• Thirteen compounds were identified. • The major compounds were hexanal, 3-methyl-2-pentanone, phenylacetaldehyde, and E-nerolidol, and nine compounds had lower concentrations. • Literature data shows that these compounds from bryophytes or other organisms present toxic, repellent or attractive effects on insects. Bryophytes are natural sources of volatile organic compounds (VOCs) with bioactive properties whese can be used for bioprospecting and biotechnological applications. This study determines the VOC composition from the moss Calymperes palisotii Schwägr. The volatile concentrate of the species was obtained by simultaneous micro hydrodistillation-extraction (SDE), and analyzed by gas chromatography coupled to mass spectrometry (GC/MS). Among 13 compounds, hexanal, 3-methyl-2-pentanone, phenylacetaldehyde, and E-nerolidol were major compounds,. This was first record of the volatile chemical composition of C. palisotii, with some substances was unprecedented in moss species.