Abstract
A highly stable flow-injection amperometric sensor for dexamethasone (DEX) was developed using a pencil graphite electrode (PGE) modified with Fe-based metal organic frameworks, MIL-100(Fe) and graphene oxide composite materials (MIL-100(Fe)/GO). Scanning electron microscopy and energy-dispersive X-ray spectroscopy, transmission electron microscopy, powder X-ray diffraction, and Fourier-transform infrared spectroscopy were used to characterize the MIL-100(Fe) composites. The MIL-100(Fe)/GO-modified PGE (denoted MIL-100(Fe)/GO/PGE) was further electrochemically characterized using cyclic voltammetry. As an electrode material, MIL-100(Fe) is a sensing element that undergoes oxidation from Fe(ii)-MOF to Fe(iii)-MOF, and GO possesses high conductivity and a large surface area, which exhibits high absorbability. In the presence of DEX, Fe(iii) is reduced, which accelerates electron transfer at the electrode interface. Therefore, DEX can be quantitatively detected by analyzing the anodic current of MIL-100(Fe). When coupled with amperometric flow injection analysis, excellent performance can be obtained even when a low detection potential is applied (+0.10 V vs. Ag/AgCl). The concentration was linear in the range 0.10-5.0 μM and 0.010-5.0 mM with LOD of 0.030 μM based on 3(sd/slope). The modified electrode also exhibited a remarkably stable response under optimized conditions, and up to 55 injections can be used per electrode. The sensor exhibits high repeatability, reproducibility, and anti-interference properties when used for DEX detection. The effective determination of dexamethasone in real pharmaceutical and cosmetic samples demonstrated the feasibility of the electrochemical sensor, and the results were in good agreement with those obtained from the HPLC-DAD analysis. Acceptable percentage recoveries from the spiked pharmaceutical and cosmetic samples were obtained, ranging from 93-111% for this new method compared with 84-107% for the HPLC-DAD standard method.