Abstract: A confirmative method was developed with liquid chromatography-atomic fluorescence spectrometry(LC-AFS)to detect mercury species in aquatic animals and their products,and the type of flow phase,velocity,pH,injection volume,the concentration of reducing agent and load current(HCl)were optimized. Three mercury species,inorganic mercury(Hg²⁺),methyl mercury(MeHg),ethyl mercury(EtHg)was completely separated in 14 minutes. Experimental results showed that,three species of mercury were in good linearity(r>0.9990),and relative standard deviations(RSD)were less than 5.0%. Adding the mixture standard solution to the different samples with the addition of 5 ng/mL,20 ng/mL,100 ng/mL,respectively,to conduct the standard recovery test,The recoveries of Hg²⁺,MeHg,EtHg were 80.1%~95.8%,92.1%~105%,80.3%~97.6%,respectively,and the detection limit was 0.017,0.112,0.142 mg/kg,respectively. The fish tissue standard substance BCR463 and ERM-CE464 were measured by using this method,and the measured value was consistent with the standard value,which further verifies the accuracy and reliability of this method. Moreover,this method has simple pretreatmentand high extraction efficiency,so it is applicable to the detection of mercury species in aquatic products.