Abstract: A high performance liquid chromatography with fluorescence detection(HPLC-FLD) method was built for determination of residues of thiamphenicol(TAP) in chicken muscle. TAP was extracted with acetone and dichloromethane from chicken muscle. Extract solution was degreased with n-hexane and evaporated with nitrogen evaporator，the mobile phase was acetonitrile-sodium dihydrogen phosphate solution(0.01 mol/L，containing 0.005 mol/L SDS and 0.1% triethylamine)(32∶68)，the flow rate was 1.0 mL/min. The fluorescence detection was with an excitation wavelength of 225 nm and an emission wavelength of 290 nm. The data showed that the linear relationship of TAP was nice (r＝0.9991) in 0.01 mg/L to 1.75 mg/L concentration range. At spiked level 5 to 500 μg/kg for TAP，the average recovery ranged from 79.49% to 89.71%，relative standard deviation(RSD) ranged from 4.96% to 9.61%，the within-day RSD ranged from 5.68% to 7.47%，the between day RSD ranged from 8.89% to 11.32%. The lowest detection limit of TAP was 1.5 μg/kg(S/N＝3) and the lowest quantitative limit of TAP was 5 μg/kg (S/N＝10). This HPLC-FLD method is simple，rapid，high sensitivity and suitable for high sensitivity determination of TAP in chicken muscle.

Key words: high performance liquid chromatography（HPLC）; fluorescence detection; thiamphenicol（TAP）; chicken muscle; residues