Silica-coated magnetic iron oxide functionalized with hydrophobic polymeric ionic liquid: a promising nanoscale sorbent for simultaneous extraction of antidiabetic drugs from human plasma prior to their quantitation by HPLC

Abstract

Herein, silica-coated iron oxide nanoparticles modified with imidazolium-based polymeric ionic liquid (Fe₃O₄@SiO₂@PIL) were fabricated as a sustainable sorbent for magnetic solid-phase extraction (MSPE) and simultaneous determination of trace antidiabetic drugs in human plasma by high-performance liquid chromatography-ultraviolet detection (HPLC-UV). The Fe₃O₄ core was functionalized by silica (SiO₂) and vinyl layers where the ionic liquid 1-vinyl-3-octylimidazolium bromide (VOIM-Br) was attached through a free radical copolymerization process. In order to achieve hydrophobic magnetic nanoparticles and increase the merits of the sorbent, Br⁻ anions were synthetically replaced with PF₆⁻. The properties and morphology of the sorbent were characterized by various techniques and all the results illustrated the prosperous synthesis of Fe₃O₄@SiO₂@PIL. A comprehensive study was carried out to investigate and optimize various parameters affecting the extraction efficiency. The limit of detection (LOD, S/N = 3) for empagliflozin, metformin and canagliflozin was 1.3, 6.0 and 0.8 ng mL⁻¹, respectively. Linearity (0.997 ≥ r² ≥ 0.993) and linear concentration ranges of 5.0–1200.0, 20.0–1800.0 and 5.0–1000.0 ng mL⁻¹ were obtained for empagliflozin, metformin and canagliflozin, respectively. Intra-assay (3.8–7.5%, n = 9) and inter-assay (3.2–8.5%, n = 12) precisions as well as accuracies (≤9.1%) displayed good efficiency of the method. Finally, the method was applied for the quantitation of antidiabetic drugs in human plasma after oral administration and main pharmacokinetic data including T_max (h), C_max (ng mL⁻¹), AUC_0–24 (ng h mL⁻¹), AUC_0–∞ (ng h mL⁻¹), and T_1/2 (h) were evaluated.