Analytical dataset of Ecuadorian cocoa shells and beans.

Full analytical data of Ecuadorian cocoa wastes (raw shells) and beans (as benchmark), are herein reported. A detailed characterization of production residues may pave the road to a zero-waste strategy for the cocoa industry. Multiple analytical techniques have been exploited to define the composition of the matrices, among them: elemental analyses, FTIR, Py-GC/MS/FID and UHPLC-ESI-MS/MS. Quali-quantitative data of carbohydrates, lipids, lignin, polyphenols, alkaloids and proteins have been obtained by Py-GC/MS/FID and UHPLC-ESI-MS/MS. Assignations are fully supported by literature references. The FAMEs composition of lipophilic UAE extract is also reported for sake of comparison with cocoa butter. This data collection completes a wider valorization work, "Cocoa bean shell waste valorisation; extraction from lab to pilot-scale cavitational reactors" (Grillo et al., 2018).


Subject area
Chemistry More specific subject area Extraction and Valorization Type of data Tables and figures (chromatograms, spectra and instruments) How data was acquired

Data format
Raw, analysed and formatted.

Experimental factors
Analysed samples are composed by cocoa shells, raw or extracted by UAE. Cocoa beans were used as a benchmark.

Experimental features
Multiple analysis were performed for the sake of comparison between cocoa beans and residual biomass (shells) or its extract. Data source location All matrices originate from Ecuador. The Cocoa bean shells were kindly provided by Gobino S.r.l. (Turin, Italy).

Data accessibility
Data are reported in this article.

Value of the data
Full chemical characterization of raw waste material from cocoa industry (shells). Spectra and chromatograms can be used as fingerprints for quick matching. The comparison with cocoa beans composition shed light on the potential use and exploitability of the recovered fractions.
Reported data could pave the way to new valorization processes, providing a useful benchmark.

Data
A fingerprint of the matrices is obtained by FTIR spectra and elemental analysis. Carbohydrates composition was defined by alditol acetate protocol and by Py-GC/MS/FID. This technique was also used to quantify lipids, lignin, alkaloids, proteins and polyphenols by means of precursor identification. Definition of polyphenols was achieved by UHPLC-ESI-MS/MS analysis. Furthermore, FAMEs identification and quantification of shells lipophilic extract is reported. All data can be used for a full comparison with extracts reported by Grillo et al. [1].

Materials
Cocoa beans and shells from Ecuador were kindly provided by Gobino S.r.l. (Turin, Italy). Shells extracts are provided according the procedure reported by Grillo et al. (see Ref. [1], Paragraph 2.3.1 US-assisted extraction).

FTIR analysis
FTIR spectra of the cocoa beans and shells (raw material) samples were recorded in KBr pellets on a Spectrum One FTIR spectrometer (PerkinElmer) in the 4000-450 cm À 1 range (resolution 4 cm À 1 , number of scans 64). The resulting spectra ( Fig. 1) were normalised to the highest absorption intensity in each spectrum (in the ca. 3400 cm -1 range). Bands assignments are reported in Table 1, according to wave numbers.

Carbohydrate composition
Carbohydrate composition of cocoa beans and shells (raw material) was determined using an alditol acetate procedure by Blakeney, Harris, Henry and Stone, 1983 [2] after cocoa sample hydrolysis with 72% sulphuric acid. The alditol acetates were quantified by GC-FID (Agilent 6850 Series GC system) using a DB1701 column (60 m x 0.25 mm, film thickness 0.25 mm), and methyl α-D-glucopyranoside as the internal standard.

Pyrolyser(Py)-GC/MS/FID analysis
Py-GC/MS/FID analysis of cocoa beans and shells (raw material) were performed using a Frontier Lab Micro Double-shot Pyrolyser Py-3030D (pyrolysis temperature 500°C, heating rate 600°C/s) that was directly coupled to a Shimadzu 2D FID/MS gas chromatography system MS-GC/GC-MS-2010 with a RTX-1701 capillary column (Restek, 60 m x 0.25 mm x 0.25 μm film). The injector temperature was 250°C, the ion source 250°C (EI 70 eV), the MS scan range m/z was 15 to 350, the carrier gas was helium (flow rate 1 mL min -1 ) and the split ratio was 1:30. The amount of sample analysed was 1.00C2.00 mg. The oven temperature was kept at 60°C for 1 min, increased at 6°C/min to 270°C and finally held at 270°C for 10 min.
The identification of the individual compounds was performed using GC/MS chromatograms from the Library MS NIST 14, whereas the relative peak area of individual compounds was calculated using Shimadzu software on the basis of GC/FID data. The summed molar areas of the relevant peaks were normalised to 100% and the data for 5 repetitive pyrolysis experiments, at least, were averaged. Relative peak areas, calculated as percentages, for pyrolysis products of different origin were used to      (Table 3). Measurement error did not exceed 5% of the mean area value.
Peaks assignments has been performed by mass fragmentations (Table 4), available literature reference are shown. A composition comparison is possible, referring to UHPLC-ESI-MS/MS analysis of  Table 4 Polyphenols detected in the UHPLC-ESI-MS/MS analysis of the conventional extracts obtained from cocoa shells (Fig. 3).

GC analysis of fatty acid methyl esters (FAMEs)
The fatty acid composition of the lipophilic (hexane) phase derived from a ternary mixture extracts.
FAMEs identification was performed by checking correspondence with C8-C24 saturated and unsaturated external standards (Sigma-Aldrich), which were prepared in solution with GC grade cyclohexane, and with Wiley7n and NIST11 GC libraries (for GC-MS analysis). All identification and quantification results are reported in Table 5, showing an overall matching with cocoa butter content profile, according to literature [9].

Acknowledgements
This work was supported by the University of Turin (Fondi Ricerca Locale 2016). The authors warmly acknowledge EPIC srl for their kind assistance with the Rotocav s tests.

Transparency document. Supporting information
Transparency data associated with this article can be found in the online version at https://doi.org/ 10.1016/j.dib.2018.11.129. Table 5 FAMEs composition of the hexane phase from UAE extracts obtained using the ternary mixture, expressed as w/w percentage on the extract.