Due to be able to migrate or leach from food packaging materials into the foods and/or beverages, development of a new, sensitive and selective analytical methods for low levels of antimony as a food contaminant is of great importance in terms of food safety. In this context, an ultrasonic-assisted cloud point extraction method was developed for the preconcentration and determination of antimony as Sb(III) using 4-(2-thiazolylazo)resorcinol (TAR) and 2-(2-thiazolylazo)-p-cresol (TAC) as chelating agents and sodium dodecyl sulfate as signal enhancing agent at pH 6.0 and mediated by nonionic surfactant, t-octylphenoxypolyethoxyethanol by flame atomic absorption spectrometry. Using the optimized conditions, the calibration curves obtained from Sb(III) with TAR and TAC were linear in the concentration ranges of 0.5-180 and 1-180 mu g L-1 with detection limits of 0.13 and 0.28 mu g L-1, respectively. The precision (as relative standard deviations, RSDs) was lower than 3.9 % (25 and 100 mu g L-1, n: 6). The method accuracy was validated by the analysis of two standard reference materials. The results obtained were statistically in a good agreement with the certified values at 95 % confidence limit. The method has successfully been applied to the determination of Sb(III) and total Sb in selected beverages, milk and fruit-flavored milk products before and after pre-reduction of Sb(V) to Sb(III) with a mixture of KI/ascorbic acid in acidic media. The Sb(V) contents of samples were quantitatively calculated from analytical difference between total Sb and Sb(III) levels.