Volatile compounds present on fruits and leaves of Mangifera indica var. coquinho were investigated by headspace solid phase microextraction (HS-SPME) and hydrodistillation (HD). Conventional techniques, such as hydrodistillation, may impart chemical changes to the original oil composition being also time-consuming. On the other hand, HS-SPME provides solvent-less extractions, shorter extraction times and may supply complementary information about the composition of the compounds. The HS-SPME technique was previously evaluated by the comparative study among the fibres: commercial PDMS, NiTi-ZrO(2) and NiTi-ZrO(2)-PDMS. The fibre NiTi-ZrO(2)-PDMS showed better sensitivity and precision and was used on the extraction of components. The influence of several parameters like the time and temperature of extraction and desorption time were examined to obtain better efficiency. Fruits and leaves were analysed in mature and immature stages. The profiles corresponding to the volatile compounds detected by both techniques are discussed.