A novel polyamidoamine dendrimer functionalized with Fe3O4 nanoparticles (Fe3O4@PAMAM) had been fabricated and used as magnetic solid-phase extraction (MSPE) adsorbent. The Fe3O4@PAMAM nanocomposites were characterized by X-ray powder diffraction, Fourier transform infrared spectroscopy, field-emission scanning electron spectroscopy, elemental analytical, and thermal gravimetric analysis. The MSPE method coupled with high-performance liquid chromatography with an ultraviolet detection system was applied for the separation/analysis of non-steroidal anti-inflammatory drugs (NSAIDs). Major parameters affecting the extraction efficiency of the selected drugs were optimized. Under optimal conditions, the enrichment factors for the proposed method were 701single bond835. The linear range, limit of detection, correlation coefficient (r), and relative standard deviation (RSD) were found to be 0.15–500 ng mL−1, 0.05single bond0.08 ng mL−1, 0.9932single bond0.9967, and 4.5–7.0% (n = 5, 0.2, 10 and 300 ng mL−1), respectively. The method was successfully applied to the determination of NSAIDs in the real water samples. The recoveries of spiked water samples were in the range of 93.6–98.9% with RSDs varying from 6.1% to 9.0%, showing the good accuracy of the method.

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