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Sourdough is an old example of a natural starter composed of a mixture of flour, water, and metabolites and is produced by naturally occurring lactic acid bacteria and yeasts that influence bread aroma. In this work, four types of sourdough were used to prepare bread: one sourdough with yeast beer and three with bacteria and yeasts. The physicochemical parameters (pH, moisture, water activity, and organic acids) of the bread and sourdoughs were assessed. Lactic, acetic, and succinic acids were found in considerable amounts in sourdoughs and the corresponding breads. The fermentation quotient (molar ratio between lactic and acetic acid) ranged from 0.39 to 3.4 in sourdoughs. Lactic acid was prevalent in all types of bread and showed the highest value in bread made from sourdough with a 1.5 bacteria/yeast ratio (8722.24 mg/kg). Moreover, volatile organic compounds were identified in bread samples. Alcohols, aldehydes, and acetic acid were mainly found. The alcohol concentration ranged from 140.88 to 401.20 ng/g. Aldehydes ranged from 185.01 to 454.95 ng/g, and acetic acid ranged from 91.40 to 173.81 ng/g. Bread prepared from sourdough with a 1.5 bacteria/yeast ratio showed a considerable amount of alcohols and acetic acid.