Abstract： Objective:To develop asolvent extraction-direct mercury analyzer method for determination of methylmercury in urine.Methods:After the urinehydrolyzesd by hydrobromic acid, methylmercury was extracted by tolueneand reverse-extracted from L-cysteine solution, it was then detectedbydirect mercuryanalyzer.Results:The linear range was 0.2-50.0 μg/L, and the related coefficient was 0.9999. The relative standard deviations ( RSD) within the group were 5.04%-6.64%, and the RSD between the group were 5.65%-8.11 %. The average recovery efficiencies were 85.4%-95.5%. The detection limitation was 0.0482 μg/L and the quantification concentrations was 0.1607 μg/L. Conclusion:The method, which has low detection limit, high sensitivity, easy to operate, is stability for the determination of methylmercury in urine.