Determination of fluoroquinolone antibiotics in wastewater using ultra high‐performance liquid chromatography with mass spectrometry and fluorescence detection |
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Authors: | Marcela Seifrtová Jana Aufartová Jitka Vytlačilová Angelina Pena Petr Solich Lucie Nováková |
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Institution: | 1. Department of Analytical Chemistry, Faculty of Pharmacy, Charles University, Hradec Králové, Czech Republic;2. Department of Pharmaceutical Botany and Ecology, Faculty of Pharmacy, Charles University, Hradec Králové, Czech Republic;3. Institute for Environmental Studies, Faculty of Science, Charles University, Prague, Czech Republic;4. Group of Health Surveillance, CEF, Faculty of Pharmacy, University of Coimbra, Coimbra, Portugal |
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Abstract: | A new ultra HPLC (UHPLC) method using both MS and fluorescence detection (FD) was developed for the determination of five fluoroquinolones in wastewaters. Systematic method development approach was compared with a conventional one. During the systematic approach, a possibility of automatic switching among four independent analytical columns of different chemistries has been used. Acidic as well as basic pH using ACN and methanol as organic modifiers was tested. The best separation of fluoroquinolones was obtained on phenyl analytical column at pH 10.5, which is a completely novel approach for separation of fluoroquinolones. Further, a new SPE procedure was developed for the sample preparation using basic pH as well. The sensitivity and selectivity of FD and MS detection were compared. FD at basic pH 10.5 demonstrated lower sensitivity than at acidic pH, which is conventionally performed. At basic pH, UHPLC‐MS/MS was found about two orders of magnitude more sensitive than FD. Both methods were validated and subsequently UHPLC‐FD method was used for the evaluation of stability of fluoroquinolones. UHPLC‐MS/MS method was used for the analysis of wastewater samples. Norfloxacin and ciprofloxacin were detected in samples of influent and effluent from wastewater treatment plant. Ofloxacin was detected only in influent from wastewater treatment plant. |
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Keywords: | Fluoroquinolones Systematic method development Ultra HPLC Wastewaters |
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