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Feasibility of Applying Untargeted Metabolomics with GC-Orbitrap-HRMS and Chemometrics for Authentication of Black Pepper (Piper nigrum L.) and Identification of Geographical and Processing Markers.

Black pepper is one of the most consumed spices all over the world. Due to its high demand and nutritional value, a metabolomics approach based on GC-Orbitrap-HRMS fingerprinting and chemometrics was applied to assess its geographical traceability and processing authenticity. GC-HRMS-based fingerprints were obtained using a simple ultrasound-assisted extraction method, which may be easily implemented in routine activities of quality control. Unsupervised methods, such as principal component analysis (PCA), were performed for sample overview according to the investigated origins (Brazil, Vietnam, and Sri Lanka) and processing (sterilized vs nonsterilized samples). Further orthogonal partial least squares discriminant analysis (OPLS-DA) models were validated by cross- and external validation, providing satisfactory performance for geographical and processing authentication, as well as excellent predictive ability for further samples. Furthermore, reliable putative identification of 12 key metabolites (markers) was performed, highlighting the feasibility of combining untargeted GC-HRMS analysis with chemometrics for quality control of black pepper.