A non-targeted screening through headspace/solid-phase microextraction coupled to gas chromatography with time-of-flight mass spectrometry (HS/SPME-GC-TOF-MS) of the ground cocoa pulp, cocoa beans, and chocolate-making samples was conducted, in triplicate, using a Trace 1300 gas chromatograph (Thermo Fisher Scientific) equipped with a Stabilwax-MS column (Restek), as described previously (Díaz-Muñoz et al., 2021 (link)). This metabolite fingerprinting technique served as a selection of VOCs to be quantified.
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