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Degradation of fluoroquinolone antibiotics and identification of metabolites/transformation products by liquid chromatography-tandem mass spectrometry

Title
Degradation of fluoroquinolone antibiotics and identification of metabolites/transformation products by liquid chromatography-tandem mass spectrometry
Type
Article in International Scientific Journal
Year
2014
Authors
Alexandra S. Maia
(Author)
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Catarina L. Amorim
(Author)
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Juliana C. Barreiro
(Author)
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Quezia B. Cass
(Author)
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Paula M. L. Castro
(Author)
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Maria Elizabeth Tiritan
(Author)
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Journal
Vol. 1333
Pages: 87-98
ISSN: 0021-9673
Publisher: Elsevier
Other information
Authenticus ID: P-009-63K
Abstract (EN): Antibiotics are a therapeutic class widely found in environmental matrices and extensively studied due to its persistence and implications for multi-resistant bacteria development. This work presents an integrated approach of analytical multi-techniques on assessing biodegradation of fluorinated antibiotics at a laboratory-scale microcosmos to follow removal and formation of intermediate compounds. Degradation of four fluoroquinolone antibiotics, namely Ofloxacin (OFL), Norfloxacin (NOR), Ciprofloxacin (CPF) and Moxifloxacin (MOX), at 10 mg L-1 using a mixed bacterial culture, was assessed for 60 days. The assays were followed by a developed and validated analytical method of LC with fluorescence detection (LC-FD) using a Luna Pentafluorophenyl (2) 3 pm column. The validated method demonstrated good selectivity, linearity (r(2) > 0.999), intra-day and inter-day precisions (RSD < 2.74%) and accuracy. The quantification limits were 5 mu g L-1 for OFL, NOR and CPF and 20 mu g L-1 for MOX. The optimized conditions allowed picturing metabolites/transformation products formation and accumulation during the process, stating an incomplete mineralization, also shown by fluoride release. OFL and MOX presented the highest (98.3%) and the lowest (80.5%) extent of degradation after 19 days of assay, respectively. A representative number of samples was selected and analyzed by LC-MS/MS with triple quadrupole and the molecular formulas were confirmed by a quadruple time of flight analyzer (QqTOF). Most of the intermediates were already described as biodegradation and/or photodegradation products in different conditions; however unknown metabolites were also identified. The microbial consortium, even when exposed to high levels of FQ presented high percentages of degradation, never reported before for these compounds.
Language: English
Type (Professor's evaluation): Scientific
No. of pages: 12
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