Multi-residue analysis of pharmaceuticals in wastewater by liquid chromatography-magnetic sector mass spectrometry: method quality assessment and application in a Belgian case study.

Through systematic research a novel analytical method using solid-phase extraction (SPE) and liquid chromatography magnetic sector mass spectrometry was developed for the measurement of 43 pharmaceuticals in wastewater. A thorough method validation quantified the contribution of both the extraction recovery and matrix effects in the overall method process efficiency, and a detailed uncertainty analysis was performed to elaborate a quality labelling strategy to be used in data interpretation. Compounds for which a precise (relative standard deviation<20%) process efficiency between 60% and 140% was determined, were labelled as 'quantitative' whereas the results for other compounds should be interpreted as 'indicative'. Method application on influent and effluent samples of (i) a conventional active sludge system and (ii) a parallel membrane bioreactor/conventional active sludge wastewater treatment plant in Belgium revealed the occurrence of 22 pharmaceuticals. The anti-inflammatory drug diclofenac and the antidepressant venlafaxine were measured in the effluents at concentrations ranging from 0.5 to 1.8 μg L(-1) and 0.2 to 0.5 μg L(-1), respectively, which indicated to be of high potential environmental risk for the receiving river Dender, Belgium.

[1]  Jianying Hu,et al.  Occurrence and fate of quinolone and fluoroquinolone antibiotics in a municipal sewage treatment plant. , 2012, Water research.

[2]  P. Fong,et al.  Antidepressants (venlafaxine and citalopram) cause foot detachment from the substrate in freshwater snails at environmentally relevant concentrations , 2012 .

[3]  D Fatta-Kassinos,et al.  Urban wastewater treatment plants as hotspots for the release of antibiotics in the environment: a review. , 2013, Water research.

[4]  J. Dewulf,et al.  Selective accurate-mass-based analysis of 11 oxy-PAHs on atmospheric particulate matter by pressurized liquid extraction followed by high-performance liquid chromatography and magnetic sector mass spectrometry , 2012, Analytical and Bioanalytical Chemistry.

[5]  J. Dewulf,et al.  From multi-residue screening to target analysis of pharmaceuticals in water: development of a new approach based on magnetic sector mass spectrometry and application in the Nairobi River basin, Kenya. , 2012, The Science of the total environment.

[6]  M. Birkved,et al.  Environmental risk assessment of human pharmaceuticals in Denmark after normal therapeutic use. , 2000, Chemosphere.

[7]  F. Hernández,et al.  Risk assessment for drugs of abuse in the Dutch watercycle. , 2013, Water research.

[8]  Arun Kumar,et al.  Pharmaceuticals, personal care products and endocrine-disrupting chemicals in U.S. surface and finished drinking waters: a proposed ranking system. , 2010, The Science of the total environment.

[9]  Félix Hernández,et al.  Rapid non-target screening of organic pollutants in water by ultraperformance liquid chromatography coupled to time-of-light mass spectrometry , 2008 .

[10]  N. Nakada,et al.  Occurrence and fate of oseltamivir carboxylate (Tamiflu) and amantadine in sewage treatment plants. , 2010, Chemosphere.

[11]  Herman Van Langenhove,et al.  Accurate mass determination, quantification and determination of detection limits in liquid chromatography-high-resolution time-of-flight mass spectrometry: challenges and practical solutions. , 2013, Analytica chimica acta.

[12]  E. C. Vasconcelos,et al.  Environmental risk assessment of antibiotics: an intensive care unit analysis. , 2009, Chemosphere.

[13]  M. Ibáñez,et al.  Qualitative validation of a liquid chromatography-quadrupole-time of flight mass spectrometry screening method for organic pollutants in waters. , 2013, Journal of chromatography. A.

[14]  J. Lester,et al.  Fate of drugs during wastewater treatment , 2013 .

[15]  A. Pollio,et al.  Environmental risk assessment of six human pharmaceuticals: Are the current environmental risk assessment procedures sufficient for the protection of the aquatic environment? , 2004, Environmental toxicology and chemistry.

[16]  D. Dietrich,et al.  Water-borne diclofenac affects kidney and gill integrity and selected immune parameters in brown trout (Salmo trutta f. fario). , 2005, Aquatic toxicology.

[17]  B. Matuszewski,et al.  Strategies for the assessment of matrix effect in quantitative bioanalytical methods based on HPLC-MS/MS. , 2003, Analytical chemistry.

[18]  J. D. Jong,et al.  Accurate mass screening of pharmaceuticals and fungicides in water by U-HPLC–Exactive Orbitrap MS , 2012, Analytical and Bioanalytical Chemistry.

[19]  E. Cooper,et al.  Preliminary risk assessment database and risk ranking of pharmaceuticals in the environment. , 2008, The Science of the total environment.

[20]  K Kümmerer,et al.  Promoting resistance by the emission of antibiotics from hospitals and households into effluent. , 2003, Clinical microbiology and infection : the official publication of the European Society of Clinical Microbiology and Infectious Diseases.

[21]  A. Zafra-Gómez,et al.  Removal of quinolone antibiotics from wastewaters by sorption and biological degradation in laboratory-scale membrane bioreactors. , 2013, The Science of the total environment.

[22]  D. Barceló,et al.  Environmental risk assessment of pharmaceutical residues in wastewater effluents, surface waters and sediments. , 2006, Talanta.

[23]  P. Verlicchi,et al.  Occurrence of pharmaceutical compounds in urban wastewater: removal, mass load and environmental risk after a secondary treatment--a review. , 2012, The Science of the total environment.

[24]  F. Hernández,et al.  Current use of high-resolution mass spectrometry in the environmental sciences , 2012, Analytical and Bioanalytical Chemistry.

[25]  Colin R. Janssen,et al.  Heterogeneous photocatalysis of moxifloxacin in water: chemical transformation and ecotoxicity. , 2015, Chemosphere.

[26]  Hans Sanderson,et al.  Ranking and prioritization of environmental risks of pharmaceuticals in surface waters. , 2004, Regulatory toxicology and pharmacology : RTP.

[27]  Ralf Schulz,et al.  Antiviral drugs in wastewater and surface waters: a new pharmaceutical class of environmental relevance? , 2010, Environmental science & technology.

[28]  D. A. Barry,et al.  Methodology to account for uncertainties and tradeoffs in pharmaceutical environmental hazard assessment. , 2012, Journal of environmental management.

[29]  S. Lacorte,et al.  Liquid chromatography coupled to tandem mass spectrometry and high resolution mass spectrometry as analytical tools to characterize multi-class cytostatic compounds. , 2013, Journal of chromatography. A.

[30]  K. Thomas,et al.  Environmental assessment of Norwegian priority pharmaceuticals based on the EMEA guideline. , 2008, Ecotoxicology and environmental safety.