HS-SPME-GC-TOFMS Methodology for Verification of Geographical Origin and Authenticity Attributes of Coffee Samples
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Increasing consumer awareness of food safety issues requires the development of highly sophisticated techniques for the authentication of food commodities. The food products targeted for falsification are either products of high commercial value or those produced in large quantities. For this reason, the present investigation is directed toward the characterization of coffee samples according to geographical origin attributes. In addition, the current examination is focused on the identification of particular marker compounds that compose the volatile and semivolatile aroma fraction of flavoured and dessert coffees. The conducted research involved the development of a rapid headspace solid phase microextraction (HS-SPME) – gas chromatography – time-of-flight mass spectrometry (GC-TOFMS) method for the verification of geographical origin traceability of coffee samples. As opposed to the utilization of traditional univariate optimization methods, the current study employs the application of multivariate experimental designs to the optimization of extraction-influencing parameters. Hence, the two-level full factorial first-order design aided in the identification of two influential variables: extraction time and sample temperature. The optimum set of conditions for the two variables was 12 min and 55 oC, respectively, as directed by utilization of the Doehlert matrix and response surface methodology. The high-throughput automated SPME procedure was completed under optimized conditions by implementing a single divinylbenzene/carboxen/polydimethylsiloxane (DVB/CAR/PDMS) metal fiber with excellent properties of durability, which ensured the complete analysis of coffee samples in sequence. The coffee sample originating from an authentic Brazilian coffee producing region and characterized by rich volatile and semivolatile chromatographic profiles was selected as a reference starting point for data evaluation. The combination of the retention index (RI) system using C8-C40 alkanes and the mass spectral library search was utilized for the confirmation of analyte identity in this reference sample. Twenty-nine volatile and semivolatile compounds selected across the wide range of GC chromatogram were then evaluated in terms of chromatographic peak areas for all samples that are to be submitted to this classification study. The semiquantitative results were submitted to statistical evaluation, namely principal component analysis (PCA) for the establishment of corresponding geographical origin discriminations.
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Sanja Risticevic (2008). HS-SPME-GC-TOFMS Methodology for Verification of Geographical Origin and Authenticity Attributes of Coffee Samples. UWSpace. http://hdl.handle.net/10012/3574