The main objective of the present study was to determine the effect of the distillation technique: (i) fractional column distillation (FCD), (ii) copper alembic distillation (CAD), and (iii) home distillation (HD) on the aroma profile of the distilled spirit “tsipouro”. Volatile compounds were identified and semi-quantified in all above fractions for comparison purposes using Solid Phase Micro-extraction–Gas chromatography/Mass Spectrometry (SPME–GC/MS). Τhe richest (p < 0.05) distillate in volatile compounds was that of the FCD, with a total concentration of 768.38 mg/L followed by the HD (577.79 mg/L) and CAD (315.30 mg/L). The concentrations of the volatiles determined (alcohols, aldehydes, ketones, acetals, esters, organic acids, terpenes, hydrocarbons, and heterocyclic compounds) were found to be similar to those of other Greek and European distilled marc spirits. Ethanol and total volatile compound content were within limits set by Greek and EU legislation. Methanol, a toxic compound of grape marc distillates, was determined only in the entire product of CAD 1st distillation (19.35 mg/L) and the “head + tail” fraction of the CAD 2nd distillation (12.82 mg/L) in amounts well below the EU legal limit of 1000 g/hL of absolute alcohol. A general reducing trend was noted in most volatile compound concentration proceeding from the 1st to the 2nd CAD distillation refining the flavor of tsipouro.
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