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The feasibility of applying synchronous fluorescence technology was studied to quickly detect the residues of sarafloxacin hydrochloride (SARH) and doxycycline hydrochloride (DCH) in chicken. Firstly, the three-dimensional synchronous fluorescence spectra of SARH standard solution, DCH standard solution, chicken extract without antibiotics and chicken extract containing SARH and DCH were analyzed, and the wavelength difference Δλ of both SARH and DCH were determined as 110nm, and the fluorescence excitation peaks of SARH and DCH were respectively determined as 320nm and 381nm for the detection of SARH and DCH residues in chicken. Secondly, the effects of the concentrations of magnesium sulfate solution and SDS solution, as well as time, on the fluorescence intensities through the single factor test were analyzed. The best detection conditions of SARH and DCH residues in chicken were as follows: the concentration of magnesium sulfate solution of 0.375mol/L, the concentration of SDS solution of 0.300 mol/L and time of 12min. Thirdly, the prediction models of SARH and DCH residues in chicken were established through the algorithms of multiple linear regression (MLR), partial least squares regression (PLSR), and support vector regression (SVR), respectively. The experimental results showed that the comprehensive evaluation of the prediction model based on the PLSR algorithm was the best among these algorithms. For the prediction model of SARH residues based on the PLSR algorithm, the R2P, RMSEP, and RPD were 0.8465, 0.3441mg/kg, and 2.5882, respectively. For the prediction model of DCH prediction based on the PLSR algorithm, the R2P, RMSEP, and RPD were 0.9141, 5.8909mg/kg, and 3.2435, respectively. The results showed that the detection of SARH and DCH residues in chicken was feasible through synchronous fluorescence technique, the implemented method was straightforward and fast, and could provide a reference for the rapid detection of SARH and DCH residues in chicken.