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Herein, a composite of polyacrylonitrile (PAN)/agar/silver nanoparticles (AgNPs) electrospun nanofibers was fabricated and applied as an efficient sorbent for thin-film micro-extraction (TFME) of five metal ions followed by inductively coupled plasma optical emission spectroscopy (ICP-OES). Incorporating agar into the nanofibers followed by in situ photo-reductive reaction under UV-lamp resulted in highly uniform dispersion of AgNPs in the nanofibers. Under the optimized conditions, agreeable linearity was acquired in the range of 0.5–250.0 ng mL⁻¹ (R² ≥ 0.9985). The LODs (based on S/N = 3) were attained in the range of 0.2 to 0.5 ng mL⁻¹. The relative standard deviations (RSDs) were between 4.5% and 5.6% (intra-day, n = 5) and 5.3%–5.9% (inter-day, n = 3) for three sequential days. The developed method was investigated with water and rice samples, and recoveries (93.9–98.0%) indicated that the PAN …