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This work describes a new analytical method useful for monitoring the human exposure to the endocrine-disrupting plasticizer triphenyl phosphate (TPP) via nail polish use. The method allows trace determination of this parent compound and its main metabolite, namely diphenyl phosphate (DPP), in urine samples of nail polish users. The method is based on a novel microextraction technique termed stir bar sorptive-dispersive microextraction (SBSDME) using a magnetic composite made of CoFe₂O₄ magnetic nanoparticles embedded into a mixed-mode weak anion exchange polymer (Strata^™-X-AW), followed by liquid chromatography-tandem mass spectrometry (LC–MS/MS). The main parameters involved in the extraction procedure were evaluated and optimized. Under the optimized conditions, the method was successfully validated showing good linearity (at least up to 100 ng mL⁻¹) and enrichment factors …