| Content Provider |
World Health Organization (WHO)-Global Index Medicus |
| Author |
Rossini, D. Ciofi, L. Ancillotti, C. Checchini, L. Bruzzoniti, M. C. Rivoira, L. Fibbi, D. Orlandini, S. Del Bubba, M. |
| Description |
Country affiliation: Italy Author Affiliation: Rossini D ( Department of Chemistry 'Ugo Schiff', University of Florence, Via della Lastruccia 3, 50019 Sesto Fiorentino, Florence, Italy); Ciofi L ( Department of Chemistry 'Ugo Schiff', University of Florence, Via della Lastruccia 3, 50019 Sesto Fiorentino, Florence, Italy.); Ancillotti C ( Department of Chemistry 'Ugo Schiff', University of Florence, Via della Lastruccia 3, 50019 Sesto Fiorentino, Florence, Italy.); Checchini L ( Department of Chemistry 'Ugo Schiff', University of Florence, Via della Lastruccia 3, 50019 Sesto Fiorentino, Florence, Italy.); Bruzzoniti MC ( Department of Chemistry, University of Turin, Via Pietro Giuria 5, 10125 Turin, Italy.); Rivoira L ( Department of Chemistry, University of Turin, Via Pietro Giuria 5, 10125 Turin, Italy.); Fibbi D ( GIDA S.p.A., Via di Baciacavallo 36, 59100 Prato, Italy.); Orlandini S ( Department of Chemistry 'Ugo Schiff', University of Florence, Via della Lastruccia 3, 50019 Sesto Fiorentino, Florence, Italy.); Del Bubba M ( Department of Chemistry 'Ugo Schiff', University of Florence, Via della Lastruccia 3, 50019 Sesto Fiorentino, Florence, Italy. Electronic address: delbubba@unifi.it.) |
| Abstract |
For the first time QuEChERS extraction of sewage sludge was combined with the automatic solid-phase pre-concentration and purification of the extract (following indicated as SPE) and LC-MS/MS analysis, for the determination of the non-steroidal anti-inflammatory drugs acetylsalicylic acid (ASA), diclofenac (DIC), fenbufen (FEN), flurbiprofen (FLU), ketoprofen (KET), ibuprofen (IBU) and naproxen (NAP), and their metabolites salicylic acid (SAL), 4'-hydroxydiclofenac (4'-HYDIC), 1-hydroxyibuprofen (1-HYIBU), 2-hydroxyibuprofen (2-HYIBU), 3-hydroxyibuprofen (3-HYIBU) and o-desmethylnaproxen (O-DMNAP). Various commercial pellicular stationary phases (i.e. silica gel functionalized with octadecyl, biphenyl, phenylhexyl and pentafluorophenyl groups) were preliminarily investigated for the resolution of target analytes and different sorbent phases (i.e. octyl or octadecyl functionalized silica gel and a polymeric phase functionalized with N-benzylpyrrolidone groups) were tested for the SPE phase. The optimized method involves the QuEChERS extraction of 1 g of freeze-dried sludge with 15 mL of water/acetonitrile 1/2 (v/v), the SPE of the extract with the N-benzylpyrrolidone polymeric phase and the water/acetonitrile gradient elution on the pentafluorophenyl stationary phase at room temperature. Matrix effect was always suppressive and in most cases low, being it ≤20% for ASA, DIC, FLU, KET, IBU, 1-HYIBU, 2-HYIBU, 3-HYIBU, NAP and O-DMNAP, and included in the range of 35-47% for the other analytes. Recoveries were evaluated at three spiking levels, evidencing almost quantitative values for HYIBUs and O-DMNAP; for ASA, SAL and KET the recoveries were included in between 50 and 76%, whereas for the other compounds they ranged from 36% to 55%. The proposed method showed better analytical performances than those so far published, being suitable for target compound determination in real samples from tens of pg g(-1) to ng g(-1) of freeze-dried sludge, with a total analysis time of 30 min per sample. |
| File Format |
HTM / HTML |
| ISSN |
00032670 |
| Journal |
Analytica Chimica Acta |
| Volume Number |
935 |
| e-ISSN |
18734324 |
| Language |
English |
| Publisher |
Elsevier |
| Publisher Date |
2016-09-07 |
| Publisher Place |
Netherlands |
| Access Restriction |
One Nation One Subscription (ONOS) |
| Content Type |
Text |
| Resource Type |
Article |
| Subject |
Spectroscopy Environmental Chemistry Analytical Chemistry Biochemistry |
