RESUMO
A novel extraction technique is proposed in which the Multiple Headspace Extraction (MHE) approach is used in conjunction with Headspace Sorptive Extraction (HSSE) and Gas Chromatography-Mass Spectrometry (GC-MS) detection. The extraction method was developed to determine volatile compounds in macroalgae. Optimization of the extraction parameters was carried out using design of experiments to identify factors that affect the extraction: extraction time, temperature, twister length and amount of sample. The results of the optimization led to an extraction of 2â¯g of sample using a 20â¯mm Twister® at 66⯰C for 180â¯min. The progression constants (ß) were calculated for 43 volatile compounds, 29 of which could be quantified using the method. Linearity was attained with a determination coefficient higher than 0.99 for all studied compounds. Inter-day and inter-twister precisions ranged from 0.22% to 19.01% and from 0.69% to 14.76% respectively, and values below 10% were obtained for the majority of compounds. LOD and LOQ values ranged from the values obtained for diethyl succinate (0.012⯵g/L and 0.088⯵g/L, respectively) and those obtained for dimethyl sulfide (5.544⯵g/L and 40.286⯵g/L, respectively). However, for the majority of compounds values obtained were below 1⯵g/L (LOD) and 5⯵g/L (LOQ). Compounds such as ethyl acetate, hexanal, heptadecane, 2-hexenal, 6-methyl-5-hepten-2-one, dimethyl sulfide, benzyl alcohol, beta ionone, or beta cyclocitral, among others were correctly determined in three species of macroalgae: Ulva sp., Gracillaria sp. and Enteromorpha sp.