We evaluated the volatile organic compounds (VOCs) present in human odor by using headspace solid phase microextraction gas chromatography-mass spectrometry for the extraction, separation, and analysis of the collected samples. Volatile organic compounds present in the headspace above axillary sweat samples collected from different individuals showed the presence of various types of compounds including organic fatty acids, ketones, aldehydes, esters, and alcohols. Qualitative differences and similarities noted between the males and females studied along with differences in chemical ratio patterns among the common compounds demonstrated the ability to differentiate between individuals through the examination of VOCs.