Scheda di dettaglio – i prodotti della ricerca
| Dato | Valore |
|---|---|
| Title | Liquid chromatography mass spectrometry determination of perfluoroalkyl acids in environmental solid extracts after phospholipid removal and on-line turbulent flow chromatography purification |
| Abstract | An on-line TFC (Turbulent Flow Chromatography) clean up procedures coupled with UHPLC-MS/MS(Ultra High Performance Liquid Chromatography Mass Spectrometry) multi-residue method was devel-oped for the simultaneous determination of 8 perfluroalkyl carboxylic acids (PFCA, from 5 to 12 carbonatoms) and 3 perfluoroalkyl sulfonic acids (PFSA, from 4 to 8 carbon atoms) in environmental solid matri-ces. Fast sample preparation procedure was based on a sonication-assisted extraction with acetonitrile.Phospholipids in biological samples were fully removed by an off-line SPE purification before injection,using HybridSPE®Phospholipid Ultra cartridges.The development of the on-line TFC clean-up procedure regarded the choice of the stationary phase,the optimization of the mobile phase composition, flow rate and injected volume.The validation of the optimized method included the evaluation of matrix effects, accuracy and repro-ducibility. Signal suppression in the analysis of fortified extracts ranged from 1 to 60%, and this problemwas overcome by using isotopic dilution. Since no certified reference materials were available for PFAS inthese matrices, accuracy was evaluated by recoveries on spiked clam samples which were 98-133% forPFCAs and 40-60% for PFSAs. MLDs and MLQs ranged from 0.03 to 0.3 ng g-1wet weight and from 0.1 to0.9 ng g-1wet weight respectively. Repeatability (intra-day precision) and reproducibility (inter-day pre-cision) showed RSD from 3 to 13% and from 4 to 27% respectively. Validated on-line TFC/UHPLC-MS/MSmethod has been applied for the determination of perfluoroalkyl acids in different solid matrices (sedi-ment, fish, bivalves and bird yolk). |
| Source | Journal of chromatography A (Online) 1453, pp. 62–70 |
| Keywords | PFASTFCLC-MS |
| Journal | Journal of chromatography A (Online) |
| Editor | Elsevier Science, , |
| Year | 2016 |
| Type | Articolo in rivista |
| DOI | 10.1016/j.chroma.2016.05.047 |
| Authors | M. Mazzoni, S. Polesello, M. Rusconi, S. Valsecchi |
| Text | 359762 2016 10.1016/j.chroma.2016.05.047 ISI Web of Science WOS WOS 000378182800007 Scopus 2 s2.0 84969811634 PFAS TFC LC MS Liquid chromatography mass spectrometry determination of perfluoroalkyl acids in environmental solid extracts after phospholipid removal and on line turbulent flow chromatography purification M. Mazzoni, S. Polesello, M. Rusconi, S. Valsecchi IRSA CNR, Water Research Institute, Via del Mulino 19, 20861 Brugherio, Italy An on line TFC Turbulent Flow Chromatography clean up procedures coupled with UHPLC MS/MS Ultra High Performance Liquid Chromatography Mass Spectrometry multi residue method was devel oped for the simultaneous determination of 8 perfluroalkyl carboxylic acids PFCA, from 5 to 12 carbonatoms and 3 perfluoroalkyl sulfonic acids PFSA, from 4 to 8 carbon atoms in environmental solid matri ces. Fast sample preparation procedure was based on a sonication assisted extraction with acetonitrile.Phospholipids in biological samples were fully removed by an off line SPE purification before injection,using HybridSPE®Phospholipid Ultra cartridges.The development of the on line TFC clean up procedure regarded the choice of the stationary phase,the optimization of the mobile phase composition, flow rate and injected volume.The validation of the optimized method included the evaluation of matrix effects, accuracy and repro ducibility. Signal suppression in the analysis of fortified extracts ranged from 1 to 60%, and this problemwas overcome by using isotopic dilution. Since no certified reference materials were available for PFAS inthese matrices, accuracy was evaluated by recoveries on spiked clam samples which were 98 133% forPFCAs and 40 60% for PFSAs. MLDs and MLQs ranged from 0.03 to 0.3 ng g 1wet weight and from 0.1 to0.9 ng g 1wet weight respectively. Repeatability intra day precision and reproducibility inter day pre cision showed RSD from 3 to 13% and from 4 to 27% respectively. Validated on line TFC/UHPLC MS/MSmethod has been applied for the determination of perfluoroalkyl acids in different solid matrices sedi ment, fish, bivalves and bird yolk . 1453 Published version 12/05/2016 paper_TFC 2016_Mazzoni_TFC.pdf Articolo in rivista Elsevier Science 1873 3778 Journal of chromatography A Online Journal of chromatography A Online Journal of chromatography A mariannarusconi RUSCONI MARIANNA MAZZONI MICHELA stefano.polesello POLESELLO STEFANO saramaria.valsecchi VALSECCHI SARA MARIA |