During the deep fat food frying process, the frying media, oil, continuously degenerates when exposed to high temperature, oxygen and moisture. This leads to physical and chemical changes including the formation of hydrolysis products such as Free Fatty Acids (FFAs) which are associated with undesirable darkening in colour, off-flavouring and a lowering of the smoke point. This study was aiming to develop a method capable of identifying and quantifying individual free fatty acids within oil using a small sample size (100mg of oil). We used liquid/liquid extraction (LLE) technique to separate FFAs from the rest of the oil followed by esterification using boron trifluoride (BF3) and then gas chromatography (GC) analysis. Various extraction conditions were tested. A mixture of 0.02M phosphate buffer at pH 12 and acetonitrile at buffer: solvent ratio larger than 2:1 showed the highest efficiency in extraction of FFAs. The method was capable of producing accurate fatty acid profiles of FFAs and showed good precision on medium rancidity oil samples. It also captured the differences induced by adding free fatty acids to samples. An interesting discrepancy was found between the new method and the traditional titration method in terms of overall FFA content, which suggests further optimisation and investigation are required.