Abstract: The benefits promoted by natural products on human health have motivated industry to search for alternative separation systems in order to purify active compounds present in renewable sources. Amongst natural products of current interest for food, pharmaceutical, cosmetic, and chemical industries is methyl chavicol (MC). MC is a natural ingredient found in several herbs as tarragon, sweet basil, sweet fennel, and their essential oils, and its widest application is in food industry as flavoring agent. In this work, basil essential oil was used as raw material to study MC concentration through a hybrid evaporation system. The evaporative system was constituted of a cylindrical evaporator, an internal condenser located concentrically to the evaporator, and an external condenser. It generates 3 outside streams: distilled, side, and residue, which were recovered at the bottom of external condenser, internal condenser, and evaporator, respectively. From experimental results, it was verified that higher MC concentration was reached at the side stream because its intermediate volatility when compared with other substances present in basil essential oil. Central composite experimental design using 2 factors and 4 replicates at central point was considered in this work to determine the effect of operating conditions on methyl chavicol separation. Response variables were methyl chavicol concentration (%MCside) at side stream, distilled (%D) and side (%S) streams amounts. The factors studied in this work were: evaporator temperature (Tevap) and feed flow rate (FFR). Analyzing the variables effects, two variables presented a statistically significant effect on distilled percentage: evaporator temperature and feed flow rate. For the side stream, the variables: evaporator temperature, feed flow rate, and the interaction between evaporator stream and feed flow rate influenced the side amount and methyl chavicol concentration. [Copyright &y& Elsevier]