An HS-SPME method was developed and applied for the isolation of volatile organic compounds from plants native or acclimatized to Brazil. Method optimization was performed using typical analytes from the target samples; fibers coated with 100 mum PDMS and 75 mum Carboxen/PDMS were tested. Using PIDMS 100 pm fibers and GC-MS for separation and identification, up to 99.9% of the peak area in the chromatograms from plants were identified. The method was also applied to quantify the major volatile components of one of the samples (Aloysia gratissima) with results comparable to those from the conventional steam distillation method.5741795351356