Abstract: Total acid content (TAC) and soluble salt-free solids content (SSFSC) in Chinese vinegar are 2 important indicators in the assessment of its quality. This paper shows the feasibility to determine TAC and SSFSC in Chinese vinegar by near-infrared (NIR) spectroscopy. Synergy interval partial least square (Si-PLS) algorithm was performed to calibrate the regression model. The number of PLS factors and the number of intervals were optimized simultaneously by cross-validation. The performance of the model was evaluated according to root mean square error of prediction (RMSEP) and correlation coefficient (R) in the prediction set. The optimum Si-PLS model for TAC was achieved with RMSEP= 0.264 g/100 mL and Rp= 0.9655; the optimum Si-PLS model for SSFSC was achieved with RMSEP= 1.93 g/100 mL and Rp= 0.9302. The overall results demonstrated that NIR spectroscopy combined with Si-PLS could be utilized to determinate TAC and SSFSC in Chinese vinegar, and NIR spectroscopy has a potential to be used in vinegar industry.