A simple direct labeling method was used to synthesize the iodinated ultrafine polystyrene particles. The assay of X-ray photoelectron spectroscopy (XPS) as well as Fourier-transform infrared (FT-IR) spectroscopy indicated the formation of stable covalent bond to aryl group of the polymer particles. The purified radioiodinated product was incubated with serum of rat, and then evaluated by in vitro stability test. The result showed that these synthesized ultrafine polystyrene particles were unmetabolized at 2 hours post-exposure, indicating the potential useful application of this labeled polymer particles as a promising probe in biomedical sciences.