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A simple and effective pretreatment method based on matrix solid-phase dispersion was developed for the determination of pharmaceutical and personal care products (PPCPs) and their metabolites in fish by high-performance liquid chromatography tandem mass spectrometry. The type and amount of dispersant, adsorbent, and eluting solvent were optimized by a single-factor experiment and Box−Behnken design. Under the optimal conditions with 2.5 g of Florisil as a dispersant, 500 mg of C 18 as an adsorbent, and 5 mL of acetonitrile as an eluting solvent, the recoveries ranged from 70.4 to 99.9% with relative standard deviations less than 10.5%, and the limits of quantitation ranged from 0.13 to 1.01 μg/kg. The developed method was successfully applied to detect PPCPs in marketed fish, and five PPCPs, including triclocarban, sulfadiazine, sulfadimidine, sulfamethoxazole, and carbamazepine, were detected at trace levels. The proposed method, which has the advantages of short analysis time, less solvent consumption, and high sensitivity, can be used for the determination of trace PPCPs in fish.

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