Arsenic speciation was carried out in muscle tissues of freshwater fish species. Inorganic arsenic species (As3+and As5+) were extracted with chloroform, prior to microwave assisted digestion with concentrated HClO4 and Fe2(SO4)3. The extracted As3+ and As5+ were determined by electrothermal atomic absorption spectrometry (ETAAS). The accuracy of the technique was evaluated by using certified reference material DORM-2. The limit of detection of the method was 0.004 and 0.005 lg/g for As3+ and As5+, respectively. The mean relative standard deviation values (RSD) in real sample analysis were 1.90 and 3.92 for As3+ and As5+, respectively. The results demonstrated the suitability of the procedure for screening and quantification of As species in biological samples. The mean concentration of As3+ and As5+ in muscle tissues of studied fish species ranged from 1.19 to 2.05 and 0.17 to 0.46 lg/g, respectively. The contribution of the daily intake of inorganic As, based on the consumption of 250 g fresh fish muscles/body weight/ day was found in the range of 1.21–1.91 lg/kg/day.