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

作者:Maia Alexandra S; Ribeiro Ana R; Amorim Catarina L; Barreiro Juliana C; Cass Quezia B; Castro Paula M L; Tiritan Maria Elizabeth*
来源:Journal of Chromatography A, 2014, 1333: 87-98.
DOI:10.1016/j.chroma.2014.01.069

摘要

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) %26gt; 0.999), intra-day and inter-day precisions (RSD %26lt; 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.

  • 出版日期2014-3-14