Magnetic-Dispersive Solid Phase Extraction Based on Graphene Oxide-Fe₃O₄ Nanocomposites Followed by High Performance Liquid Chromatography-Fluorescence for the Preconcentration and Determination of Terazosin Hydrochloride in Human Plasma

In the present study, a facile modified impregnation method was employed to synthesize superparamagnetic graphene oxide-Fe3O4 (GO-Fe3O4) nanocomposites. Based on the GO-Fe3O4 as adsorbent, a simple and fast magnetic-dispersive solid phase extraction followed by high performance liquid chromatography with fluorescence detection (M-dSPE-HPLC-FL) method was established and validated for the preconcentration and determination of terazosin hydrochloride (TRZ) in human plasma samples. The obtained nanomaterials were characterized by X-ray diffraction, Fourier transform infrared spectroscopy, scanning electron microscopy, energy dispersive X-ray spectroscopy and vibrating sample magnetometry. Different parameters affecting the extraction efficiency, such as sample pH, amount of sorbent, extraction time, elution solvent and its volume and desorption time, were evaluated and optimized. The linearity of the proposed method was excellent over the range 0.3-50.0 ng mL(-1) with an acceptable coefficient of determination (R-2 = 0.9989). The limit of quantification and limit of detection were found to be 0.3 and 0.09 ng mL(-1), respectively, and the preconcentration factor of 10 was achieved. Intra-and inter-day precision expressed as relative standard deviation (RSD %, n = 6) were between 2.2-3.8% and 4.7-6.4%, respectively. Accuracy, estimated by recovery assays, was 97.7-106.6% with RSD <= 5.2%. Ultimately, the applicability of the method was successfully confirmed by the extraction and determination of TRZ in human plasma samples.