Determination of 19 sulfonamides in environmental water samples by automated on-line solid-phase extraction-liquid chromatography–tandem mass spectrometry (SPE-LC–MS/MS)

The present study describes the development, validation and a practical application of a fully automated analytical method based on on-line solid-phase extraction-liquid chromatography–tandem mass spectrometry (SPE-LC–MS/MS) for the simultaneous determination of 19 sulfonamides, including one acetylated metabolite, in different water matrices. MS/MS detection was carried out in a quadrupole-linear ion trap (QqLIT) mass analyzer. Target compounds were identified in the selected reaction monitoring (SRM) mode, recording two transitions between precursor ions and the two most abundant product ions. The method developed was applied to evaluate the occurrence of the target antibiotics in different water samples: influent and effluent water from waste water treatment plants (WWTP), ground water and surface water. Under optimal conditions, the method detection limits achieved were in the range 0.05–7.84 ng/L for WWTP influent water, 0.01–6.90 ng/L for WWTP effluent water, 0.02–5.13 ng/L for ground water and 0.02–4.52 ng/L for surface water samples. The instrumental repeatability, expressed as RSD, was usually below 10% for the different water matrices. Results showed the wide presence of sulfonamides in the four types of water, including one acetylated metabolite, with maximum concentrations up to 855 ng/L corresponding to sulfapyridine in an influent waste water sample near a densely populated urban area.This work has been funded by the EU project NOMIRACLE (No. 003956-2) and by the Spanish Ministry of Science and Innovation through the project CTM2006-26225-E and reflects the author's view. The EU is not liable for any use that may be made of the information contained in it. M.S.D.C. acknowledges her Ramón y Cajal contract from the Spanish Ministry of Science and Innovation. Maria Jesús García acknowledges the European Social Fund and AGAUR (Generalitat de Catalunya, Spain) for their economical support through the FI pre-doctoral grant. We express our thanks to C. Postigo for her collaboration with the Prospekt 2™ extractor, to Spark Holland for the gift of SPE cartridges, and to M. Llorca for participating in the water sampling campaign.Peer reviewe

Determination of 19 sulfonamides in environmental water samples by automated on-line solid-phase extraction-liquid chromatography–tandem mass spectrometry (SPE-LC–MS/MS)

The present study describes the development, validation and a practical application of a fully automated analytical method based on on-line solid-phase extraction-liquid chromatography–tandem mass spectrometry (SPE-LC–MS/MS) for the simultaneous determination of 19 sulfonamides, including one acetylated metabolite, in different water matrices. MS/MS detection was carried out in a quadrupole-linear ion trap (QqLIT) mass analyzer. Target compounds were identified in the selected reaction monitoring (SRM) mode, recording two transitions between precursor ions and the two most abundant product ions. The method developed was applied to evaluate the occurrence of the target antibiotics in different water samples: influent and effluent water from waste water treatment plants (WWTP), ground water and surface water. Under optimal conditions, the method detection limits achieved were in the range 0.05–7.84 ng/L for WWTP influent water, 0.01–6.90 ng/L for WWTP effluent water, 0.02–5.13 ng/L for ground water and 0.02–4.52 ng/L for surface water samples. The instrumental repeatability, expressed as RSD, was usually below 10% for the different water matrices. Results showed the wide presence of sulfonamides in the four types of water, including one acetylated metabolite, with maximum concentrations up to 855 ng/L corresponding to sulfapyridine in an influent waste water sample near a densely populated urban area.This work has been funded by the EU project NOMIRACLE (No. 003956-2) and by the Spanish Ministry of Science and Innovation through the project CTM2006-26225-E and reflects the author's view. The EU is not liable for any use that may be made of the information contained in it. M.S.D.C. acknowledges her Ramón y Cajal contract from the Spanish Ministry of Science and Innovation. Maria Jesús García acknowledges the European Social Fund and AGAUR (Generalitat de Catalunya, Spain) for their economical support through the FI pre-doctoral grant. We express our thanks to C. Postigo for her collaboration with the Prospekt 2™ extractor, to Spark Holland for the gift of SPE cartridges, and to M. Llorca for participating in the water sampling campaign.Peer reviewe