Yerba mate ( Ilex paraguariensis ) traditionally grown in South America. Its extract contains bioactive compounds which are associated with pharmacological activities. Freeze-concentration (cryoconcentration) process allows the removal of water preserving the bioactive compounds in extracts. Furthermore, yerba mate extract incorporation into starches is promising for food and pharmaceutical uses. This process can be evaluated using simultaneous Thermogravimetry and differential thermal analysis (TG–DTA). The aim of this study was to obtain corn starch incorporated with freeze-concentrated yerba mate extract. The evaluation of freeze-concentration was carried by extracts analyses of density, total dry matter and ash. The evaluation of yerba mate extract incorporation into corn starch was performed using simultaneous TG–DTA system. Density results revealed extracts different composition and dry matter indicated that compounds were concentrated at 0.576% ratio after freeze-concentration stage. Nevertheless, incorporated starches showed exothermic peaks in DTA curves at temperatures between 287 and 514 °C, which increased in intensity in agreement with freeze-concentration stages advance. Thus, yerba mate oxygenated compounds were incorporated into starches. Nutraceutical products can be obtained using the incorporation of yerba mate extract into starches; however, further studies are necessary to extend these applications.