In this study, a novel electrospun nanofiber adsorbent based on polyacrylonitrile (PAN)/Cu (0.6) @MIL-100 (Fe) was developed and applied for ultrasonic-assisted thin film microextraction (UA-TFME) of nitrosamines (N-nitrosodimethylamine (NDMA), and N-nitrosodiethylamine (NDEA)) in pharmaceutical samples, followed by determination using gas chromatography–mass spectrometry (GC–MS). The method was optimized by evaluating critical factors such as extraction time, desorption solvent, pH, and ultrasonic power, leading to enhanced extraction efficiency. Under optimized conditions, low limits of detection (S/N = 3) were achieved at 0.03 μg kg−1 for NDMA and 0.04 μg kg−1 for NDEA, with excellent linearity (0.1–50 μg L−1, r2 > 0.998). Precision studies revealed satisfactory intra-day and inter-day repeatability with RSD values between 1.3 and 6.1 %. The applicability of the developed method was demonstrated by analyzing several widely used pharmaceutical products, including ranitidine, metformin, losartan, omeprazole, valsartan, paracetamol, amlodipine, ibuprofen, nifedipine, and cimetidine. The method achieved recoveries ranging from 93.8 % to 98.5 %, confirming its reliability for trace analysis of nitrosamines in complex pharmaceutical matrices. These findings demonstrate that PAN/Cu (0.6) @MIL-100(Fe) nanofibers represent a promising sorbent for sensitive and selective monitoring of nitrosamines contaminants in pharmaceuticals.
