Metabolic Profiling of Varronia curassavica Jacq. Terpenoids by Flow Modulated Two-Dimensional Gas Chromatography Coupled to Mass Spectrometry

Abstract

In this study, a metabolomic approach was used to investigate the effect of seasonality on the chemical composition and yield of anti-inflammatory active principle, α-humulene, in the essential oil of three genotypes of Varronia curassavica Jacq. (Syn. Cordia verbenaceae). The essential oils were extracted by hydrodistillation and analyzed by comprehensive two-dimensional gas chromatography coupled to mass spectrometry (GC×GC-MS). The GC×GC approach a three-fold improvement in qualitative analysis (48 compounds were identified by GC-MS versus 135 by GC×GC-MS). The improved resolving power of GC×GC resolved important coelutions and enabled the detection of unusual substances in V. curassavica essential oil. The chromatographic data was analyzed by using peak table-based chemometrics, namely, principal component analysis (PCA) and hierarchical cluster analysis (HCA). The metabolic study showed that seasonality has a significant effect on the chemical composition. The α-humulene content was affected by genotype and season. Spring and summer were the best harvest seasons for the yield of the active ingredient, found in higher concentrations in the VC2 genotype. The proposed metabolomic workflow was successfully applied to terpene analysis found in V. curassavica essential oil, and such results have broadened our understanding of the influence of seasonal factors on the specialized metabolism of the species.

Essential Oils of New Lippia alba Genotypes Analyzed by Flow-Modulated Comprehensive Two-Dimensional Gas Chromatography (GC×GC) and Chemometric Analysis

“…A reproducible division of approximately 1:6 was achieved throughout the experiments. The interested reader is directed elsewhere for more details on the instrument setup [ 17 , 18 , 19 ].…”

“…Analytical tools that provide high resolution and sensitivity for untargeted analysis of the plant metabolome are desperately needed. Among these tools, comprehensive two-dimensional gas chromatography coupled to mass spectrometry (GC×GC-MS) is characterized for the increased peak capacity [ 17 , 18 , 19 ], increasing the identification power of plants volatiles and semi-volatiles composition [ 20 , 21 ].…”

Recent trends in the chromatographic analysis of volatile flavor and fragrance compounds: Annual review 2020

“…In addition to the detailed characterization of the V. curassavica essential oil, the active ingredient in the oil that is monitored by the pharmaceutical industry, α‐humulene, was quantified in the different oil samples. It was found that the concentration of this compound is influenced by both the genotype as well as the harvest season 77 …”

Advanced tuning of the ion management parameters in GC × GC-HRMS using a Fourier transform Orbitrap mass analyzer for pixel-based data handling and multivariate analysis

“…This technique combines two sequential separations by exploring complementary solvation properties, signicantly enhancing the peak capacity of the composite system. 1,2 For instance, GC Â GC separations have been successfully applied to metabolomics, [3][4][5] food analysis, [6][7][8] and petroleomics [9][10][11][12] where analyte discovery and identication beneted from the improved chromatographic resolution. Also, the enhanced peak capacity of GC Â GC enables simplication of sample preparation methods, 13 which is interesting for non-targeted analyses with limited sample availability or scouting studies.…”