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. 2019 Mar 9;13(1):28.
doi: 10.1186/s13065-019-0543-5. eCollection 2019 Dec.

Salting-out assisted liquid-liquid extraction for the determination of ciprofloxacin residues in water samples by high performance liquid chromatography-diode array detector

Teshome Gezahegn  1 , Bisratewongel Tegegne  1   2 , Feleke Zewge  1 , Bhagwan Singh Chandravanshi  1
Affiliations

Salting-out assisted liquid-liquid extraction for the determination of ciprofloxacin residues in water samples by high performance liquid chromatography-diode array detector

Teshome Gezahegn et al. BMC Chem. .

Abstract

Background: The occurrence of emerging pollutants like pharmaceuticals and related compounds in the aquatic and terrestrial environments is of increasing concern. Ciprofloxacin is one of the pharmaceuticals which is active against a wide range of bacteria. The main objective of this research is to develop a simple method for the extraction and determination of ciprofloxacin residues in environmental water samples.

Results: A salting-out assisted liquid-liquid extraction (SALLE) method for the determination of ciprofloxacin in water samples by high-performance liquid chromatography with diode array detector (HPLC-DAD) was developed. The calibration curve was linear over the range of 0.1-100 μg/L with coefficient of determination (r2) of 0.9976. The limits of detection (LOD) and quantification (LOQ) of the method were 0.075 and 0.25 µg/L, respectively. The reproducibility in terms of relative standard deviation (% RSD) was less than 10%. The applicability of the developed method was investigated by analyzing tap water, bottled mineral water and waste water and demonstrated satisfactory recoveries in the ranges of 86.4-120%.

Conclusion: The method offered a number of features including wide linear range, good recovery, short analysis time, simple operation process and environmental friendly. The developed method can be utilized as an attractive alternative for the determination of ciprofloxacin residues in environmental water matrices.

Keywords: Ciprofloxacin; Emerging pollutants; High performance liquid chromatography–diode array detector; Pharmaceuticals; Potable water; Salting-out assisted liquid–liquid extraction; Wastewater.

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Conflict of interest statement

The authors declare that they have no competing interests.

Figures

Fig. 1
Fig. 1
Structure of ciprofloxacin
Scheme 1
Scheme 1
Flow chart of SALLE for the determination of ciprofloxacin
Fig. 2
Fig. 2
Effect of volume of extraction solvent on the SALLE efficiency
Fig. 3
Fig. 3
Effects of pH on the SALLE efficiency
Fig. 4
Fig. 4
Effect of salt type on the SALLE efficiency
Fig. 5
Fig. 5
Effect of the salt amount on the SALLE efficiency
Fig. 6
Fig. 6
Effect of centrifuge speed on the SALLE efficiency
Fig. 7
Fig. 7
Effect of extraction time on the SALLE efficiency
Fig. 8
Fig. 8
Typical representative chromatogram of a unspiked and b spiked wastewater. Extraction conditions: 10 mL spiked at 0.1 μg/mL; volume of acetonitrile, 5 mL; amount of salt added, 4 g MgSO4; extraction time, 6 min; pH of the sample solution, 3; centrifugation speed, 4000 rpm; n = 3
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