This study describes the determination of trace levels of antimony(III) by UV-Vis spectrophotometer after preconcentration by the deep eutectic solvent/dithizone probe-based liquid-liquid microextraction method. Ditizone was used as a ligand to form the coordinated antimony complex before extraction in the preconcentration process. In the microextraction method developed in the study, deep eutectic solvent was used to dissolve the complexing agent; thus, the complexation was performed at the same time as the extraction of antimony complex by deep eutectic solvent. All variables likely to affect the ligand-antimony(III) complex, extraction efficiency, and spectroscopic measurement were optimized to lower the detection limit. Under the determined optimum conditions, the detection limit for Sb was calculated as 1.6 × 10-3mg/L. The detection limit obtained with the method is much lower than the value obtained in the Uv-Vis spectrophotometer with the traditional method. In this study, the percent relative standard deviation for the lowest concentration was calculated as 3.12% (n = 8). This value indicates that the analysis performed has high precision. The applicability of the method was determined by performing spiked recovery tests on tap water taken from different regions. Satisfactory recovery results were obtained between 91 and 105% at three different concentrations.