Metabolite Profiling of “Green” Extracts of Cynara cardunculus subsp. scolymus, Cultivar “Carciofo di Paestum” PGI by 1H NMR and HRMS-Based Metabolomics

Abstract

Globe artichoke (Cynara cardunculus L. var. scolymus (L.), is a perennial plant widely cultivated in the Mediterranean area, known for its edible part named capitula or heads. Its functional properties are related to its high levels of polyphenolic compounds and inulin. “Carciofo di Paestum”, an Italian traditional cultivar, is a labeled PGI (Protected Geographical Indication) product of the Campania region, representing an important economic resource. So far, a few chemical investigations were performed on this cultivar, mainly focused on the analysis of methanol extracts. Due to the increasing use of food supplements, in this study, a comprehensive analysis of green extracts of Carciofo di Paestum” PGI heads was performed. EtOH, EtOH: H2O (80:20, 70:30, 60:40) extracts, as well as infusions and decoctions prepared according to Pharmacopeia XII were analyzed by LC-ESI/QExactive/MS/MS. A total of 17 compounds corresponding to caffeoylquinic acid derivatives, phenolics, flavonoids, and terpenoids were identified. The extracts were further submitted to NMR analysis to highlight the occurrence of primary metabolites. Both LCMS and NMR data were analyzed by Principal Component Analysis (PCA), showing significant differences among the extraction methods. Moreover, 5-caffeoylquinic acid and 1,5-dicaffeoylquinic acid were quantified in the extracts by LC-ESI/QTrap/MS/MS using the Multiple Reaction Monitoring (MRM) method. Furthermore, the phenolic content, antioxidant activity, and α-glucosidase inhibitory activity of C. cardunculus var. scolymus “Carciofo di Paestum” extracts were evaluated.

Metabolite Profiling for Typization of “Rucola della Piana del Sele” (PGI), Eruca sativa, through UHPLC-Q-Exactive-Orbitrap-MS/MS Analysis

“…A quantitative analysis was performed on an LC-ESI/QTrap/MS system, operating in multiple reaction monitoring (MRM) mode [ 22 ], on a C18 reversed-phase (RP) column (50 mm, 2.1 mm; Luna Omega C18, 1.6 µm; Phenomenex, Aschaffenburg, Germany) kept at 30 °C, with a flow rate of 0.30 mL/min. A mobile phase consisting of a combination of A (0.5% HCOOH in water, v / v ) and B (0.5% HCOOH in acetonitrile, v / v ) was used.…”

Development of a New Extraction Method for Pomegranate and Metabolite Profiling by a LC-MS and 1H NMR Combined Approach

“…To detect not only the specialised metabolites but also the primary metabolites present in juice, NAV(EtOH:H2O), and NAV(EtOH:juice) extracts, an approach based on 1 H NMR analysis was carried out [39] (Figure 3). The non-destructive nature, simplicity of sample preparation, rapid analysis and avoidance of the need of chromatographic separations make 1 H NMR a valuable technique in metabolite analysis [40]. This type of analysis is common in metabolomics and natural product studies, where the goal is to identify and quantify various compounds present in a complex mixture.…”

Compound-Specific 1D 1H NMR Pulse Sequence Selection for Metabolomics Analyses

“…One-dimensional (1D) 1 H NMR-based metabolomics studies utilize different methods to analyze metabolites in biological samples of plants, animals, humans, and marine organisms. These samples may include serum; plasma; urine; cell extracts; intestinal content; tissue; − plant seeds, flesh, leaves, stems, and roots; − and corals, algae, and jellyfish. − In high-resolution NMR spectroscopy, the focus is on the relational quantification of metabolites and estimation of metabolite concentrations in response to some perturbation. Metabolomics is used to observe relative quantitative changes and find out biomarkers. − Higher-dimensional NMR like pulse sequences of two-dimensional (2D) NMR is also used in metabolomics. − However, compared to a matching 1 H NMR data set, 2D NMR data-processing time is significantly shorter because the signal overlap is not a significant issue and deconvolution is not necessary …”