HPLC-ICP-MS method was established to separate AsB, As(Ⅲ), monmethyl arsenic ( MMA ) , dimethyl arsenic ( DMA ) and As(V) in rat viscera. Ultrasonic water bath extraction was used for sample pretreatment. Dionex IonPac AS19 anion-exchange column and 20 mmol/L (NH4)2CO3(pH=9. 7) were used to analyze arsenic species in rat liver and kidney after realgar infected. The results showed that the method was not interfered by 40 Ar35 Cl+ peak, the linear ranges for five arsenic species were all between 1 and 300 μg/L with linear coefficients more than 0. 9990, and the detection limits were between 0. 3 and 0. 5 μg/L. The relative standard deviations ( RSDs) for the determination of five species were less than 5% and the recoveries were between 83. 8% and 111. 7%. After speciation analysis, DMA, As(Ⅲ) and unknown compound 2 were found in liver;DMA, MMA, As(Ⅲ), unknown compound 1, unknown compound 2 and unknown compound 3 were found in the kidney. The results indicated that this method could be used for arsenic species analysis of realgar metabolism.