The aim of this work was to determine the heating effect on the thermo-degradation process of rapeseed oil (RO) by rapid fluorescence method. Reference measurements were carried out by chromatographic methods in order to compare results with those obtained by fluorescence spectroscopy. The main compounds which were monitored are polar compounds and tocopherols. During heating process, two temperatures were used: 171°C and 189°C for 4.5 h. The results have showed that the tocopherol content decreases, especially at the highest temperature, and the polar content increases of 20% at the end of heating. These results are in agreement with literature. PLS model was built in order to predict polar and tocopherol contents. The results obtained from this method were satisfactory.