## 2 Materials and Methods
### Gas Chromatography-Olfactometry Study
#### 2.2.2 GC-O and GC-MS Analysis  
The concentrated extract (1 \(\mu\)L) obtained for SPE was used for GC-O analysis. The analyses were carried out using an Agilent HP 5890 Series II Plus gas chromatograph (Santa Clara, CA, USA) equipped with a flame ionization detector (FID) and a sniffing port. The column used was a DB-WAX (30 m \(\times\) 0.25 mm L.D., 0.5 \(\mu\)m film thickness; J&W Scientific, Folsom, CA, USA). The chromatograph had a standard split/spitless injector, and an SPME liner with a 0.75 mm internal diameter was used. The injection mode used was pulsed-spitless at a temperature of 250 \({}^{\circ}\)C with a pressure pulse of 62 kPa for 3 min. The carrier gas was H\({}_{2}\) at a rate of 1 mL/min and a pressure of 45 kPa. At the output of the chromatographic column, the flow was divided into equal parts between the olfactory detector and the FID. Injector and detector were both kept at 250 \({}^{\circ}\)C. The oven temperature was held initially at 40 \({}^{\circ}\)C for 3 min, then increased by 5 \({}^{\circ}\)C/min to 220 \({}^{\circ}\)C, and finally kept for 59 min.  
A panel of five expert judges (two women and three men, with ages ranging from 20 to 37) from the laboratory staff with extensive experience in GC-O analysis was used in this study. Snorting time was approximately 15 min per judge, randomly distributed during the section, per replicate. Panelists were asked to score the intensity of each odor stimulus using a 4-point scale (0 = not detected, 1 = weak, 2 = light but not intense note, 3 = intense note) [21]. Afterward, the modified frequency (MF) was calculated [22] with Equation (1).  
\[MF(\%)=[F\cdot I]^{\frac{1}{2}} \tag{1}\]  
where \(F\) is the detection frequency of an aromatic attribute, expressed as a percentage of the total number of judges, and \(I\) is the average intensity, expressed as a percentage of the maximum intensity. Only those odorants that reached an \(MF\) higher than 15% in at least one of the samples are included in the present work.  
The gas chromatograph mass spectrometry analyses were carried out in an Agilent 6890 gas chromatograph (Santa Clara, CA, USA) simultaneously coupled to an odoriferous door (Gerstel ODP, Linthicum, MD, USA) 2 and a 5973 Network mass spectrometry detector with a quadruple analyzer. The chromatograph had a standard split/spitless injector  
Figure 1: Percentage of compounds by chemical classification identified in “Cerrado” cashew (**A**) and cagaita (**B**) pulps obtained using headspace solid-phase extraction (HS-SPE) and headspace solid-phase microextraction (HS-SPME) with gas chromatography-olfactometry (GC-O).  
(270 \({}^{\circ}\)C) with a pressure pulse of 62 kPa for 3 min. Helium was used (analytical grade 5.0) as the carrier gas at a constant flow of 1 mL/min during the entire analysis.  
The chromatograph was equipped with the HP INNOWax column (50 m \(\times\) 0.25 I.D., 0.25 \(\upmu\)m film thickness) (Agilent, Santa Clara, CA, USA). The oven temperature was held initially at 50 \({}^{\circ}\)C for 3 min and then increased to 160 \({}^{\circ}\)C by 4 \({}^{\circ}\)C/min. It was later increased to 250 \({}^{\circ}\)C by 25 \({}^{\circ}\)C/min and finally kept for 22 min at 250 \({}^{\circ}\)C.  
An alkane solution (C\({}_{8}\)-C\({}_{28}\)) (Sigma-Aldrich Corp., St. Louis, MO, USA), 10 mg/L in dichloromethane, was used to calculate the linear retention indices (LRI) for each analyte. The odorants were identified by a comparison of their odor and chromatographic retention index (LRI) on the DB-WAX column and MS spectra with those of pure chemical standards. The Spectral Works AnalyzerPro software, equipped with NIST 2.0 MS library (NIST, Gaithersburg, MD, USA), was utilized in the identification.