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A method for determining low levels of As and Cd by dispersive liquid-liquid microextraction (DLLME) and inductively coupled plasma mass spectrometry (ICP-MS) was proposed. The following parameters that affect extraction efficiency were investigated: type and volume of extraction solvent (1000 µL acetone), type and volume of dispersive solvent (75 µL carbon tetrachloride), amount of ammonium pyrrolidinedithiocarbamate and sodium diethyldithiocarbamate as chelating agents, sample mass (0.5 g in 10 mL ultrapure water), pH of sample solution (2.0) and number of washing steps (one). Accuracy was evaluated by analytes determination in sugar samples by ICP-MS after digestion by microwave-induced combustion (MIC). No significant difference was observed between results of the proposed DLLME method and MIC in the case of both analytes. Instrument calibration was performed by the standard addition method and good linearity was achieved. Limits of quantification (LOQs) were 0.7 and 0.2 ng g -1 for As and Cd, respectively. The main advantages of this method are relatively high sample mass, low dilution, suitable preconcentration factors and significantly low LOQs (ng g -1 range). When the proposed method was used for determining As and Cd in four sugar samples, their concentrations ranged from 1.13 to 2.95 ng g -1 and from 0.31 to 0.43 ng g -1 , respectively.Keywords: dispersive liquid-liquid microextraction, sugar, arsenic, cadmium, inductively coupled plasma mass spectrometry IntroductionSugar has been widely consumed around the world by people of all ages, since it is an important ingredient found in several products, such as sweets, softdrinks and bread. 1,2 Similarly to other food, it is prone to contamination by toxic elements throughout its production and manufacturing processes.3 Some elements can be classified into essential or toxic, depending on the role they play in the metabolism of living organisms. Ca, Cu and Zn are essential for life whereas As, Cd and others do not have any known biological function and may be toxic, depending on their concentrations, thus posing potential risks to human health. [4][5][6][7] Arsenic may cause several health problems with mutagenic, carcinogenic and teratogenic effects. In humans, it can affect neurological, cardiovascular and respiratory systems, besides causing hypertension. [7][8][9] Cadmium is the most toxic element to humans, since it leads to renal failure, hypertension, emphysema and carcinogenic hazards, mainly in the kidney and prostate. 8,9 Therefore, As and Cd must be considered toxic even at low concentrations and must be monitored in the environment, food and beverages.Several techniques have been developed for simultaneous element determination at ultratrace levels in food samples. Inductively coupled plasma optical emission spectrometry (ICP-OES) 10 and inductively coupled plasma mass spectrometry (ICP-MS) 11 are the most successful examples. Regarding these techniques, the latter, which is the most sensitive, versatile and suitable one for routine applicati...