title: Fluoroquinolone residues in compost by green enhanced microwave-assisted extraction followed by ultra performance liquid chromatography tandem mass spectrometry.
abstract: A novel, simple and straightforward method for determination of fluoroquinolones (FQs) in compost has been developed. The procedure entails a low-pressurized microwave-assisted extraction (MAE) carried out by a high performance instrument, in alkaline aqueous solution containing magnesium ions as FQs complexing agent, followed by ultra performance liquid chromatography tandem mass spectrometry (UPLC-MS). Ciprofloxacin (CIP), Enrofloxacin (ENR), Levofloxacin (LEV) and Norfloxacin (NOR), four widely used FQ antibiotics, were simultaneously extracted from compost by a single MAE cycle (20min, 135°C). The method was validated in terms of linearity, selectivity, sensitivity and accuracy. Quantitative absolute recovery (70-112%, n=3) and suitable precision (RSD<15%, n=3) were observed, at concentration levels ranging from 25 ng g(-1) to 2500 ng g(-1). Analytes were separated in a 10min chromatographic run and quantified/confirmed in single reaction monitoring (SRM) mode. UPLC coupled to SRM-MS detection allowed to achieve improved sensitivity, and selective detection. Method detection and quantification limits, MDLs and MQLs, were in the range 2.2-3.0 ng g(-1) and 6.6-9.0 ng g(-1), respectively. The high-performance microwave system here used strongly improved the extraction efficiency with respect to a conventional apparatus. The procedure proved to be simpler, less expensive, faster, and more green with respect to the few methods currently described in literature, providing at the same time suitable recovery and reproducibility. The analytical method has been applied to the analysis of actual compost samples, wherein FQs have been quantified at concentrations up to 88 ng g(-1).
authors.affiliation: Department of Chemistry, University of Pavia, via Taramelli 12, 27100 Pavia, Italy.
authors.forename: Andrea
authors.initials: A
authors.lastname: Speltini
authors.affiliation: Department of Chemistry, University of Pavia, via Taramelli 12, 27100 Pavia, Italy. Electronic address: michela.sturini@unipv.it.
authors.forename: Michela
authors.initials: M
authors.lastname: Sturini
authors.affiliation: Department of Chemistry, University of Pavia, via Taramelli 12, 27100 Pavia, Italy.
authors.forename: Federica
authors.initials: F
authors.lastname: Maraschi
authors.affiliation: Department of Chemistry, University of Pavia, via Taramelli 12, 27100 Pavia, Italy.
authors.forename: Simona
authors.initials: S
authors.lastname: Viti
authors.affiliation: Department of Chemistry, University of Pavia, via Taramelli 12, 27100 Pavia, Italy.
authors.forename: Davide
authors.initials: D
authors.lastname: Sbarbada
authors.affiliation: Department of Chemistry, University of Pavia, via Taramelli 12, 27100 Pavia, Italy.
authors.forename: Antonella
authors.initials: A
authors.lastname: Profumo
mesh_terms: D000900:Anti-Bacterial Agents / Q000032:analysis*; D002851:Chromatography, High Pressure Liquid / Q000379:methods; D002939:Ciprofloxacin / Q000032:analysis; D004350:Drug Residues; D000077422:Enrofloxacin; D024841:Fluoroquinolones / Q000032:analysis*; D008872:Microwaves; D009643:Norfloxacin / Q000032:analysis; D015203:Reproducibility of Results; D012987:Soil / Q000737:chemistry*; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods; D053719:Tandem Mass Spectrometry / Q000379:methods
chemical_list: D000900:Anti-Bacterial Agents; D024841:Fluoroquinolones; D012987:Soil; D000077422:Enrofloxacin; D002939:Ciprofloxacin; D009643:Norfloxacin
keywords: Compost; Emerging pollutants; Fluoroquinolones; Green analytical chemistry; Microwave-assisted extraction; UPLC–MS