Rotating-disk sorptive extraction combined with LC/TOF-MS for determination of pharmaceuticals in environmental and biological samples

Becerra-Herrera, Mercedes; Cañas, Alejandro; Honda, Luis

Keywords: Sample preparation, LC/TOF-MS, pharmaceuticals, water, plasma

Abstract

Our research team developed in 2009 the sample preparation technique “rotating disk sorptive extraction” (RDSE). Currently this technique is available in two configurations. In the classic version, the sorbent phase is a polymer film adhered to one side of the Teflon disk (e.g. PDMS or C18). The second configuration consists of a disk that contains a cavity that is loaded with a sorbent phase (powder) and is then covered with a glass-fiber filter and sealed with a ring of Teflon. This configuration, with Oasis ® HLB and styrene-DVB, was used in this work for extraction of NSAIDs from wastewaters and lincomycin (LCM) and spectinomycin (SPM) from animal plasma, respectively. After optimization of the extraction process, chromatographic analyses were performed by UHPLC (Flexar FX-15), using a C18 (2.1 mm × 75 mm, 2.7 mm) column. In both analyses optimum separation was achieved with a binary mobile phase gradient at a flow rate of 0.3 mL/min. Quantification of the analytes was performed using an AxION 2 TOF MS system with a Dual Probe ESI source considering specific conditions for each analyte group (negative ionization for NSAIDs and positive for LCM and SPM). Acquisition function was always in Trap mode. Recoveries in both determinations were higher than 97% con relative standard deviation lower than 8%. NSAIDs were quantified in influent of a WWTP from the Santiago city. The concentrations of the drugs were from 0.25 to 1.35 µgL-1. Regarding LCM and SPM, the method was applied in pharmacokinetic studies in animal plasma.

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Fecha de publicación: 2015