Development of a Multiresidue Method for the Determination of 24 Pharmaceuticals in Clams by QuEChERS and Liquid Chromatography-Triple Quadrupole Tandem Mass Spectrometry
Data on different therapeutic classes of pharmaceutical compounds (PhCs) in clams or other bivalves living in natural conditions are scarce. The aim of this work was the optimization and validation of a method for the determination of PhCs in clams for further evaluation of any potential human exposure risk due to their consumption. A quick, easy, cheap, effective, rugged, and safe (QuEChERS) approach is proposed for sample clean-up and concentration of 24 PhCs in clams, with subsequent analysis by liquid chromatography-tandem mass spectrometry. This method showed a good linear range for all PhCs with determination coefficients (r2) between 0.9949 and 0.9993 and coefficients of variation (CVm) lower than 5.5%. This method allowed the quantification of target compounds at trace concentration levels (ng g−1), being the most abundant PhC in clam caffeine. This PhC was detected in more than 70% of samples with concentrations ranging from 0.10 to 12 ng g−1 wet weight.
KeywordsPharmaceuticals Clams HPLC-MS/MS QuEChERS
The authors would like to thank the financial support from the project co-funded by the European Commission, LIFE Environment Programme, “LIFE Impetus - Improving current barriers for controlling pharmaceutical compounds in urban wastewater treatment plants” (LIFE14 ENV/PT/000739).
Compliance with Ethical Standards
Conflict of Interest
João Rodrigues declares that he has no conflict of interest. Stephanie Albino declares that she has no conflict of interest. Sofia Silva declares that she has no conflict of interest. Alexandra Cravo declares that she has no conflict of interest. Vitor Cardoso declares that he has no conflict of interest. Maria João Benoliel declares that she has no conflict of interest. Cristina Almeida declares that she has no conflict of interest.
This article does not contain any studies with human or animal subjects.
- Alvarez-Munoz D, Rodriguez-Mozaz S, Maulvault A, Tediosi A, Fernandez-Tejedor M, Van den Heuvel F, Kotterman M, Marques A, Barcelo D (2015b) Occurrence of pharmaceuticals and endocrine disrupting compounds in macroalgaes, bivalves, and fish from coastal areas in Europe. Environ Res 143:56–64CrossRefGoogle Scholar
- AOAC (2007) Official method 2007.01 pesticide residues in foods by acetonitrile extraction and partitioning with magnesium sulfate gas chromatography/mass spectrometry and liquid chromatography/tandem mass spectrometry first action 2007Google Scholar
- Directive (2000) Directive 2000/60/EC of the European Parliament and of the Council of 23 October 2000 establishing a framework for Community action in the field of water policy. Off J Eur Union L 327Google Scholar
- Directive (2008) Directive 2008/105/EC of the European Parliament and of the Council of 16 December 2008 on environmental quality standards in the field of water policy. Off J Eur Union L 384/84Google Scholar
- Directive (2013) Directive 2013/39/EU of the European Parliament and of the Council of 12 August 2013 regarding prioritary substances in the field of water policy. Off J Eur Union L 226/1Google Scholar
- ESM (2008) European Standard Method EN 15662:2008. Foods of plant origin – determination of pesticide residues using GC-MS and/or LC-MS/MS following acetonitrile extraction/partitioning and cleanup by dispersive SPE–QuEChERS-methodGoogle Scholar
- Fusco G, Aprea G, Galiero G, Guarino A, Viscardi M (2013) Escherichia coli, Salmonella spp., hepatitis a virus and norovirus in bivalve molluscs in Southern Italy. Vet Ital 49(1):55–58Google Scholar
- Gaffney V, Cardoso V, Cardoso E, Teixeira A, Martins J, Benoliel M, Almeida C (2017) Occurrence and behaviour of pharmaceutical compounds in a Portuguese wastewater treatment plant: removal efficiency through conventional treatment processes. Environ Sci Pollut Res 24(17):14717–14734CrossRefGoogle Scholar
- Gaw S, Thomas KV, Hutchinson TH (2014) Sources, impacts and trends of pharmaceuticals in the marine and coastal environment. Phil Trans R Soc B 369:20130572Google Scholar
- INE (2016) Statistical yearbook of Portugal 2016. Instituto Nacional de Estatística, IP, PortugalGoogle Scholar
- Infarmed (2011). Monitorization of the market. Available at: 〈http://www.infarmed.pt/portal/page/portal/infarmed/monitorizacao_do_mercado/observatorio/estatistica_do_medicamento/estmed-2011.pdf〉. Accessed on 05.10.12
- Infarmed (2013) Infarmed (Autoridade Nacional do Medicamento e Produtos de Saúde, I.P.), Medicines Statistic. In. Ministério da Saúde, Infarmed, LisboaGoogle Scholar
- Ramirez AJ, Brain RA, Usenko S, Mottaleb MA, O'Donnell JG, Stahl LL, Wathen JB, Snyder BD, Pitt JL, Perez-Hurtado P, Dobbins LL, Brooks BW, Chambliss CK (2009) Occurrence of pharmaceuticals and personal care products in fish: results of a national pilot study in the United States. Environ Toxicol Chem 28(12):2587–2597CrossRefGoogle Scholar
- Vandermeersch G, Lourenco H, Alvarez-Munoz D, Cunha S, Diogene J, Cano-Sancho G, Sloth J, Kwadijk C, Barcelo D, Allegaert W, Bekaert K, Fernandes J, Marques A, Robbens (2015) Environmental contaminants of emerging concern in seafood - European database on contaminant levels. Environ Res 143:29–45CrossRefGoogle Scholar