## 2 Materials and Methods
### Identification of Volatile Compounds through GC-MS  
The analysis of volatile compounds was carried out by GC-MS, in two different conditions. (1) Initially the analysis was performed using a GC-MS equipment (QP 2010 Plus, Shimadzu, Kyoto, Japan) coupled with an autosampler AOC-5000 and a Teknokroma Sapiens 5 MS column (5%-Phenyl- 95% Dimethyl Polysiloxane column) 30 m \(\times\) 0.25 mm ID, film thickness 0.25 \(\upmu\)m and an AOC-5000 Shimadzu autosampler. Helium was used as a carrier gas, and after the splitless injection, runs were performed in a column flow at 2 mL/min, using a temperature gradient for the separation of sample components: column oven was initially maintained at 40 \({}^{\circ}\)C during 5 min, followed by a gradual increase of 5 \({}^{\circ}\)C/min until 170 \({}^{\circ}\)C and programmed to rise to 230 \({}^{\circ}\)C at the rate of 30 \({}^{\circ}\)C/min; at the end the temperature was kept for 4 min. (2) The volatile compounds of the samples were also analyzed through a GC-MS QP 2010, Shimadzu coupled to an autosampler AOC-5000 Plus, and a Teknokroma Sapiens Wax MS, 60 m, 0.25 mm (i.d.), 0.25 \(\upmu\)m column. Carrier flow was performed at 4 mL/min, with an injection mode in splitless and detector at 250 \({}^{\circ}\)C. The gradient temperature used was the same abovementioned. For both conditions, the ionization energy was 70 eV, a scan range of 29-300 \(m/z\), while the detector and ionization temperatures were at 250 \({}^{\circ}\)C. Each sample was weighted to a 20 mL-vial (around 5-6 mg of LEE, 60-70 mg of both ME and Macro). Then, the volatile compounds present in the headspace of each sample were extracted using solid phase microextraction (SPME). A fiber of DVB/CAR/PDMS from Supelco, 23 Ga, 50/30 \(\upmu\)m, gray fiber assembly was used. Samples were heated for 40 min at 40 \({}^{\circ}\)C and were injected at 250 \({}^{\circ}\)C.  
The data acquisition was made using Shimadzu software, GC-MS solution, version 2.10 when analyzed with 5-MS column, while a different version (4.50 SP1) was used for the analysis performed with a Wax column. The identification of the components was assigned through comparison of the peak detected in the chromatogram obtained by GC-MS analysis, according to experimental conditions, with installed spectra from the libraries (NIST 21, 27, 107, 147 and Wiley 229). Only volatile compounds whose spectra presented a similarity index higher than 80% were considered for the comparison of Kovats retention indices. This retention index is used to confirm the identity of each volatile compound. Briefly, an injection of an alkane standard solution C8-C20 was performed using the same chromatographic conditions overmentioned. According with the retention time of each alkane, the retention index of each volatile compound in the sample chromatogram was determined based on the equation used for the calculation of non-isothermal Kovats retention indices. The Cal RI were compared with retention index found in the literature (Lit RI), and when the difference between both RI was higher than 15 units, the compound was assigned as \"not identified\". Considering these criteria, Tables 1 and 2 present the volatile compounds that were identified.  
In order to evaluate the contribution of each peak, they were integrated and the relative percentage of the area was determined, considering the total area of all integrated peaks in the chromatogram.