Journal
JOURNAL OF CHROMATOGRAPHY A
Volume 1216, Issue 32, Pages 5949-5954Publisher
ELSEVIER SCIENCE BV
DOI: 10.1016/j.chroma.2009.06.029
Keywords
Sewage sludge; Fluoroquinolones; Tetracyclines; Sulfonamides; PLE; SPE; HPLC-ESI-MS
Funding
- Estonian Environmental Investment Centre, Estonian Science Foundation [6658, 7127]
- Estonian research target [SF 0180058s07]
- Estonian Nanotechnology Competence Centre
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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%. (C) 2009 Elsevier B.V. All rights reserved.
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