One-step green synthesis of β-cyclodextrin/iron oxide-reduced graphene oxide nanocomposite with high supramolecular recognition capability: Application for vortex-assisted magnetic solid phase extraction of organochlorine pesticides residue from honey samples

Abstract

In this research, β-cyclodextrin/iron oxide reduced graphene oxide hybrid nanostructure (β-CD/MRGO) with high water dispersability, excellent magnetic responsivity and molecular selectivity was prepared via a facile one step green strategy. The obtained nanomaterial was characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), Raman spectroscopy, and vibrating sample magnetometry (VSM), which confirmed the modification of GO with β-CD and magnetic nanoparticles. The formation mechanism of β-CD/MRGO was also discussed. The prepared magnetic nanocomposite was then applied as adsorbent in the vortex-assisted magnetic solid phase extraction (MSPE) of 16 organochlorine pesticides (OCPs) from honey samples prior to gas chromatography-electron capture detection (GC-ECD) analysis. Optimum extraction conditions have been assessed with respect to vortex time, sample pH, adsorbent amount, and salt concentration as well as desorption conditions (type and volume of desorption solvent and desorption time). A good level of linearity (2–10,000ngkg−1) with satisfactory determination coefficients (R2>0.9966) and suitable precision (%RSDs less than 7.8) was obtained for OCPs under the optimal conditions. The limits of detection and quantification of the method were obtained in the sub-parts per trillion (ppt) to parts per trillion range (LOD: 0.52–3.21ngkg−1; LOQ: 1.73–10.72ngkg−1) based on 3 and 10 signal to noise ratios, respectively. The MSPE method was successfully applied to analysis of OCPs in honey samples with recoveries in the range of 78.8% to 116.2% and RSDs (n=3) below 8.1%. The results demonstrated that β-CD/MRGO could exhibit good supramolecular recognition, enrichment capability and high extraction recoveries toward OCPs.