title: Multiresidue trace analysis of pharmaceuticals, their human metabolites and transformation products by fully automated on-line solid-phase extraction-liquid chromatography-tandem mass spectrometry.
abstract: A novel, fully automated analytical methodology based on dual column liquid chromatography coupled to tandem mass spectrometry (LC-LC-MS(2)) has been developed and validated for the analysis of 12 pharmaceuticals and 20 metabolites and transformation products in different types of water (influent and effluent wastewaters and surface water). Two LC columns were used - one for pre-concentration of the sample and the second for separation and analysis - so that water samples were injected directly in the chromatographic system. Besides the many advantages of the methodology, such as minimization of the sample volume required and its manipulation, both compounds ionized in positive and negative mode could be analyzed simultaneously without compromising the sensitivity. A comparative study of different mobile phases, gradients and LC pre-concentration columns was carried out to obtain the best analytical performance. Limits of detection (MLODs) achieved were in the low ngL(-1) range for all the compounds. The method was successfully applied to study the presence of the target analytes in different wastewater and surface water samples collected near the city of Girona (Catalonia, Spain). Data on the environmental presence and fate of pharmaceutical metabolites and TPs is still scarce, highlighting the relevance of the developed methodology.
authors.affiliation: LEQUIA, Institute of the Environment, University of Girona, Campus Montilivi, E-17071 Girona, Spain; ICRA, Catalan Institute for Water Research, Emili Grahit 101, E-17003 Girona, Spain.
authors.forename: María Jesús
authors.initials: MJ
authors.lastname: García-Galán
authors.affiliation: ICRA, Catalan Institute for Water Research, Emili Grahit 101, E-17003 Girona, Spain.
authors.forename: Mira
authors.initials: M
authors.lastname: Petrovic
authors.affiliation: ICRA, Catalan Institute for Water Research, Emili Grahit 101, E-17003 Girona, Spain.
authors.forename: Sara
authors.initials: S
authors.lastname: Rodríguez-Mozaz
authors.affiliation: ICRA, Catalan Institute for Water Research, Emili Grahit 101, E-17003 Girona, Spain.
authors.forename: Damià
authors.initials: D
authors.lastname: Barceló
mesh_terms: D002853:Chromatography, Liquid; D002947:Cities; D004784:Environmental Monitoring; D006801:Humans; D057230:Limit of Detection; D009862:Online Systems; D004364:Pharmaceutical Preparations / Q000032:analysis*; D045483:Rivers / Q000737:chemistry*; D052616:Solid Phase Extraction; D013030:Spain; D053719:Tandem Mass Spectrometry; D062065:Wastewater / Q000032:analysis*; D014874:Water Pollutants, Chemical / Q000032:analysis*
chemical_list: D004364:Pharmaceutical Preparations; D062065:Wastewater; D014874:Water Pollutants, Chemical
keywords: Environmental waters; LC-LC analysis; Metabolites; Transformation products