Samples were dealt with microwave digestion. A method of determination of arsenic and mercury in foods by hydride generation-atomic fluorescence spectrometry was studied. The result showed that the detection limit of As and Hg were 0.42 μg/L and 0.06 μg/L, the recovery of As and Hg proved to be 95%-105% and 92%-103% respectively under optimum conditions, the RSD of analysis result was within 10%. The detect limitation, precision and accuracy could meet the demand of food test and it can be widely used for a...