Molecularly Imprinted Poly(Trimethylolpropane Triacrylate‐Co‐Ethylene Glycol Dimethacrylate‐Co‐Methacrylic Acid) Monolithic Sorbent for Pipette‐Tip Solid‐Phase Extraction of N‐Nitrosodimethylamine in Medicaments

A novel pipette‐tip solid‐phase extraction method was developed using a molecularly imprinted monolithic sorbent composed of poly(trimethylolpropane triacrylate‐co‐ethylene glycol dimethacrylate‐co‐methacrylic acid) for the selective extraction of N ‐nitrosodimethylamine from pharmaceutical formulations. The sorbent was synthesized by in situ thermopolymerization within 1 mL pipette tips, resulting in a hierarchically porous monolithic structure with good permeability and specific recognition sites for N ‐nitrosodimethylamine. The structural and physicochemical characteristics of the sorbent were investigated by several techniques, confirming its macroporous nature, thermal stability, and efficient polymerization. Adsorption studies demonstrated a five‐fold increase in capacity for the imprinted material compared to its non‐imprinted counterpart. The extraction procedure was optimized for eluent type, extraction/elution cycle numbers, and sample volume and evaluated for greenness using the AGREEprep metric, achieving a score of 0.76. The proposed method was validated, demonstrating excellent linearity ( r > 0.997), recoveries between 95.6% and 98.5%, relative standard deviation < 4.1%, and a limit of quantification of 2 ng g −1 . The optimized and validated method was applied to commercial drug samples showing no detectable nitrosamine, while spiked samples yielded high recovery rates (92%–96%). This work presents a fast, eco‐friendly, and effortless alternative for determining N ‐nitrosodimethylamine in commercial drugs, with performance comparable to more advanced methods.