In this study, the distillation fractions of cider brandy produced illegally in Lithuania using gas chromatographic-mass spectrometry method were investigated. The conditions of gas chromatography-mass spectrometry were firstly optimized. A qualitative analysis of three distillation fractions was performed and estimated. The first fraction (initial) of distillation products was collected for 0.5 h, the second one (intermediate) was collected for the next 1.5 h and the third (main) fraction for the next 5 h. A method of the quantitative analysis of different volatile analytes such as acetaldehyde, methanol, ethanol, 1-propanol, isobutanol, 1-butanol, isoamyl alcohol and benzyl alcohol in the distillation products was also developed. The concentration of ethanol decreased significantly in the main fraction in comparison with those of the initial and intermediate fractions. The concentration of 1-propanol, isobutanol, 1-butanol and isoamyl alcohol in the last fraction decreased drastically as well.