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Human exposure to microplastics (MPs) and nanoplastics (NPs) is increasing; however, some potential adverse health effects might remain unclear, due to analytical challenges in detecting trace concentrations. To address this, we propose a workflow for NPs assessment in biological samples combining three complimentary methods, namely inductively coupled plasma mass spectrometry (ICP-MS), X-ray fluorescence imaging (XFI), and imaging mass cytometry (IMC) to detect palladium-doped NPs (Pd-NPs). This approach was used to quantify the temporal distribution and accumulation of Pd-NPs in mouse models under different experimental conditions, dosages, and time frames. Acute exposure showed a clear particle excretion from the gastrointestinal tract into feces, while subchronic exposure led to tissue accumulation. 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