Comparison of Gas Chromatography–Mass Spectrometry and Headspace-Solid phase Microextraction Methods for the Qualitative and Semi-Quantitative Determination of Aroma Compounds in Fruit-Based Spirits (Rakija) from Serbia

The qualitative and semi-quantitative composition of aroma compounds in plum-, pear-, and quince-based spirits from Serbia was determined and mutually compared by liquid-liquid extraction and solid-phase microextraction ( HS-SPME ) coupled with GC/MS analysis. Based on economic considerations, HS-SPME was suggested as the preferred method for the aroma analysis. The main volatile compounds in all three liquid-liquid extracts belonged to the group of alcohols (3-methyl-1-butanol and 2-methyl-1-butanol, as representatives) and esters (ethyl lactate, as the most abundant). 3-Methyl-1-butanol, 2-methyl-1-butanol, and ethyl lactate dominated in plum spirit; 3-methyl-1-butanol, 2-methyl-1-butanol, isobutanol, ethyl lactate, and ethyl-( E , Z )-2,4-decadienoate—in pear spirit; and 3-methyl-1-butanol, isobutanol, ethyl lactate, and ( E , E )-α-farnesene—in quince spirit. The main volatile compounds in all three HS-SPME extracts belonged to alcohols, esters, and terpenes. 3-Methyl-1-butanol, ethyl decanoate, and ethyl octanoate dominated in plum spirit; ( E , E )-α-farnesene, 3-methyl-1-butanol, ethyl decanoate, and ethyl-( E , Z )-2,4-decadienoate—in pear spirit; and ( E , E )-α-farnesene, 3-methyl-1-butanol, ethyl decanoate, and ethyl octanoate—in quince spirit.