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Quantitative analysis of 8 pharmaceuticals and 1 pesticide in surface water and waste water with liquid chromatography coupled to tandem mass spectrometry: method development and field study

(2010)
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Abstract
A major part of this thesis is about the development of an SPE-LC-MS/MS method for the determination of pharmaceuticals in surface water and waste water. It is proven that careful optimisation of an LC-MS method is mandatory for these matrices, due to the complex nature of the samples leading to possible matrix effects. Special attention should be paid to extraction, sample clean-up, chromatography and the choice of internal standards. In addition, problems rise when pharmaceuticals with different structures should be analysed, without the availability of labelled internal standards. Structural analogues as internal standards should be carefully picked: pharmaceuticals or pesticides from the same class can be present in the environment. In our case, matrix effects could not be fully resolved with the SPE-HPLC-MS/MS method, and were also different for different samples. Standard addition was the only way to ensure accurate quantification. Thanks to UPLC-analysis, matrix effects could be minimised and could be compensated for with structural analogues. Quantification could be performed with internal standards (structural analogues). This results in a less time-consuming and labour-intensive method. The studies in the waste water treatment plants of Aquafin and in surface water samples of VMM, analysed with the HPLC-MS/MS method, gave us insight in pollution for a number of pharmaceuticals in Belgium. By our knowledge, this is one of the first reports on occurrence of pharmaceuticals in surface water and waste water in Flanders. From the study in the public waste water treatment plants, it could be concluded that several pharmaceuticals could not be removed, and introduction into the environment by discharge is proven. Generally, it can be concluded that pollution of the selected pharmaceuticals in the aquatic environment is very low – only minor concentrations up to 26.4 ng/l were found. Propiconazole was found in higher concentrations up to 85.9 ng/l. However, pollution of pharmaceuticals was higher in the vicinity of a chemo-pharmaceutical company and industrial companies (up to 961.3 ng/l). Concentrations were all lower than PNEC-concentrations, so no environmental concern have to be raised from these data. Further sampling and investigation is necessary to know if these concentrations are ‘typical’ concentrations.
Keywords
determination, analytical chemistry, LC-MS, pesticide, pharmaceuticals, waste water, environment, surface water

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Citation

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MLA
Van De Steene, Jet. “Quantitative Analysis of 8 Pharmaceuticals and 1 Pesticide in Surface Water and Waste Water with Liquid Chromatography Coupled to Tandem Mass Spectrometry: Method Development and Field Study.” 2010 : n. pag. Print.
APA
Van De Steene, Jet. (2010). Quantitative analysis of 8 pharmaceuticals and 1 pesticide in surface water and waste water with liquid chromatography coupled to tandem mass spectrometry: method development and field study. Ghent University. Faculty of Pharmaceutical Sciences, Ghent, Belgium.
Chicago author-date
Van De Steene, Jet. 2010. “Quantitative Analysis of 8 Pharmaceuticals and 1 Pesticide in Surface Water and Waste Water with Liquid Chromatography Coupled to Tandem Mass Spectrometry: Method Development and Field Study”. Ghent, Belgium: Ghent University. Faculty of Pharmaceutical Sciences.
Chicago author-date (all authors)
Van De Steene, Jet. 2010. “Quantitative Analysis of 8 Pharmaceuticals and 1 Pesticide in Surface Water and Waste Water with Liquid Chromatography Coupled to Tandem Mass Spectrometry: Method Development and Field Study”. Ghent, Belgium: Ghent University. Faculty of Pharmaceutical Sciences.
Vancouver
1.
Van De Steene J. Quantitative analysis of 8 pharmaceuticals and 1 pesticide in surface water and waste water with liquid chromatography coupled to tandem mass spectrometry: method development and field study. [Ghent, Belgium]: Ghent University. Faculty of Pharmaceutical Sciences; 2010.
IEEE
[1]
J. Van De Steene, “Quantitative analysis of 8 pharmaceuticals and 1 pesticide in surface water and waste water with liquid chromatography coupled to tandem mass spectrometry: method development and field study,” Ghent University. Faculty of Pharmaceutical Sciences, Ghent, Belgium, 2010.
@phdthesis{921378,
  abstract     = {A major part of this thesis is about the development of an SPE-LC-MS/MS method for the determination of pharmaceuticals in surface water and waste water. It is proven that careful optimisation of an LC-MS method is mandatory for these matrices, due to the complex nature of the samples leading to possible matrix effects. Special attention should be paid to extraction, sample clean-up, chromatography and the choice of internal standards. In addition, problems rise when pharmaceuticals with different structures should be analysed, without the availability of labelled internal standards. Structural analogues as internal standards should be carefully picked: pharmaceuticals or pesticides from the same class can be present in the environment. In our case, matrix effects could not be fully resolved with the SPE-HPLC-MS/MS method, and were also different for different samples. Standard addition was the only way to ensure accurate quantification. Thanks to UPLC-analysis, matrix effects could be minimised and could be compensated for with structural analogues. Quantification could be performed with internal standards (structural analogues). This results in a less time-consuming and labour-intensive method. 
The studies in the waste water treatment plants of Aquafin and in surface water samples of VMM, analysed with the HPLC-MS/MS method, gave us insight in pollution for a number of pharmaceuticals in Belgium. By our knowledge, this is one of the first reports on occurrence of pharmaceuticals in surface water and waste water  in Flanders. From the study in the public waste water treatment plants, it could be concluded that several pharmaceuticals could not be removed, and introduction into the environment by discharge is proven. Generally, it can be concluded that pollution of the selected pharmaceuticals in the aquatic environment is very low – only minor concentrations up to 26.4 ng/l were found. Propiconazole was found in higher concentrations up to 85.9 ng/l. However, pollution of pharmaceuticals was higher in the vicinity of a chemo-pharmaceutical company and industrial companies (up to 961.3 ng/l). Concentrations were all lower than PNEC-concentrations, so no environmental concern have to be raised from these data. Further sampling and investigation is necessary to know if these concentrations are ‘typical’ concentrations.},
  author       = {Van De Steene, Jet},
  keywords     = {determination,analytical chemistry,LC-MS,pesticide,pharmaceuticals,waste water,environment,surface water},
  language     = {eng},
  pages        = {173},
  publisher    = {Ghent University. Faculty of Pharmaceutical Sciences},
  school       = {Ghent University},
  title        = {Quantitative analysis of 8 pharmaceuticals and 1 pesticide in surface water and waste water with liquid chromatography coupled to tandem mass spectrometry: method development and field study},
  url          = {http://lib.ugent.be/fulltxt/RUG01/001/385/901/RUG01-001385901_2010_0001_AC.pdf},
  year         = {2010},
}