Abstract: HG-AFS was applied to the determination of total amount of arsenic in seafood. Sample was digested with mixed acid of HNO3-HClO4(4+1), and prereduced with mixed solution of thiourea and ascorbic acid. Hydride of As(Ⅲ) were generated from HCl(5+95) solution using solution of 10 g·L-1 KBH4 dissolved 5 g·L-1 KOH solution as reducing reagent. Flow-rates of 400 mL·min-1 for the carrier gas and 800 mL·min-1 for the shielding gas were taken in analysis. Linear relationship between the fluorescence intensity and mass concentration of As was found in the range within 20 μg·L-1, with detection limit (3s/k)of 0.015 μg·L-1. Using 3 samples of seafood as matrixes, tests for recovery and precision were made by standard addition method, values of recovery and RSD′s (n=6)found were in the range of 98.5%-101.0% and 3.4%-4.2% respectively.