In this work, a novel method was developed for the speciation of inorganic antimony by solidified floating organic drop microextraction (SFODME) and electrothermal vaporization inductively coupled plasma mass spectrometry (ETV-ICP-MS). Ammonium pyrroinedithiocarbamate (APDC) was used as both a chelating reagent in SFODME and a chemical modifier in ETV. Sb(III) could react with APDC to form complexes at pH 6.0, and the complexes were quantitatively extracted into the organic phase of 1-dodecanol, whereas Sb(V) remained as free species in the aqueous phase. Sb(III) was directly determined by ETV...