Aging has become common practice among producers seeking to increase the value of their products. The objective of this work was to conduct periodic monitoring by solid‐phase microextraction–gas chromatography–mass spectrometry of the physical and chemical quality of aging cachaça in terms of the alcohol content, volatile acidity, esters, aldehydes, higher alcohols, furfural, methanol, dry extract, copper and volatile compounds in the production process (distilled fractions) and during storage in casks newly made from oak (Quercus sp.), amburana (Amburana cearensis), jatoba (Hymenaeae carbouril), balsam (Myroxylon peruiferum) and peroba (Paratecoma peroba). The barrels were made in a specialized cooperage, and cachaça was obtained from a production unit in the southern region of Minas Gerais. Distinct physicochemical values were obtained for the distilled fractions; head and tail fractions had inappropriate concentrations of alcohol, aldehydes and butan‐1‐ol. Values within the limits established by law were obtained for the heart fraction, both in the distillation process and during aging, and it is, therefore, suitable for consumption. Several important compounds responsible for the aroma and flavour of the cachaças were observed, and alcohols, acids, esters and sesquiterpenes were found to compose the main groups. Through variance and main component analysis, important chemical changes were observed in the beverages. Copyright © 2016 The Institute of Brewing & Distilling

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