The food industry has a direct interest into bittertasting substances either for the identification of negative off-flavors or for the monitoring of a desired organoleptic quality. A rapid technique, based on Fourier transform-near infrared (FT-NIR) spectroscopy and able to detect taste molecular markers in bakery commodities, was developed, focusing the attention on biscuits category. Xanthines (caffeine, theobromine, and theophylline) and polyphenols (catechins and epicathechins), considered as mainly responsible for the bitter-taste of coffee\cocoa\chocolate based products, were firstly checked using a confirmatory liquid chromatography (LC)-ESI\mass spectrometry (MS)-MS procedure after hot methanol–water extraction. Correspondent data were used for the calibration of the FT-NIR through PLS regression. Values of the standard errors of prediction (lower than 10 %) were comparable to the values of the standard errors of cross-validation. Coefficients of determination indicated a good predictive power in the calibration model (R2 xanthines00.97, R2 polyphenols00.96) and a satisfying discriminating power among different contents in the validation models (R2 xanthines00.96, R2 polyphenols00.96). A testing phase on the generated model was executed by a comparison of LC-MS and sensory panel data with FT-NIR responses recorded on unknown biscuits: differences between found and predicted levels were generally below 5 % and the best predictability was achievable in chocolate-based biscuits. This methodology is able to work directly on solid products, has the potential to be expanded on other categories of gustative molecular markers (like sugars) and can be conceived as applicable for a routine control of a standardized bitter taste quality in a real industrial production.
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