Abstract: Sample of Chinese yam was digested with HNO3 and H2O2, and the sample solution obtained was adjusted to pH 11-12 and 0.1 mol·L-1 LaCl3 solution was added for coprecipitation with As and Se. The precipitates were separated by centrifugation and dissolved in HCl (1+1) solution, which was used for HG-AFS determination. Under the optimum conditions, linear relationships between fluorescence intensity and mass concentration of As and Se were found in the same range within 40.0 μg·L-1, with detection limits (3σ) of 0.014 μg·L-1 and 0.022 μg·L-1, respectively. The proposed method was applied to the analysis of sample of Chinese yam, values of recovery found were 102% for As and 96.8% for Se.