Multi-walled carbon nanotubes modified with iron oxide and silver nanoparticles (MWCNT-Fe3O4/Ag) as a novel adsorbent for determining PAEs in carbonated soft drinks using magnetic SPE-GC/MS method

Abstract

The synthesis of compounds with an excellent adsorption capability plays an essential role to remove contaminants such as phthalic acid esters (PAEs) with potential carcinogenic characteristics from different food products. In this context, for the first time, a novel adsorbent (MWCNT-Fe3O4/Ag) was synthesized by using iron (magnetic agent), and silver (catalytic and surface enhancer agent) to further approach in a magnetic SPE-GC/MS method for determining of PAEs in carbonated soft drink samples. The limit of detection (LOD) and limit of quantification (LOQ) values of MSPE-GC/MS were determined in six PAEs as a range of 10.8–22.5 and 36–75 ng/L, respectively. Also, the calibration curves of PAEs were linear (R2 = 0.9981–0.9995) over the concentration level of 10.000 ng/L and the recoveries of the six PAEs were ranging from 96.60% to 109.22% with the RSDs less than 8%. Moreover, scanning electron microscopy (SEM), energy-dispersive X-ray (EDX), X-ray diffraction (XRD), vibrating sample magnetometry (VSM) and transmission electron microscopy analyses (TEM) were utilized to characterize the produced MWCNT-Fe3O4/Ag. Based on the findings, the surface of MWCNT is relatively uniform, which became coarser after loading with Fe3O4/Ag particles. Also, EDX spectrum showed the carbon (C), iron (Fe), oxygen (O), Ag and copper (Cu) are the main components of synthesized MWCNTs-Fe3O4/Ag. The successful adhesion of Fe3O4/Ag on the texture of MWCNTs using a co-precipitation method was confirmed by XRD and FT-IR assays. Additionally, excellent crystallinity and clear lattice nanocrystals fringes of prepared MWCNT-Fe3O4/Ag was demonstrated by TEM analysis. Based on the obtained VSM images, the prepared sorbent (MWCNT-Fe3O4/Ag) has the good magnetic performance for magnetic separation and extraction processes. It was concluded that the synthesized MWCNT-Fe3O4/Ag could be used as an efficient adsorbent for determining contaminants such as PAEs in different beverage samples. Keywords: Magnetic solid phase extraction (MSPE), Multi-walled carbon nanotubes (MWCNTs), Iron oxide (Fe3O4), Silver (Ag), Phthalic acid esters (PAEs)