The application of syringe to syringe dispersive liquid phase microextraction-solidified floating organic drop was extended for the separation and preconcentration of trace amounts of cadmium ions from water and cereal samples. The extracted cadmium was quantified by electrothermal atomic absorption spectrometry. Factors affecting the complex formation as well as microextraction efficiency such as the concentration of dithizone as the chelating agent, sample pH, type and volume of the extractant, number of injections, ionic strength and sample volume were optimized. Under optimized conditions, the calibration curve was linear in the range of 1.0-14.0 ng L-1 with the coefficient of determination of 0.9994. The limit of detection and quantification were found to be 0.25 and 0.85 ng L-1, respectively. The inter-day and intra-day precision at two concentration levels (3.0 and 10.0 ng L-1) were in the range of 3.9-9.2%. The accuracy of the developed method was evaluated through recovery experiments and the analysis of certified reference material (SLRS-6).