Improved resolution of fluoroquinolones using cetyltrimethyl ammonium bromide–micellar electrokinetic chromatography and its application to residue analysis in surface water

Abstract

A simple micellar electrokinetic chromatography (MEKC), using cetyltrimethyl ammonium bromide (CTAB) as micelles, for the determination of ciprofloxacin (CIP), enrofloxacin (ENR), norfloxacin (NOR) and ofloxacin (OFL) residues in surface water was developed. Peak Master was used for predicting amounts of analyte ionic forms to reduce numbers of tedious experiments in optimizing the analyte capacity factors. A baseline separation (Rs > 2.8) of the analytes was achieved in 7 min using 15 mM sodium dihydrogen phosphate (pH 6.0) containing 3 mM CTAB and a capillary with an effective length of 56.0 cm. A negative polarity voltage of 20 kV was used to enable the migration of the cationic micelles toward the detection site. The method shows good linearity in a range of 5 and 20 μg mL−1 and precision (%RSD < 6.45). Percent recoveries of the method were in a range of 65.1–88.7%. The limits of detection and quantitation were in the ranges of 1–2 and 3–5 μg mL−1, respectively. Two steps sample clean-up and preconcentration of surface water samples by hydrophilic-lipophilic balance and fluoroquinolone-molecularly imprinted polymer were advantageous for removal of humic acids and enabling the detection of fluoroquinolone residues in the samples. Finally, the method was applied for fluoroquinolone residues analysis of surface water in Thailand.