Multi-residue analytical method for the determination of emerging pollutants in water by solid-phase extraction and liquid chromatography-tandem mass spectrometry |
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Authors: | Rodil Rosario Quintana José Benito López-Mahía Purificación Muniategui-Lorenzo Soledad Prada-Rodríguez Darío |
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Affiliation: | 1. Department of Analytical Chemistry, Faculty of Sciences, University of A Coruña, Campus A Zapateira S.N., 15071 A Coruña, Spain;2. Department of Analytical Chemistry, Nutrition and Food Sciences, IIAA-Institute for Food Analysis and Research, University of Santiago de Compostela, 15782 Santiago de Compostela, Spain;3. IUMA-University Institute of Environment, University of A Coruña, Pazo da Lóngora, Liáns, 15179 Oleiros (A Coruña), Spain |
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Abstract: | This paper describes the development and validation of a method for the simultaneous determination of 53 multi-class emerging organic pollutants in water samples using solid-phase extraction (SPE) followed by liquid chromatography-tandem mass spectrometry (LC-MS/MS), using electrospray ionisation (ESI) in both positive and negative modes. Target compounds include acidic herbicides, UV filters, insect repellents, organophosphorous flame retardants, a bactericide, pharmaceuticals and metabolites. A single SPE consisting on the loading of 200-500 mL of sample adjusted to pH 7 on Oasis HLB 200mg cartridges and elution with methanol, permitted obtaining good recoveries: higher than 60% for tap, surface and wastewater in most cases. The 7 isotopically labelled internal standards effectively compensated losses during sample preparation and matrix effects at LC-MS/MS determination. The precision of the method, calculated as relative standard deviation (RSD) was below 15% for all compounds and all tested matrices. Detection limits (LODs) based on the confirmation, less intense, MRM (multiple reaction monitoring) transition and considering blanks varied between 0.3 and 30 ngL(-1). Finally, the developed method was applied to the determination of target analytes in various samples, including tap, surface and waste water. Among the tested emerging pollutants, 31 were found in wastewater in concentrations reaching up to 10 microgL(-1) in the case of ibuprofen. Also, 13 species were detected in tap water with concentrations up to 0.13 microgL(-1) for tri(chloropropyl) phosphate (TCPP). |
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Keywords: | Emerging pollutants Pharmaceuticals Organophosphorous flame retardant/plasticizers UV filters Sunscreen agents Acidic herbicides Liquid chromatography–tandem mass spectrometry (LC–MS/MS) Electrospray ionisation (ESI) Solid-phase extraction (SPE) Water samples |
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