Abstract
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.
Highlights
Black pepper (Piper nigrum L.), known as the “king of spices”, is one of the most widely used spices all over the world.[1]
The aim of this study was to demonstrate the feasibility of gas chromatography (GC)-Orbitrap-high-resolution mass spectrometry (HRMS) fingerprinting combined with multivariate data analysis, using unsupervised principal component analysis (PCA) and hierarchical cluster analysis (HCA) as well as supervised OPLS-DA, for geographical traceability of Brazilian, Sri Lankan, and Vietnamese black pepper samples
A metabolomics approach based on GCOrbitrap-HRMS fingerprinting was applied for black pepper authentication, and the extraction procedure, as well as the chromatographic conditions, were optimized to obtain as much metabolite information as possible from nonpolar volatile chemicals
Summary
Black pepper (Piper nigrum L.), known as the “king of spices”, is one of the most widely used spices all over the world.[1] The largest producers of black pepper include worldwide tropical regions such as India, Brazil, Vietnam, and Sri Lanka, among others.[2] This spice, belonging to the Piperaceae plant family, is largely used as a food condiment[3] and applied in traditional medicine due to its well-known medicinal properties.[4] The essential oil of black pepper has been reported to be composed of monoterpenes (47−64%) followed by sesquiterpenes (30−47%), containing a huge variety of naturally occurring volatile compounds such as β-caryophyllene, myrcene, sabinene, and β-pinene, among others.[2] It is wellknown that the metabolic composition of black pepper may be influenced by several factors including crop conditions, time of harvest (maturity), extraction method, storage, geographical origin, and spice processing, among others,[5] with the remarkable influence of the region of origin.[4] the heat treatment applied during some spice processing (e.g., sterilization or drying processes) may lead to the inactivation of some compounds, and the increase of others by inhibiting some enzymes, as well as the formation of some chemicals.[6]
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