Application of Graphene-based Solid-Phase Extraction Coupled with Ultra High-performance Liquid Chromatography-Tandem Mass Spectrometry for Determination of Macrolides in Fish Tissues

A novel analytical protocol for the determination of five macrolides (MLs) in crucian carp tissues has been developed. Two-dimensional (2D) planar graphene powder was utilized as the solid-phase extraction (SPE) sorbent for analyte enrichment and cleanup. The target analytes were separated by ultra high-performance liquid chromatography (LC) and quantified by a triple-quadrupole linear ion trap mass spectrometer. The proposed analytical procedures were carefully optimized and validated. Average recoveries of MLs were between 81.7 and 110.5 %, which was the highest comparing with the conventional sorbents including C18 silica and multiwalled carbon nanotubes (MWCNTs). Method validation proved the feasibility of the developed nanoparticles for the quantificatation of the investigated analytes at trace levels obtaining low limit of quantitation values in the microgram per kilogram range. Good precision with coefficients of variations always lower than 10 % was obtained. The proposed method has been successfully applied to the analysis of ML in several aquaculture product samples, indicating that graphene was a potential SPE sorbent for the enrichment of trace residues in food samples.