Comprehensive two-dimensional gas chromatography utilising a semi-rotating cryogenic modulator was applied to the analysis of dietary milk derived fatty acids. Four column combinations were tested: two polar-nonpolar and two different nonpolarpolar column combinations. Best results were obtained with a nonpolar-polar column set, with narrow-bore (50 microm ID) Carbowax column as the second column. The GC x GC method clearly improved the separation efficiency of the fatty acids in comparison with one-dimensional GC analysis and proved to be suitable for the quantification of the analytes. The relative standard deviations (RSD) of the retention times in the first and second dimensions were on average 0.06% and 4.9%, respectively. The relative RSD for peak volumes was on average 2.9%.