Milk fat is an important food component, and plays a significant role in the economics, functional nutrition, and chemical properties of dairy products. Dairy products also contain nutritional resources and essential fatty acids (FAs). Because of the increasing demand for dairy products, milk fat is a common target in economic fraud. Specifically, milk fat is often replaced with cheaper or readily available vegetable oils or animal fats. In this study, a method for the discrimination of milk fat was developed, using FAs profiles, and triacylglycerols (TGs) profiles. A total of 11 samples were evaluated: four milk fats (MK), four vegetable oils (VG), two pork lards (PL), and one beef tallow (BT). Gas chromathgraphy analysis were performed, to monitor the FAs content and TGs composition in MK, VG, PL, and BT. The result showed that qualitative determination of the MK of samples adulterated with different vegetable oils and animal fats was possible by a visual comparision of FAs, using C14:0, C16:0, C18:1n9c, C18:0, and C18:2n6c, and of TGs, using C36, C38, C40, C50, C52, and C54 profiles. Overall, the objective of this study was to evaluate the potential of the use of FAs and TGs in the detection of adulterated milk fat, and accordingly characterize the samples by the adulterant oil source, and level of adulteration. Also, based on this preliminary investigation, the usefulness of this approach could be tested for other oils in the future.