title: An on-line solid phase extraction-liquid chromatography-tandem mass spectrometry method for the determination of perfluoroalkyl acids in drinking and surface waters.
abstract: An UHPLC-MS/MS multiresidue method based on an on-line solid phase extraction (SPE) procedure was developed for the simultaneous determination of 9 perfluorinated carboxylates (from 4 to 12 carbon atoms) and 3 perfluorinated sulphonates (from 4 to 8 carbon atoms). This work proposes using an on-line solid phase extraction before chromatographic separation and analysis to replace traditional methods of off-line SPE before direct injection to LC-MS/MS. Manual sample preparation was reduced to sample centrifugation and acidification, thus eliminating several procedural errors and significantly reducing time-consuming and costs. Ionization suppression between target perfluorinated analytes and their coeluting SIL-IS were detected for homologues with a number of carbon atoms less than 9, but the quantitation was not affected. Total matrix effect corrected by SIL-IS, inclusive of extraction efficacy, and of ionization efficiency, ranged between -34 and +39%. The percentage of recoveries, between 76 and 134%, calculated in different matrices (tap water and rivers impacted by different pollutions) was generally satisfactory. LODs and LOQs of this on-line SPE method, which also incorporate recovery losses, ranged from 0.2 to 5.0 ng/L and from 1 to 20 ng/L, respectively. Validated on-line SPE-LC/MS/MS method has been applied in a wide survey for the determination of perfluoroalkyl acids in Italian surface and ground waters.
authors.affiliation: IRSA-CNR, Water Research Institute, Via Mulino 19, 20861 Brugherio, Italy.
authors.forename: Michela
authors.initials: M
authors.lastname: Mazzoni
authors.affiliation: IRSA-CNR, Water Research Institute, Via Mulino 19, 20861 Brugherio, Italy.
authors.forename: Marianna
authors.initials: M
authors.lastname: Rusconi
authors.affiliation: IRSA-CNR, Water Research Institute, Via Mulino 19, 20861 Brugherio, Italy.
authors.forename: Sara
authors.initials: S
authors.lastname: Valsecchi
authors.affiliation: Thermo Fisher Scientific, 16 avenue du Québec, Silic 765, Villebon-sur-Yvette, 91963 Courtaboeuf Cedex, France.
authors.forename: Claudia P B
authors.initials: CP
authors.lastname: Martins
authors.affiliation: IRSA-CNR, Water Research Institute, Via Mulino 19, 20861 Brugherio, Italy.
authors.forename: Stefano
authors.initials: S
authors.lastname: Polesello
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