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The present study aimed to evaluate methylmercury in fish and human hair samples from an important hydroelectrical reservoir, Balbina (Brazil, Amazon). It presents a quite intense fishing activity and there is no known goldmining activity in its watershed. Fish and human hair were analyzed with a new extraction technique and measured by GC-ECD. Analytical quality was checked through intercomparisons between two laboratories with local samples and certified standards from IAEA. Methylmercury in hair ranged from 2.0 to 21.6 μg · g⁻¹with a mean of 8.76±5.20 μg · g⁻¹(N=20), while the methylmercury percentages were above 90. Fish presented methylmercury levels ranging from 0.03 to 0.9 μg · g⁻¹wet wt with a mean of 0.24±0.18 μg · g⁻¹wet wt (N=32), which is below the limit established for food by Brazilian legislation (0.5 μg · g⁻¹wet wt) and methylmercury mean percentages were above 95%. The total …