Magnetic Solid-Phase Extraction Based on Silica and Graphene Materials for Sensitive Analysis of Emerging Contaminants in Wastewater with the Aid of UHPLC-Orbitrap-MS

With the advancement of technology and nanotechnology, new extraction sorbents have been created and effectively used for the magnetic solid-phase extraction of target analytes. Some of the investigated sorbents have better chemical and physical properties, exhibiting high extraction efficiency and strong repeatability, combined with low detection and quantification limits. In this study graphene oxide (GO) magnetic composites were prepared and used as magnetic solid-phase extraction (MSPE) adsorbents along with synthesized silica based magnetic nanoparticles (MNPs) functionalized with the C18 group for the preconcentration of emerging contaminants (ECs) in wastewater samples generated from hospital and urban facilities. The sample preparation with magnetic materials was followed by UHPLC-Orbitrap MS analysis for the accurate identification and determination of trace amounts of pharmaceutical active compounds and artificial sweeteners in effluent wastewater. Optimal conditions were used for the extraction of ECs from the aqueous samples, prior to UHPLC-Orbitrap MS determination. The proposed methods achieved low quantitation limits between 1.1-33.6 ng L-1 and 1.8-98.7 ng L-1 and satisfactory recoveries in the range of 58.4%-102.6%. An intra-day precision of less than 23.1% was achieved, while inter-day RSD% values in the range of 5.6-24.8% were observed. These figures of merit suggest that our proposed methodology is suitable for the determination of target ECs in aquatic systems.