Bacterial cellulose-supported dual-layered nanofibrous adsorbent for thin-film micro-solid-phase extraction of antibiotics in municipal wastewaters.

In this study, bacterial cellulose was coated with composite nanofibers of polyvinyl alcohol doped with beta cyclodextrin and alginate (PVA-SA-βCD), constructed using the electrospinning technique. This novel material served as an effective adsorbent for thin-film micro-solid-phase extraction (TF-μSPE) of antibiotics from water samples, followed by HPLC-UV analysis. The adsorbent was subjected to a comprehensive characterization using ATR-FTIR, FE-SEM, and BET techniques. These analyses provided valuable insights into its physicochemical structure and properties. Several key parameters that affect the performance of the TF-μSPE method were investigated including electrospinning factors (voltage, flow rate, needle tip-collector distance, and electrospinning time), desorption solvent type and volume, adsorbent dose, adsorption and desorption times, pH value, and salt percentage. Under the optimized conditions, the limits of detections and quantifications for target antibiotics were obtained in the ranges of 0.02-0.03 and 0.07-0.1 μg L⁻, respectively. The linear range was 0.07-1000 μg L⁻ with satisfactory determination coefficients (r) of 0.9944-0.9984. The intra-day and inter-day precisions were obtained as 1.1-1.7 % and 2.2-3.5 %, respectively. The developed method was successfully applied to determine antibiotics in municipal wastewater samples, yielding recoveries within the range of 70-100 % (RSD%<3.7). The green features of the method were also assessed based on AGREE tool. This is the first report on the fabrication of a double-layered nanofibrous adsorbent and its application for the adsorption of antibiotics in wastewater. This robust approach combines efficiency with analytical accuracy, making it a valuable tool for antibiotic analysis in environmental samples.