Adulteration has gained much concern in the oils and fats industry due to health and religious issues. This study assesses the effect of heating on the profiling of lard (15% and 30% lard) spiked in refined bleached deodorized (RBD) palm oil at 120 oC, 180 oC and 240 oC for 1, 2 and 3 hours. The volatile compounds released were identified using (gas chromatography mass spectrometry headspace) GC-MS-HS method. Multivariate data from GC-MS-HS were mean centred prior to Principal Components Analysis (PCA) using Unscrambler software. The result obtained from the scores plot for 30% lard and 15% lard in the RBD palm oil showed the same pattern for heating temperature at 120 oC and 180 oC. At 240 oC, both sample and control were scattered in the scores plot. However, the GC-MS-HS technique did not differentiate between 0% lard with 15% or 30% lard in RBD palm oil.