Considering the negative impacts on human health and the environment, determinations of arsenic (As) and antimony (Sb), is of unquestionable importance. The present study describes the development of innovative and practical deep eutectic solvent (DES) based vortex assisted microextraction (DES-VAME) method for preconcentration of As and Sb from environmental waters, honey and rice prior to analysis by hydride generationatomic absorption spectrometry (HG-AAS). The use of As(III) and Sb(III) in presence of dithizone at pH 10.5 by means of donor-acceptor mechanism were decided as analyzes. Total As and Sb were determined after reduction process. The analytical properties obtained following optimization were as follows. Limit of detection (LOD), precision (as RSD%), recoveries and enhancement factor for As and Sb were calculated as 7.5 ng L-1/1. 5.6 ng L-1, 2.1% /2.7%, 93.5%/96.2% and 104/85, respectively. Following validation with certified reference material, the method was successfully applied to the analysis of real samples.