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Introduction A major risk factor for chronic obstructive pulmonary disease (COPD) is tobacco smoke, which generates oxidative stress in airways, resulting in the production of volatile organic compounds (VOCs). The purpose of this study was to identify VOCs in exhaled breath and to determine their possible use as disease biomarkers. Method Exhaled breath from 100 healthy volunteers, divided into 3 groups (never smokers, former smokers and active smokers) and exhaled breath from 57 COPD patients were analyzed. Samples were collected using BioVOC ® devices and transferred to universal desorption tubes. Compounds were analyzed by thermal desorption, gas chromatography and mass spectrometry. VOCs analyzed were linear aldehydes and carboxylic acids. Results The COPD group and healthy controls (never smokers and former smokers) showed statistically significant differences in hexanal concentrations, and never smokers and the COPD group showed statistically significant differences in nonanal concentrations. Conclusions Hexanal discriminates between COPD patients and healthy non-smoking controls. Nonanal discriminates between smokers and former smokers (with and without COPD) and never smokers.