Based on solidified floating organic drop microextraction (SFODME), a novel method was developed for the simultaneous speciation of inorganic arsenic (As(V)/As(III)) and antimony (Sb(V)/Sb(III)) by electrothermal vaporization inductively coupled plasma mass spectrometry (ETV-ICP-MS). Ammonium pyrroine-dithiocarbamate (APDC) was used as both a chelating reagent in SFODME and a chemical modifier in ETV. As(III)/Sb(III) could react with APDC to form complexes at pH 5.5, and the complexes were quantitatively extracted into organic phase of 1-dodeca...