## 2 Materials and Methods
### NMR Analysis  
Sample extraction for NMR analysis was carried out by modifying a previously described protocol [19]. In detail, 100 mg of the sample was added to 3 mL of a CH\({}_{3}\)OH/CHCl\({}_{3}\) 2:1 \(v/v\) mixture and 0.8 mL of bidistilled water. The obtained system was sonicated at room temperature for 10 min, followed by the addition of 1 mL of chloroform and 1 mL of bidistilled water. The hydroalcoholic phase was finally separated after centrifugation for 15 min (25 \({}^{\circ}\)C, 7200 \(\times\)\(g\)) and dried with a soft N\({}_{2}\) flux. The entire procedure was repeated two more times on the sample residue, guaranteeing a quantitative metabolite extraction.  
The dried hydroalcoholic phase was dissolved in 700 \(\upmu\)L of 200 mM phosphate buffer/D\({}_{2}\)O containing 0.4 mM TSP (3-(trimethylsilyl))propionic acid sodium salt) as the internal standard for metabolite quantification. NMR analyses were carried out on a Jeol JNM-ECZ 600R (JEOL Ltd., Tokyo, Japan) operating at a proton frequency of 600.17 MHz and equipped with a Jeol 5 mm FG/RO DIGITAL AUTOTUNE probe. \({}^{1}\)H NMR experiments were carried out using the following parameters: 298 K, 128 scans, residual water signal suppression with a presaturation pulse, 7.7 s relaxation delay, 90\({}^{\circ}\) pulse of 8.3 \(\upmu\)s, 64 K data points, and 9000 Hz spectral width. \({}^{1}\)H spectra were referenced to methyl group signals of TSP (\(\mathrm{\delta_{H}}\) = 0.00 ppm) in D\({}_{2}\)O. A homonuclear \({}^{1}\)H-\({}^{1}\)H TOCSY experiment was carried out with 52 scans, 8 K data points in \(f_{2}\) and 128 in \(f_{1}\), 50 ms mixing time, 2 s relaxation delay, and 9000 Hz spectral width in both dimensions. A heteronuclear \({}^{1}\)H-\({}^{13}\)C HSQC experiment was carried out with 76 scans, 8 K data points in \(f_{2}\) and 256 in \(f_{1}\), 3 s relaxation delay, and a spectral width of 9000 Hz and 33,000 Hz for \(f_{2}\) and \(f_{1}\), respectively. A heteronuclear \({}^{1}\)H-\({}^{13}\)C HMBC experiment was carried out with 64 scans, 8 K data points in \(f_{2}\) and 165 in \(f_{1}\), 2 s relaxation delay, and a spectral width of 9000 Hz and 37,500 Hz for \(f_{2}\) and \(f_{1}\), respectively. Spectrum processing and signal integration were carried out with JEOL Delta software (v5.3.1). For metabolite quantification, the integrals of the corresponding selected resonances in the \({}^{1}\)H-NMR spectra were measured with respect to TSP. Three replicates were made for each batch, and the results are expressed as mg/100 g of sample \(\pm\) SD by applying the following equations:  
\[\mathrm{C_{X}}=(\mathrm{I_{X}}/\mathrm{I_{TSP}})*(\mathrm{N_{TSP}}/\mathrm{N_ {X}})*\mathrm{C_{TSP}} \tag{1}\]  
\[\mathrm{P_{X}}=\mathrm{C_{X}}*\mathrm{V}*\mathrm{MW_{X}} \tag{2}\]  
where \(\mathrm{C_{X}}\) is the mM concentration of the quantified metabolite, \(\mathrm{I_{X}}\) is the area of the metabolite integrated signal, \(\mathrm{I_{TSP}}\) is the area of the internal standard \(\mathrm{T_{SP}}\) signal, \(\mathrm{N_{TSP}}\) is the proton number corresponding to the internal standard \(\mathrm{T_{SP}}\) signal, \(\mathrm{N_{X}}\) is the proton number corresponding to the metabolite signal, \(\mathrm{C_{TSP}}\) is the mM concentration of the internal standard TSP, \(\mathrm{P_{X}}\) is the mg amount of the metabolite in 100 mg of the sample, V is the volume of deuterated solvent used to solubilize the dried extract, and \(\mathrm{MW_{X}}\) is the molecular weight of the selected metabolite.