Electrospun Graphene Oxide–Doped Nanofiber-Based Solid Phase Extraction Followed by High-Performance Liquid Chromatography for the Determination of Tetracycline Antibiotic Residues in Food Samples

In this study, electrospun graphene oxide–doped poly(acrylonitrile- co -maleic acid) nanofibers (E-spun-GO-PANCMA-NFs) were fabricated and investigated as novel adsorbent for solid phase extraction (SPE) of tetracycline antibiotics (TCs) in chicken samples. The as-synthesized E-spun-GO/PANCMA-NFs were characterized and then used as SPE adsorbent to combine with high-performance liquid chromatography-fluorescence detection (HPLC-FLD) for simultaneous determination of four TCs (tetracycline, oxytetracycline, chlorotetracycline, and doxycycline). The experimental parameters affecting the analytical performance of this method, including sample pH, ionic strength, solvent type, volume and time desorption, and sample volume, were optimized. Under the optimized conditions, the proposed method provided good linearity from 5 to 500 ng/mL, with correlation coefficients higher than 0.9990, limits of detection from 20.4 to 44.8 μg/kg, and limits of quantification from 69.7 to 115.5 μg/kg. The intra- and inter-day RSDs were less than 5%. The recoveries of TCs spiked in chicken muscle samples were from 84.7 to 106.3% with RSDs in the range of 0.4–4.5%. Finally, the proposed E-spun-GO/PANCMA-NF-based SPE-HPLC-FLD method has been successfully applied to the analysis of TCs in chicken tissue samples, and thus offered a great prospect for TC analysis mainly in the applications of food quality and safety protection.