Virgin coconut oil (VCO) can be prepared with or without the use of heat: (1) cold-process includes fermentation or centrifugation; and (2) heat-treated includes expelling. The volatile organic compounds (VOCs) from VCO samples prepared with and without the use of heat were collected using solid phase microextraction (SPME) and analyzed using gas chromatography – mass spectrometry (GC-MS). Twenty-seven VCO samples, from 9 VCO producers, were analyzed. The VOC profile of refined coconut oil (RCO) was also obtained for comparison. Thirteen compounds were identified in more than 80% of the VCO samples analyzed. These included: acetic acid; C6, C8, C10, C12, and C14 fatty acids and their corresponding δ-lactones; and C8 and C10 ethyl carboxylates. Minor volatiles occurring in less than half of the VCO samples included: other carboxylic acids, aldehydes, alcohols, and esters. The fermentation process produced more acetic acid. There were variations in the VOCs within each method as each producer used different processing times and temperature. Principal components analysis (PCA) grouped the samples according to the process used, but there were overlaps which may be due to variations in the specific procedures used by the different manufacturers. These results may help VCO manufacturers control their production processes.