Bioactive compounds of natural matrices are of interest because of their application in the food and pharmaceutical industries. One important source of bioactives is propolis, a resinous biomass that bees make from the plants surrounding the hive. Regarding Colombian propolis, studies have mostly been directed towards identifying flavonoids and their biological activity in vitro. There are no works on the oil extract of propolis and its chemical composition and bioactivity through metabolomic analysis. In this sense, this work studied the volatile composition of propolis oil extract samples from Colombia, following a metabolomic approach; in this work, the oily Colombian propolis extracts (OECP) obtained by an ultrasound assisted extraction (UAE) with different solvents were studied using spectroscopy and physicochemical analysis. A strong correlation was observed between the antioxidant activity and their concentrations of polyphenols, terpenoids, and carotenoids. Simultaneously, it was possible to expand the number of compounds identified by applying FTIR spectroscopy to the sample analysis, relating infrared bands to specific compounds. Besides, it was also possible to discriminate the samples according to their geographical origin. Colombian propolis oil extracts have characteristics as bioactive compounds such as the sesquiterpenes bisabolol, α-zingiberene, β-bisabolene, and α-trans-bergamotene and the monoterpenes α-pinene, linalool, and p-cymene.