期刊
JOURNAL OF SEPARATION SCIENCE
卷 33, 期 14, 页码 2094-2108出版社
WILEY-V C H VERLAG GMBH
DOI: 10.1002/jssc.201000215
关键词
Fluoroquinolones; Systematic method development; Ultra HPLC; Wastewaters
资金
- MSM [0021620822]
- Grant Agency of the Academy of Sciences of the Czech Republic [KJB 601100901]
- Grant Agency of the MSMT of the Czech Republic - FRVS [1106/2010]
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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