Microbial degradation is the most important process to remove organic pollutants in Waste Water
Treatment Plants. Regarding chiral compounds this process is normally enantioselective and needs the
suitable analytical methodology to follow the removal of both enantiomers in an accurate way. Thus, this
paper describes the development and validation of an enantioselective High Performance Liquid
Chromatography with Fluorescence Detection (HPLC-FD) method for simultaneous analysis of fluoxetine
(FLX) and norfluoxetine (NFLX) in wastewater effluents. Briefly, this method preconcentrated a small
volume of wastewater samples (50 mL) on 500 mg Oasis MCX cartridges and used HPLC-FD with a
vancomycin-based chiral stationary phase under reversed mode for analyses. The optimized mobile
phase was EtOH/aqueous ammonium acetate buffer (92.5/7.5, v/v) at pH 6.8. The effect of EtOH percentage,
buffer concentration, pH, column oven temperature and flow rate on chromatographic parameters
was systematically investigated. The developed method was validated within the wastewater effluent
used in microcosms laboratory assays. Linearity (R2 > 0.99), selectivity and sensitivity were achieved in
the range of 4.0–60 ng mL1 for enantiomers of FLX and 2.0–30 ng mL1 for enantiomers of NFLX. The
limits of detection were between 0.8 and 2.0 ng mL1 and the limits of quantification were between
2.0 and 4.0 ng mL1 for both enantiomers of FLX and the enantiomers of its demethylated metabolite
NFLX. The validated method was successfully applied and proved to be robust to follow the degradation
of both enantiomers of FLX in wastewater samples, during 46 days.
2
Microbial degradation is the most important process to remove organic pollutants in Waste WaterTreatment Plants. Regarding chiral compounds this process is normally enantioselective and needs thesuitable analytical methodology to follow the removal of both enantiomers in an accurate way. Thus, thispaper describes the development and validation of an enantioselective High Performance LiquidChromatography with Fluorescence Detection (HPLC-FD) method for simultaneous analysis of fluoxetine(FLX) and norfluoxetine (NFLX) in wastewater effluents. Briefly, this method preconcentrated a smallvolume of wastewater samples (50 mL) on 500 mg Oasis MCX cartridges and used HPLC-FD with avancomycin-based chiral stationary phase under reversed mode for analyses. The optimized mobilephase was EtOH/aqueous ammonium acetate buffer (92.5/7.5, v/v) at pH 6.8. The effect of EtOH percentage,buffer concentration, pH, column oven temperature and flow rate on chromatographic parameterswas systematically investigated. The developed method was validated within the wastewater effluentused in microcosms laboratory assays. Linearity (R2 > 0.99), selectivity and sensitivity were achieved inthe range of 4.0–60 ng mL1 for enantiomers of FLX and 2.0–30 ng mL1 for enantiomers of NFLX. Thelimits of detection were between 0.8 and 2.0 ng mL1 and the limits of quantification were between2.0 and 4.0 ng mL1 for both enantiomers of FLX and the enantiomers of its demethylated metaboliteNFLX. The validated method was successfully applied and proved to be robust to follow the degradationof both enantiomers of FLX in wastewater samples, during 46 days. 2
การแปล กรุณารอสักครู่..