title: Simultaneous determination of fluoroquinolones, sulfonamides and tetracyclines in sewage sludge by pressurized liquid extraction and liquid chromatography electrospray ionization-mass spectrometry.
abstract: A new scheme for the quantitative determination of traces of fluoroquinolones (FQs), tetracyclines (TCs) and sulfonamides (SAs) in sewage sludge was developed. The compounds were simultaneously extracted from sewage sludge by pressurized liquid extraction (PLE). A novel and effective method for PLE was developed. Solid-phase extraction was used for cleaning up the extracts. Identification and quantification of the compounds was done using high-performance liquid chromatography with electrospray ionization mass spectrometry in selected reaction monitoring mode. The best recovery of FQs and TCs was obtained by using hydrophilic-lipophilic balance cartridges, recoveries ranged 59% for norfloxacin to 82% for ofloxacin and 95% for doxycycline; for SAs strong cation-exchange cartridges were more efficient, recoveries were 96% for sulfamethoxazole and 43% for sulfadimethoxine. Limit of quantification ranged from 0.1 ng/g for SAs to 160 ng/g for tetracycline. Method precision for TCs was 5.06% and 1.12%, and for SAs 0.43% and 2.01%. FQs precision ranged from 0.77% to 1.89%.
authors: Department of Food Science and Hygiene, Estonian University of Life Sciences, Kreutzwaldi 58A, 51014 Tartu, Estonia.
authors: Merike
authors: M
authors: Lillenberg
authors: Sergei
authors: S
authors: Yurchenko
authors: Karin
authors: K
authors: Kipper
authors: Koit
authors: K
authors: Herodes
authors: Viljar
authors: V
authors: Pihl
authors: Kalev
authors: K
authors: Sepp
authors: Rünno
authors: R
authors: Lõhmus
authors: Lembit
authors: L
authors: Nei
mesh_terms: D005591:Chemical Fractionation / Q000295:instrumentation / Q000379:methods; D002853:Chromatography, Liquid / Q000379:methods*; D004867:Equipment Design; D024841:Fluoroquinolones / Q000032:analysis*; D011312:Pressure; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D012722:Sewage / Q000737:chemistry*; D052616:Solid Phase Extraction / Q000379:methods; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods*; D013449:Sulfonamides / Q000032:analysis*; D013754:Tetracyclines / Q000032:analysis*
chemical_list: D024841:Fluoroquinolones; D012722:Sewage; D013449:Sulfonamides; D013754:Tetracyclines