Rapid determination of trace sulfonamides in fish by graphene-based SPE coupled with UPLC/MS/MS

An analytical protocol for simultaneous determination of thirteen sulfonamides in fish tissues has been developed. Target analytes were enriched by solid-phase extraction using graphene as a sorbent and quantified by ultra-high-performance liquid chromatography coupled with triple-quadrupole linear ion trap mass spectrometry. In the present work, graphene was systematically evaluated as a solid-phase extraction sorbent for analyte enrichment and clean-up. Under optimized conditions, average recoveries of individual sulfonamides were between 76.2 and 91.5% at three different spiked levels, the matrix-matched calibration curves were prepared at six concentration levels and a good linear relationship (R-2 > 0.990) was observed. The mean values of relative standard deviation of intra-and inter-day precision ranging from 1.8 to 5.7% and from 2.9 to 7.6% were obtained, respectively. The proposed method has been successfully applied to the analysis of sulfonamides in grass carp fish samples, indicating the potential of graphene as a SPE sorbent for the enrichment of trace residues in food matrices.