Gas-Liquid Chromatography (GLC) methods such as AOAC Fat in foods 966.06 (2005), AOCS Official Methods Ce 1h-05 (2005), Ce 1j-07 (2007), allow for analyzing the fatty acids (FAs) in dietary fats using highly polar liquid phase capillary columns. However, there are still difficulties in completely separating butiric acid from solvent, FA critical pairs with similar polarity, conjugated linoleic acid (CLA) isomers, and long chain-polyunsaturated FAs (LC-PUFAs). Therefore, the selection of the temperature program to be employed is important. This work aimed to improve the AOCS Ce 1j-07 Method for the FA composition of a mixture of soybean and sunflower oil, fish oil, and butterfat, using a modified temperature program, tested among five laboratories. It takes more time, but it allows to completely separate butyric acid from the solvent, trans-18:1 from cis-18:1, 20:1 isomers from 18:3 n-3, 22:1 n-9 from 20:4 n-6, 20:5 n-3 from 24:0 and the main CLA isomers, thus permitting FA quantification in fats and oils for different purposes such as nutritional labeling, quality control and research.