Lambic beer is produced using spontaneous fermentation. Gueuze is a style of lambic beer that blends “young” (1 year old) and “aged” (2+ years old) beers. Little is known about the development of volatile aroma compounds in lambic beer during aging. Solid-phase microextraction and gas chromatography–mass spectrometry were used to analyze volatile compounds from 3, 6, 9, 12, and 28-month-old commercial samples of lambic beer. Compounds were identified using standardized retention time and mass spectra of standards. Gas chromatography–olfactometry was used to characterize the aroma profiles of the samples. A total of 41 compounds were identified using gas chromatography–mass spectrometry (GC–MS). Ethyl lactate, ethyl acetate, 4-ethylphenol and 4-ethylguaiacol were identified in the 9, 12, and 28-month old samples. These four compounds have been linked to the microorganism Brettanomyces. Twenty-one aroma active compounds were identified using Gas chromatography–olfactometry (GC–O). As the age of the gueuze samples increased, a larger number of aroma compounds were identified by the panelists; the compounds identified increased from seven for the 3-month-old samples to nine for the 6-month-old samples, and eleven for both the nine and twelve-month-old samples, and seventeen for the twenty-eight-month-old samples.