title: A sensitive multi-residue method for the determination of 35 micropollutants including pharmaceuticals, iodinated contrast media and pesticides in water.
abstract: A sensitive, multi-residue method using solid-phase extraction followed by liquid chromatography-tandem mass spectrometry (LC-MS/MS) was developed to determine a representative group of 35 analytes, including corrosion inhibitors, pesticides and pharmaceuticals such as analgesic and anti-inflammatory drugs, five iodinated contrast media, β-blockers and some of their metabolites and transformation products in water samples. Few other methods are capable of determining such a broad range of contrast media together with other analytes. We studied the parameters affecting the extraction of the target analytes, including sorbent selection and extraction conditions, their chromatographic separation (mobile phase composition and column) and detection conditions using two ionisation sources: electrospray ionisation (ESI) and atmospheric pressure chemical ionisation (APCI). In order to correct matrix effects, a total of 20 surrogate/internal standards were used. ESI was found to have better sensitivity than APCI. Recoveries ranging from 79 to 134 % for tap water and 66 to 144 % for surface water were obtained. Intra-day precision, calculated as relative standard deviation, was below 34 % for tap water and below 21 % for surface water, groundwater and effluent wastewater. Method quantification limits (MQL) were in the low ng L(-1) range, except for the contrast agents iomeprol, amidotrizoic acid and iohexol (22, 25.5 and 17.9 ng L(-1), respectively). Finally, the method was applied to the analysis of 56 real water samples as part of the validation procedure. All of the compounds were detected in at least some of the water samples analysed. Graphical Abstract Multi-residue method for the determination of micropollutants including pharmaceuticals, iodinated contrast media and pesticides in waters by LC-MS/MS.
authors.affiliation: Department of Chemistry, University of Girona, Campus Montilivi, 17071, Girona, Spain.
authors.forename: Carme
authors.initials: C
authors.lastname: Valls-Cantenys
authors.affiliation: DVGW-Technologiezentrum Wasser (The German Water Centre), Karlsruher Str. 84, 76139, Karlsruhe, Germany.
authors.forename: Marco
authors.initials: M
authors.lastname: Scheurer
authors.affiliation: Department of Chemistry, University of Girona, Campus Montilivi, 17071, Girona, Spain.
authors.forename: Mònica
authors.initials: M
authors.lastname: Iglesias
authors.affiliation: DVGW-Technologiezentrum Wasser (The German Water Centre), Karlsruher Str. 84, 76139, Karlsruhe, Germany.
authors.forename: Frank
authors.initials: F
authors.lastname: Sacher
authors.affiliation: DVGW-Technologiezentrum Wasser (The German Water Centre), Karlsruher Str. 84, 76139, Karlsruhe, Germany.
authors.forename: Heinz-Jürgen
authors.initials: HJ
authors.lastname: Brauch
authors.affiliation: Department of Chemistry, University of Girona, Campus Montilivi, 17071, Girona, Spain. victoria.salvado@udg.edu.
authors.forename: Victoria
authors.initials: V
authors.lastname: Salvadó
mesh_terms: D002853:Chromatography, Liquid / Q000379:methods*; D003287:Contrast Media / Q000032:analysis*; D060587:Groundwater / Q000032:analysis; D054879:Halogenation; D057230:Limit of Detection; D010575:Pesticides / Q000032:analysis*; D004364:Pharmaceutical Preparations / Q000032:analysis*; D052616:Solid Phase Extraction / Q000379:methods; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods; D053719:Tandem Mass Spectrometry / Q000379:methods*; D062065:Wastewater / Q000032:analysis; D014867:Water / Q000032:analysis; D014874:Water Pollutants, Chemical / Q000032:analysis*
chemical_list: D003287:Contrast Media; D010575:Pesticides; D004364:Pharmaceutical Preparations; D062065:Wastewater; D014867:Water; D014874:Water Pollutants, Chemical
keywords: Iodinated X-ray contrast media; Liquid-chromatography-electrospray ionisation-tandem mass spectrometry; Multi-residue method; Pesticides; Pharmaceuticals; Water samples