From the leaves of aloe, a succulent plant, a dried exudate commonly called aloe can be obtained, which is used as a natural drug for its cathartic effect and is widely employed as a bittering agent in alcoholic beverages. This investigation provides a tentative characterization of several commercial aloe exudates carried out both by reversed phase HPLC and by headspace GC-MS analysis. By means of HPLC the derivatives were evaluated, and by GC-MS the volatile fraction was investigated. Qualitative and quantitative differences among the constituents in various samples of different origins were found. In particular, these were evident in the HPLC profile of Kenya aloe and an Aloe barbadensis sample, which exuded a high content of isoaloeresin D and aloins, whereas GC-MS analysis showed the presence of anisole exclusively in Kenya aloe samples. Moreover, the results obtained by means of the latter technique suggested a reason for the prevailing use of Mosselbay and Port Elizabeth aloes in bitter spirits formulation.