Publication details

Determination of antibiotics (tetracyclines and sulfonamides) in biosolids by pressurized liquid extraction and liquid chromatography-tandem mass spectrometry

Authors

PAMREDDY Annapurna HIDALGO M. HAVEL Josef SALVADO Victoria

Year of publication 2013
Type Article in Periodical
Magazine / Source Journal of Chromatography A
MU Faculty or unit

Faculty of Science

Citation
Web http://authors.elsevier.com/sd/article/S0021967313007644
Doi http://dx.doi.org/10.1016/j.chroma.2013.05.014
Field Biochemistry
Keywords Liquid chromatography-tandem mass spectrometry; Pressurized liquid extraction; Tetracyclines; Sulfonamides; Sludge; Wastewater treatment plants
Description A robust and sensitive analytical method is developed to quantitatively determine tetracyclines and sulfonamides, two major antibiotic classes, in sewage sludge. The antibiotic agents, oxytetracycline, tetracycline, dioxycycline, chlorotetracycline, sulfathiazole, sulfapyridine, sulfamethazine and sulfamethoxazole, were extracted using pressurized liquid extraction (PLE) with citric acid at pH 3 and methanol (1:1 v/v). Clean-up of the extracts was performed by solid phase extraction (SPE) with hydrophilic-lipophilic balance cartridges. Identification and quantification of the compounds is by liquid chromatography-tandem mass spectrometry in multiple reaction monitoring (MRM) mode. High recoveries ranging from 90.4 to 99.9% for sulfonamides and 96.2 to 100.9% for the tetracyclines are obtained. Method detection limits (MDLs) range from 0.6 to 4.2 ng/g for sulfonamides and 3.2 to 13 ng/g for tetracyclines. After validation, the method is applied to the analysis of sludges collected from different WWTPs in Spain. (C) 2013 Elsevier B.V. All rights reserved.

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