Optimized Quechers Method for the Determination of Ciprofloxacin in Wastewater by Using High Performance Liquid Chromatography- Diode Array Detector (Hplc-Dad)

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Addis Ababa University


An optimized QuEChERS-HPLC/DAD method was developed for the detection and determination of a pharmaceutically emerging pollutant ciprofloxacin (1-cyclopropyl-6-fluoro-4-oxo-7-piperazin-1-yl quinolin-3-carboxylic acid) from river water and waste water sample from pharmaceutical, hospital and sewage treatment plant. The ciprofloxacin level was determined with high performance liquid chromatography diode array detector (HPLC-DAD). A sample of ciprofloxacin was used to develop an analytical method in the optimization experiment, which involved the selection of the most suitable salt, pH and different parameters for the extraction of ciprofloxacin from liquid sample. The usefulness of the method was verified based on the recovery. Different salt types were tested. The obtained results showed that the best recovery of 95% was obtained using MgSO4 with the addition of acetonitrile in the sample extraction steps. The optimized method was applied for the determination of ciprofloxacin in five waste water samples. The method was validated using real sample: distilled water, tap water, bottled water and waste water samples spiked with ciprofloxacin at different concentration levels. The percentage recovery ranged from 86 to 120% with relative standard deviation (RSD) less than 6% for spiked level 0.02, 0.1, 1.25, 2.5 and 5 g/mL. The calibration curve was linear in the range 0.005 to 5.0 g/mL. The limit of detection (LOD) and limit of quantification (LOQ) were 0.45 g/L and 1.5 g/L, respectively. The optimized method was adequate for the detection and determination of ciprofloxacin residue in waste water sample. The analytical parameters of the newly optimized method were compared with the literature methods and showed the optimized method is comparable with most of the literature methods.



Optimized Quechers, Method for the Determination, Ciprofloxacin in Wastewater, Performance Liquid, Chromatography- Diode Array Detector (Hplc-Dad)