Graphene oxide/Fe3O4@polythionine nanocomposite as an efficient sorbent for magnetic solid-phase extraction followed by high-performance liquid chromatography for the determination of duloxetine in human plasma

摘要

Herein, an efficient graphene oxide/Fe3O4@polythionine (GO/Fe3O4/PTh) nanocomposite sorbent was introduced for magnetic solid-phase extraction combined with high-performance liquid chromatography-ultraviolet detection of duloxetine (DLX) in human plasma. To prepare the sorbent, an oxidative polymerization of thionine on the surface of magnetic GO was utilized while PTh was simply used as a surface modifier to improve extraction efficiency. Transmission electron microscopy, scanning electron microscopy, X-ray diffraction, energy-dispersive X-ray analysis, vibrating sample magnetometry, Fourier transform-infrared spectroscopy and Brunauer-Emmett-Teller technique were applied to characterize the prepared nanoparticles. Firstly, effective parameters controlling the performance of the extraction process were evaluated in detail and optimized. Under the optimized conditions, calibration curve showed linearity in the range of 2-2500 ng mL(-1) with regression coefficient corresponding to 0.998. Limits of detection (LOD, S/N = 3) and quantification (LOQ, S/N = 10) were 0.5 and 2 ng mL(-1), respectively. Reasonable intra-assay (3.5-4.5%, n = 6) and inter-assay (3.8-6.7%, n = 9) precision represented acceptable performance of the procedure. The applicability of the method was successfully extended to the determination of DLX in human plasma after oral administration of 60 mg single dose of the drug and finally some pharmacokinetic data was achieved.