The core–shell nanosized magnetic molecularly imprinted polymers for selective preconcentration and determination of ciprofloxacin in human fluid samples using a vortex-assisted dispersive micro-solid-phase extraction and high-performance liquid chromatography
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A simple method has been developed for the selective separation/preconcentration and determination of ciprofloxacin (CIP) in human fluid samples by using a shaker vortex-assisted magnetic dispersive micro-solid-phase extraction method and high-performance liquid chromatography. The magnetic nanosized molecularly imprinted polymer (Fe3O4@SiO2@NH2-MIP), used as the solid-phase extractor, was synthesized via the surface imprinting method and was further characterized by Fourier transform infrared spectrometry, energy-dispersive X-ray spectroscopy, scanning electron microscopy and vibrating sample magnetometer. The characterization results show that the adsorbent has suitable features for further adsorption process. The nanomagnetic molecularly imprinted polymers (NMMIPs) carrying the CIP could be easily separated from the aqueous solution by applying an external magnetic field. The parameters affecting the adsorption and extraction efficiency such as pH, desorption solvent type, weight of adsorbent, shaker and vortex time were optimized. The selectivity of the NMMIPs was evaluated according to its recognition to CIP and its analogues. The synthesized NMMIPs showed high adsorption capacity and selectivity for the template molecule. The maximum adsorption capacity of adsorbent was 166 mg g−1. The experiments exhibited a wide linear range of 0.92–10,000 µg L−1 for CIP with the correlation coefficient (R2) of 0.9973 and relative standard deviations of less than 4%. The limit of detection and limit of quantitation were calculated to be 0.28 and 0.92 µg L−1, respectively. The applicability of the developed procedure was further successfully evaluated by determination of CIP in human serum, plasma, urine and pharmaceutical samples.
KeywordsCiprofloxacin Dispersive Micro-solid-phase extraction Urine Plasma Serum
The authors greatly appreciate the financial support of this work by Shahid Chamran University of Ahvaz Research Council.