Abstract
A nanohybrid material termed graphene oxide/metal-organic framework-74/Fe3O4/polytyramine (GO/MOF-74/Fe3O4/PTy) was fabricated and applied in magnetic dispersive micro-solid phase extraction (MD-µ-SPE) coupled with high performance liquid chromatography (HPLC) for simultaneous determination of fluoroquinolones compounds including, ofloxacin, ciprofloxacin, lomefloxacin, enrofloxacin and sperfloxacin in egg samples. The GO/MOF-74/Fe3O4/PTy nanocomposite was fabricated through an in situ synthesis of MOF-74 in the presence of magnetic GO and followed with an oxidative polymerization of tyramine using horsedish peroxide (HRP) enzyme. The modifier agents improved the merits of the nanoporous sorbent. Extraction protocols based on GO/MOF nanocomposites have various benefit such as, the high stability, the tunable porosity, the fast mast transfer and reasonable enrichment factor. The fabricated material was characterized via energy dispersive x-ray analysis (EDX), the scanning electron microscopy (SEM), Fourier-transform infrared spectroscopy (FT-IR), and the x-ray diffraction (XRD). The calibration curves revealed linearity (0.992 ≤ r2 ≤ 0.997) in the ranges of 1.0-475.0, 0.5-350.0, 0.5-350.0, 0.5-375.0 and 1.5-300.0 ng mL-1 with limit of detections (LODs, S/N=3) of 0.3, 0.1, 0.2, 0.1 and 0.4 ng mL-1 for ofloxacin, ciprofloxacin, lomefloxacin, enrofloxacin and sperfloxacin, respectively. The intra-assay (≤7.7%, n = 9) and inter-assay (≤7.0%, n = 9) precisions along with accuracy less than 9.0% were obtained.
Highlights
Fluoroquinolones (FQs) such as ofloxacin, ciprofloxacin, lomefloxacin, enrofloxacin and sparfloxacin (Fig. 1) have great importance due to the various hazardous side effects and allergic problems [2]
74/Fe3O4/ PTy obviously shows the modification process of graphene oxide (GO) with the layers of target polymer. As it can be seen, PTy layers have grown on the surface of GO and formed significant coating sheets, demonstrating prosperous synthesis of the final nanoscale extractor
By referring to energy dispersive x-ray analysis (EDX) spectra of MOF-74 and GO/MOF-74, it could be possible to determine the successful immobilization of MOF-74 on the surface of GO (Fig. 5)
Summary
Fluoroquinolones (FQs) such as ofloxacin, ciprofloxacin, lomefloxacin, enrofloxacin and sparfloxacin (Fig. 1) have great importance due to. In order to enhance the qualities of a carbon based material for extraction purposes, conductive polymers such as polythionine, polyaniline, polythiophene, polytyramine (PTy) seem appreciable alternatives which significantly increase π-π interaction, hydrophobic property, extraction capacity, diffusion rate and reusability [37,38,39,40,41,42,43] Among these polymers, PTy can be synthesized through a simple and inexpensive oxidative polymerization route in the presence of horseradish peroxidaze (HRP) enzyme as a catalyst and existence of alkyl groups in this polymer results the establishment of macropores on the surface of sorbent. A: Schematic diagram of the synthesis routes of GO/MOF-74/Fe3O4/PTy. B: different steps of MD-μ-SPE-HPLC-UV method in extraction, enrichment and isolation of FQs the magnet again to collect solution. 20.0 μL of the obtained sample was injected into HPLC for analyzing FQs
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