wille K.,Ghent University | Kiebooms J.A.L.,Ghent University | Claessens M.,Ghent University | Rappe K.,Ghent University | And 8 more authors.
Analytical and Bioanalytical Chemistry | Year: 2011

Organic micropollutants such as pharmaceuticals, perfluorinated compounds (PFCs), and pesticides, are important environmental contaminants. To obtain more information regarding their presence in marine organisms, an increasing demand exists for reliable analytical methods for quantification of these micropollutants in biotic matrices. Therefore, we developed extraction procedures and new analytical methods for the quantification of 14 pesticides, 10 PFCs, and 11 pharmaceuticals in tissue of marine organisms, namely blue mussels (Mytilus edulis). This paper presents these optimized analytical procedures and their application to M. edulis, deployed at five stations in the Belgian coastal zone. The methods consisted of a pressurized liquid extraction and solid-phase extraction (SPE) followed by ultra high-performance liquid chromatography coupled to triple quadrupole mass spectrometry for pharmaceuticals and pesticides, and of a liquid extraction using acetonitrile and SPE, followed by liquid chromatography coupled to time-of-flight mass spectrometry for PFCs. The limits of quantification of the three newly optimized analytical procedures in M. edulis tissue varied between 0.1 and 10 ng g -1, and satisfactory linearities (≥0.98) and recoveries (90-106%) were obtained. Application of these methods to M. edulis revealed the presence of five pharmaceuticals, two PFCs, and seven pesticides at levels up to 490, 5, and 60 ng g-1, respectively. The most prevalent micropollutants were salicylic acid, paracetamol, perfluorooctane sulfonate, chloridazon, and dichlorvos. © 2011 Springer-Verlag. Source

Wille K.,Ghent University | Noppe H.,Ghent University | Verheyden K.,Ghent University | Vanden Bussche J.,Ghent University | And 5 more authors.
Analytical and Bioanalytical Chemistry | Year: 2010

Knowledge of the presence of micropollutants such as pharmaceuticals, in coastal areas, is very limited; therefore, the main objective of this study was to optimize and validate a new analytical method for the quantitative analysis of 13 multiclass pharmaceuticals in seawater. Target compounds included antibiotics, non-steroidal anti-inflammatory drugs, β-blockers, lipid regulators and one psychiatric drug. A combination of solid-phase extraction and liquid chromatography coupled with multiple mass spectrometry enabled their detection at the low nanogram per litre level. The limits of quantification varied between 1 and 50 ng L-1, for most components the linearities were more than 0.99 and the recoveries obtained in seawater (95-108%) were satisfactory. This method was applied to seawater and estuarine water samples collected in the Belgian coastal zone, to assess the prevalence of common pharmaceuticals in this marine environment. Seven pharmaceuticals, including compounds of which the presence in marine environments had not been reported earlier, were detected, with salicylic acid and carbamazepine being the most abundant, in concentrations up to 855 ng L-1. © 2010 Springer-Verlag. Source

Wille K.,Ghent University | Vanden Bussche J.,Ghent University | Noppe H.,Ghent University | De Wulf E.,Flemish Environment Agency FEA | And 4 more authors.
Journal of Chromatography A | Year: 2010

Perfluorinated compounds (PFCs), which are extensively used in a wide variety of applications because of their specific surfactant properties, have recently appeared as an important new class of global environmental pollutants. Quantitative analysis of PFCs in aqueous matrices remains, however, a challenging task. During this study, a new analytical method for the determination of 14 PFCs in surface-, sewage- and seawater was developed and validated. The target analytes were extracted using solid-phase extraction followed by liquid chromatography coupled to a time-of-flight mass spectrometer (LC-ToF-MS). The use of very narrow mass tolerance windows (<10ppm) resulted in a highly selective MS-technique for the detection of PFCs in complex aqueous matrices. Validation of this analytical method in surface-, sewage- and seawater resulted in limits of quantification (LOQs) varying from 2 to 200ngL-1, satisfying recoveries (92-134%), and good linearity (R2=0.99 for most analytes). Analysis of samples of the North Sea, the Scheldt estuary, and three harbours of the Belgian coastal region led to the detection of four different PFCs. Perfluorooctane sulfonate (PFOS) was found to be the most abundant PFC in levels up to 38.9ngL-1. © 2010 Elsevier B.V. Source

Wille K.,Ghent University | De Brabander H.F.,Ghent University | Vanhaecke L.,Ghent University | De Wulf E.,Flemish Environment Agency FEA | And 2 more authors.
TrAC - Trends in Analytical Chemistry | Year: 2012

We present a comprehensive overview of recent developments in analytical chemistry for the most environmentally important groups of chemicals of emerging concern (CECs), including pharmaceuticals and personal-care products, pesticides, steroid hormones, perfluorinated compounds, alkylphenolethoxylates, bisphenol A and phthalates. Due to both the typically very low concentrations at which CECs occur and environmental samples being complex matrices demanding extensive extraction and clean-up procedures, very specific, sensitive analytical procedures are needed.In this context, we discuss state-of-the-art instrumentation for sample preconcentration, analyte separation and detection. We could observe several prominent trends: the common use of liquid chromatography (LC) to allow separation of CECs (instead of gas chromatography); the development and the application of multi-class methods; and, the increasing popularity of high-resolution, full-scan analysis, combined with a trend towards the use of sub-2-μm-particle sizes and high flow rates (ultra-high-performance LC).Overall, due to the recent advances in instrumentation, we could see significant progress in the analytical chemistry of CECs in environmental matrices. © 2012 Elsevier Ltd. Source

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