Determination of quinolone antibiotics in surface water by MnFe2O4@TiO2 magnetic solid phase extraction-high performance liquid chromatography

Abstract

The magnetic solid phase extraction material (MnFe2O4@TiO2) was prepared by coating TiO2 on MnFe2O4 through an in-situ formation method. The structure and properties of MnFe2O4@TiO2 were characterized by X-ray diffractometer (XRD), scanning electron microscope (SEM), nitrogen adsorption–desorption experiment, and vibrating sample magnetometer (VSM). The conditions for magnetic solid phase extraction (MSPE) of quinolone antibiotics were optimized, and an MSPE-HPLC method was established to determine quinolone antibiotics in water samples. The optimal conditions for MSPE are MnFe2O4@TiO2 amount of 15 mg, extraction time of 15 min, 5 mL of methanol solution with 20 % ammonia as eluent, and elution time of 1 min. Under the optimal conditions, 50 mL 0.1 mg/L mixed standard solutions of fleroxacin, ofloxacin, norfloxacin, ciprofloxacin, and enrofloxacin have achieved enrichment multiples of 67.8, 72.1, 59.6, 55.8, and 60.7, respectively. The linear range of five antibiotics determined by MSPE-HPLC is 0.004–1 mg/L with the relative standard deviations (RSDs) of 2.1 %–4.9 % and the limits of detection (LODs) of 0.0006–0.0020 mg/L. The method is applied to the determination of the five antibiotics in rice paddy water and fish pond water; the recoveries range from 78.9 to 105.8 %, and the RSDs (n = 5) are 3.6 %–8.7 %.