Self-synthesized TiO₂ nanoparticles-pH-mediated dispersive solid phase extraction coupled with high performance...

A simple and efficient pH-mediated dispersive solid phase extraction (dSPE) based on terbium doped titanium dioxide nanoparticles (TiO₂-Tb NPs) combined with high performance liquid chromatography (HPLC) has been firstly developed for the determination of quinolones (QNs) in various biological samples. The adsorption kinetics and isotherms were investigated to indicate that the kinetic and equilibrium adsorption were well-described by pseudo-second order kinetic and Henry, Langmuir isotherm model, respectively. The parameters influencing the extraction performance were systematically investigated. The QNs are transferred into TiO₂-Tb NPs in the first step at pH = 6.0 and eluted into acidic aqueous phase at pH = 2.5 in the second step. Under the optimum extraction and determination conditions, a linearity range with the coefficient of determination (R²) from 0.9977 to 0.9991 were obtained in a range of 10-10,000 ng mL^-1. The limits of detection (LODs) based on a signal-to-noise ratio of 3 were 3.3 ng mL^-1. The recoveries of the three QNs in human urine, rabbit plasma and serum samples ranged from 69.3% to 117.6%, with standard deviations ranging from 2.4% to 9.9%. Therefore, this pH-mediated dSPE-HPLC method exhibited the advantages of remarkable sensitivity, ease of operation, rapidity, low cost and environmental friendliness.