This work demonstrates that response surface methodology (RSM) is a powerful tool for the optimization of the production of distilled MG. Experiments with a centrifugal molecular distillator having an evaporation area of 0.0046 m(2) were carried out using RSM to identify operating conditions that can lead to higher MG purity. The independent variables studied were the evaporator temperature (TEV) and the volumetric feed flow rate (Q). The experimental range was from 100 to 300 degrees C for TEV and between 5 and 15 mL/min for Q. High-performance size exclusion chromatography was used to evaluate TG, DG, MG, FFA, and glycerol (GL) compositions. Results were presented as MG concentration surfaces. Starting from a material with 10.8% of TG, 37.7% of DG, 43.6% of MG, and 7.2% of GL, the maximum MG purity in the distillate stream with just one distillation step was 82.6% at a TEV equal to 250 degrees C and Q equal to 5 mL/min. At these conditions, the MG recovery was 61%. A strategy was developed to obtain distilled MG with 96.3% purity.829673678