A multi-analytical strategy for the valorization of goldenberry calyx, a promising source of health-promoting compounds, is presented in this work. A comprehensive characterization of P. peruviana calyx extracts, obtained by an optimized pressurized liquid extraction (PLE) procedure, is developed applying first an ultra-high-performance liquid chromatography coupled to quadrupole time-of-flight tandem mass spectrometry (UPLC-ESI-q-TOF-MS/MS) method in positive and negative electrospray ionization (ESI) mode. A total of fifty-nine phytochemicals, including major phenolic components, several withanolides (C28-isoprenoids) with a variety of biological activities, and a large family of anti-inflammatory sucrose esters were tentatively identified using this methodology. An integrated identification strategy based on accurate mass data obtained by high resolution mass spectrometry (HRMS), ion source fragmentation, MS/MS fragmentation patterns, generated molecular formulae and subsequent unsaturation degree calculation, along with database and bibliographic search is proposed.Isobaric withanolides-type compounds were tentatively identified or classified according to their different hydroxy and epoxy positions, on the basis of the complementary information provided by MS/MS product ion spectra obtained in both ESI+ and ESI-mode. The proposed structural elucidation approach provides a valuable contribution to the limited information available regarding the MS/MS structural analysis of withanolides in ESI(-) mode. Moreover, an alternative elucidation strategy based on deconvolution and database search was successfully applied for the phytochemical profiling analysis of the volatile fraction of P. peruviana calyx extracts by gas chromatography quadrupole time-of-flight mass spectrometry (GC-q-TOF-MS), which reveals the presence of relevant terpenoids, including phytosterols and tocopherols (Vitamin E). The results of the phytochemical characterization obtained herein demonstrates the great potential of applying integrated identification strategies to HRMS data obtained from complementary LC-and GC-q-TOF-MS(/MS) platforms, as powerful

The neuroprotective potential of 32 natural extracts obtained from olive oil by-products was investigated. The online coupling of supercritical fluid extraction (SFE) and dynamic adsorption/desorption allowed the selective enrichment of olive leaves extracts in different terpenoids’ families. Seven commercial adsorbents based on silica gel, zeolite, aluminum oxide, and sea sand were used with SFE at three different extraction times to evaluate their selectivity towards different terpene families. Collected fractions were analyzed by gas chromatography coupled to quadrupole-time-of-flight mass spectrometry (GC-QTOF-MS) to quantify the recoveries of monoterpenes (C10), sesquiterpenes (C15), diterpenes (C20), and triterpenes (C30). A systematic analysis of the neuroprotective activity of the natural extracts was then carried out. Thus, a set of in vitro bioactivity assays including enzymatic (acetylcholinesterase (AChE), butyrylcholinesterase (BChE)), and anti-inflammatory (lipoxidase (LOX)), as well as antioxidant (ABTS), and reactive oxygen and nitrogen species (ROS and RNS, respectively) activity tests were applied to screen for the neuroprotective potential of these extracts. Statistical analysis showed that olive leaves adsorbates from SS exhibited the highest biological activity potential in terms of neuroprotective effect. Blood–brain barrier permeation and cytotoxicity in HK-2 cells and human THP-1 monocytes were studied for the selected olive leaves fraction corroborating its potential.

In this work, a review about the applicability of eutectic solvents, mainly deep eutectic solvents (DES) and natural deep eutectic solvents (NADES), for the extraction of bioactive compounds from natural products has been carried out. These alternative solvents have shown not only to have high extraction yields but also to be environmentally friendly, exhibiting very low or almost no toxicity, compared to conventional organic solvents. The last trends and main extraction methods that have been most widely used in studies using these emerging solvents have been reviewed, as well as the varied natural sources in which they have been used, including agro-food by-products. Besides the toxicity, biodegradability of these solvents is reviewed. Likewise, different reported bioactivity tests have been included, in which extracts obtained with these ecological solvents have been tested from antioxidant activity analysis to in vivo studies with rats, through in vitro cytotoxicity tests.

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This work aimed to evaluate the nutritional composition, techno-functional, and in vitro physiological properties of flours from six different insect species and the sensorial feasibility of including them in a...

This work reports the use of GC-QTOF-MS to obtain a deep characterization of terpenoid compounds recovered from olive leaves, which is one of the largest by-products generated by the olive oil industry. This work includes an innovative supercritical CO2 fractionation process based on the online coupling of supercritical fluid extraction (SFE) and dynamic adsorption/desorption for the selective enrichment of terpenoids in the different olive leaves extracts. The selectivity of different commercial adsorbents such as silica gel, zeolite, and aluminum oxide was evaluated toward the different terpene families present in olive leaves. Operating at 30 MPa and 60 °C, an adsorbent-assisted fractionation was carried out every 20 min for a total time of 120 min. For the first time, GC-QTOF-MS allowed the identification of 40 terpenoids in olive leaves. The GC-QTOF-MS results indicate that silica gel is a suitable adsorbent to partially retain polyunsaturated C10 and C15 terpenes. In addition, aluminum oxide increases C20 recoveries, whereas crystalline zeolites favor C30 terpenes recoveries. The different healthy properties that have been described for terpenoids makes the current SFE-GC-QTOF-MS process especially interesting and suitable for their revalorization.

Staphyloxanthin (STX) is a saccharolipid derived from a carotenoid in Staphylococcus aureus involved in oxidative-stress tolerance and antimicrobial peptide resistance. In this work, a targeted metabolomics and biophysical study was carried out on native and knock-out S. aureus strains to investigate the biosynthetic pathways of STX and related carotenoids. Identification of 34 metabolites at different growth phases (8, 24 and 48h), reveal shifts of carotenoid populations during progression towards stationary phase.Six of the carotenoids in the STX biosynthetic pathway and three menaquinones (Vitamin K2) were identified in the same chromatogram. Furthermore, other STX homologues with varying acyl chain structures reported herein for the first time, which reveal the extensive enzymatic activity of CrtO/CrtN. Fourier Transform infrared spectroscopy show that STX increases acyl chain order and shifts the cooperative melting of the membrane indicating a more rigid lipid bilayer. This study shows the diversity of carotenoids in S. aureus, and their influence on membrane biophysical properties.