Innovative combination of QuEChERS extraction with on-line solid-phase extract purification and pre-concentration, followed by liquid chromatography-tandem mass spectrometry for the determination of non-steroidal anti-inflammatory drugs and their metabolites in sewage sludge.

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ID: 64949
2016
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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.
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rossini2016innovativeanalytica Use this key to autocite in the manuscript while using SciMatic Manuscript Manager or Thesis Manager
Authors Rossini, D;Ciofi, L;Ancillotti, C;Checchini, L;Bruzzoniti, M C;Rivoira, L;Fibbi, D;Orlandini, S;Del Bubba, M;
Journal analytica chimica acta
Year 2016
DOI
10.1016/j.aca.2016.06.023
URL
Keywords
sewage sludge quechers liquid chromatography-tandem mass spectrometry drug metabolites non-steroidal anti-inflammatory drugs solid-phase pre-concentration and purification

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