Confirmation of the unexpected occurrence of bitterness-inducing cucurbitacins in edible unripe melons by a two-step workflow based on liquid chromatography with combined UV and high-resolution MS detection.

Plant metabolites known as cucurbitacins are known to impart an unpleasant bitter taste to edible fruits and even lead to severe health complications after the ingestion of relatively high amounts. In this study, an analytical method based on reversed phase liquid chromatography with combined detection by UV spectroscopy and atmospheric pressure chemical ionization high-resolution single/tandem mass spectrometry was applied to confirm the occurrence of four cucurbitacins (B, D, and R, and 23,24-dihydro cucurbitacin B) previously inferred in unexpectedly bitter-tasting fruits of an Italian variety (Scopatizzo) of unripe melon (Cucumis melo L.), known for the sweetness of its fruits.

Noninvasive Assessment of portal Hypertension in Patients With Primary Biliary Cholangitis is Affected by Severity of Cholestasis.

Background & Aims: Noninvasive tests (NITs) for ruling-out clinical significant portal hypertension (CSPH) and high-risk varices (HRVs) in patients with primary biliary cholangitis (PBC) and compensated advanced chronic liver disease (cACLD) are lacking. We evaluated NITs in these patients and the influence of cholestasis on their performance.

Methods: Consecutive patients from the "Italian PBC registry" and 2 United Kingdom large-volume PBC referral centers with upper endoscopy within 6 months from biochemical evaluation and transient elastography were included.

Integrating Epoxidation, High-Resolution Mass Spectrometry and Ultraviolet Spectroscopy to Unravel the Complex Profile of Boswellic Acids and Related Compounds in the Gum Resin Extract.

The chemical characterization of natural products is often a complex task that demands powerful analytical techniques. Liquid chromatography with high-resolution tandem mass spectrometry (HRMS/MS) is often employed, yet it can face hard challenges when isomeric species are present, and reference standards are lacking. In such cases, the confidence level in compound identification can be significantly improved by the collection of orthogonal information on target analytes.

Effectiveness of gellan gum scaffolds loaded with Boswellia serrata extract for in-situ modulation of pro-inflammatory pathways affecting cartilage healing.

In this study, we developed a composite hydrogel based on Gellan gum containing Boswellia serrata extract (BSE). BSE was either incorporated directly or loaded into an MgAl-layered double hydroxide (LDH) clay to create a multifunctional cartilage substitute. This composite was designed to provide anti-inflammatory properties while enhancing chondrogenesis.

Lipidomics reveals the reshaping of the mitochondrial phospholipid profile in cells lacking OPA1 and mitofusins.

Depletion or mutations of key proteins for mitochondrial fusion, like optic atrophy 1 (OPA1) and mitofusins 1 and 2 (Mfn 1 and 2), are known to significantly impact the mitochondrial ultrastructure, suggesting alterations of their membranes' lipid profiles. In order to make an insight into this issue, we used hydrophilic interaction liquid chromatography coupled with electrospray ionization-high resolution MS to investigate the mitochondrial phospholipid (PL) profile of mouse embryonic fibroblasts knocked out for OPA1 and Mfn1/2 genes. One hundred sixty-seven different sum compositions were recognized for the four major PL classes of mitochondria, namely phosphatidylcholines (PCs, 63), phosphatidylethanolamines (55), phosphatidylinositols (21), and cardiolipins (28).

Exploration of the Lipid Profile of Edible Oleaginous Microgreens by Mass Spectrometry-Based Lipidomics.

The spreading awareness of the health benefits associated with the consumption of plant-based foods is fueling the market of innovative vegetable products, including microgreens, recognized as a promising source of bioactive compounds. To evaluate the potential of oleaginous plant microgreens as a source of bioactive fatty acids, gas chromatography-mass spectrometry was exploited to characterize the total fatty acid content of five microgreens, namely, chia, flax, soy, sunflower, and rapeseed (canola). Chia and flax microgreens appeared as interesting sources of α-linolenic acid (ALA), with total concentrations of 2.

Development, Analytical Characterization, and Bioactivity Evaluation of Extract-Layered Double Hydroxide Hybrid Composites.

extract (BSE), rich in boswellic acids, is well known as a potent anti-inflammatory natural drug. However, due to its limited aqueous solubility, BSE inclusion into an appropriate carrier, capable of improving its release in the biological target, would be highly desirable. Starting with this requirement, new hybrid composites based on the inclusion of BSE in a lamellar solid layered double hydroxide (LDH), i.

Methyl carbamates of phosphatidylethanolamines and phosphatidylserines reveal bacterial contamination in mitochondrial lipid extracts of mouse embryonic fibroblasts.

The occurrence of methyl carbamates of phosphatidylethanolamines and phosphatidylserines in the lipid extract of mitochondria obtained from mouse embryonic fibroblasts was ascertained by hydrophilic interaction liquid chromatography with electrospray ionization single and multi-stage mass spectrometry, performed using sinergically a high resolution (quadrupole-Orbitrap) and a low resolution (linear ion trap) spectrometer. Two possible routes to the synthesis of methyl carbamates of phospholipids were postulated and evaluated: (i) a chemical transformation involving phosgene, occurring as a photooxidation by-product in the chloroform used for lipid extraction, and methanol, also used for the latter; (ii) an enzymatic methoxycarbonylation reaction due to an accidental bacterial contamination, that was unveiled subsequently on the murine mitochondrial sample. A specific lipid extraction performed on a couple of standard phosphatidyl-ethanolamines/-serines, based on purposely photo-oxidized chloroform and deuterated methanol, indicated route (i) as negligible in the specific case, thus highlighting the enzymatic route related to bacterial contamination as the most likely source of methyl carbamates.

A targeted GC-MS/MS approach for the determination of eight sterols in microgreen and mature plant material.

Over the past decades, a remarkable number of scientific studies supported the correlation between an adequate dietary intake of phytosterols (PS) and the reduced risk of cardiovascular diseases. PS are known to inhibit the intestinal absorption of cholesterol, thus promoting the reduction of the low-density lipoproteins (LDL) amount in the bloodstream. Despite the fact that a non-negligible atherogenicity was recognized to PS, thus requiring a careful risk-benefits assessment for plant sterol supplementation, the potential role of PS as cholesterol-lowering agents has been contributing to the spreading awareness of the health benefits associated with the consumption of plant-based foods.

PE, or not PE, that is the question: The case of overlooked lyso-N-acylphosphatidylethanolamines.

Rationale: Lyso derivatives of N-acyl-1,2-diacylglycero-3-phosphoethanolamines (L-NAPEs) are a lipid class mostly expressed in vegetables during stress and tissue damage that is involved in the synthesis of the lipid mediator N-acylethanolamines. L-NAPEs can be challenging to distinguish from isomeric phosphatidylethanolamines (PEs), especially in extracted complex samples where they could be confused with abundant PEs.

Methods: In this study, hydrophilic interaction liquid chromatography with electrospray ionization hyphenated with (tandem) mass spectrometry (MS) was proposed to distinguish L-NAPEs and PEs as deprotonated molecules, [M - H] , using both high-resolution/accuracy Fourier transform MS and low-resolution linear ion trap (LIT) mass analyzers.

Hydrogen/Deuterium Exchange Mass Spectrometry for Probing the Isomeric Forms of Oleocanthal and Oleacin in Extra Virgin Olive Oils.

Reversed-phase liquid chromatography and electrospray ionization with Fourier-transform single and tandem mass spectrometry (RPLC-ESI-FTMS and FTMS/MS) were employed for the structural characterization of oleocanthal (OLEO) and oleacin (OLEA), two of the most important bioactive secoiridoids occurring in extra virgin olive oils (EVOOs). The existence of several isoforms of OLEO and OLEA was inferred from the chromatographic separation, accompanied, in the case of OLEA, by minor peaks due to oxidized OLEO recognized as oleocanthalic acid isoforms. The detailed analysis of the product ion tandem MS spectra of deprotonated molecules ([M-H]) was unable to clarify the correlation between chromatographic peaks and specific OLEO/OLEA isoforms, including two types of predominant dialdehydic compounds, named , containing a double bond between carbon atoms C8 and C10, and a group of diasteroisomeric closed-structure (i.

All Ion Fragmentation Analysis Enhances the Untargeted Profiling of Glucosinolates in Microgreens by Liquid Chromatography and High-Resolution Mass Spectrometry.

An analytical approach based on reversed-phase liquid chromatography coupled to electrospray ionization Fourier-transform mass spectrometry in negative ion mode (RPLC-ESI-(-)-FTMS) was developed for the untargeted characterization of glucosinolates (GSL) in the polar extracts of four microgreen crops, namely, garden cress, rapeseed, kale, and broccoli raab. Specifically, the (AIF) operation mode enabled by a quadrupole-Orbitrap mass spectrometer, i.e.

Glycerophospholipidomics of Five Edible Oleaginous Microgreens.

Microgreens are a special type of vegetal product, born as a culinary novelty (traditionally used to garnish gourmet dishes) and then progressively studied for their potentially high content in nutraceuticals, like polyphenolic compounds, carotenoids, and glucosinolates, also in the perspective of implementing their cultivation in space stations/colonies. Among further potential nutraceuticals of microgreens, lipids have received very limited attention so far. Here, glycerophospholipids contained in microgreens of typical oleaginous plants, namely, soybean, chia, flax, sunflower, and rapeseed, were studied using hydrophilic interaction liquid chromatography (HILIC), coupled to high-resolution Fourier transform mass spectrometry (FTMS) or low-resolution collisionally induced dissociation tandem mass spectrometry (CID-MS) with electrospray ionization (ESI).

HILIC-ESI-MS analysis of phosphatidic acid methyl esters artificially generated during lipid extraction from microgreen crops.

The uncontrolled activation of endogenous enzymes may introduce both qualitative and quantitative artefacts when lipids are extracted from vegetal matrices. In the present study, a method based on hydrophilic interaction liquid chromatography coupled either to high-resolution/accuracy Fourier-transform mass spectrometry (HILIC-ESI-FTMS) or to linear ion trap multiple stage mass spectrometry (HILIC-ESI-MS , with n = 2 and 3) with electrospray ionization was developed to unveil one of those artefacts. Specifically, the artificial generation of methyl esters of phosphatidic acids (MPA), catalysed by endogenous phospholipase D (PLD) during lipid extraction from five oleaginous microgreen crops (chia, soy, flax, sunflower and rapeseed), was studied.

Bioactive Secoiridoids in Italian Extra-Virgin Olive Oils: Impact of Olive Plant Cultivars, Cultivation Regions and Processing.

In the last two decades, phenolic compounds occurring in olive oils known as have attracted a great interest for their bioactivity. Four major olive oil secoiridoids, i.e.

Insight into the Storage-Related Oxidative/Hydrolytic Degradation of Olive Oil Secoiridoids by Liquid Chromatography and High-Resolution Fourier Transform Mass Spectrometry.

The study of negative effects potentially exerted by the exposure to oxygen and/or light and, thus, also by the type of container on the quality of extra virgin olive oil (EVOO) during its prolonged storage requires an appropriate choice of analytical methods and components to be monitored. Here, reverse-phase liquid chromatography coupled to high-resolution/accuracy Fourier transform mass spectrometry with electrospray ionization was exploited to study oxidative/hydrolytic degradation processes occurring on the important bioactive components of EVOO known as secoiridoids, i.e.

Influence of Horizontal Centrifugation Processes on the Content of Phenolic Secoiridoids and Their Oxidized Derivatives in Commercial Olive Oils: An Insight by Liquid Chromatography-High-Resolution Mass Spectrometry and Chemometrics.

Reversed-phase liquid chromatography with electrospray ionization-high-resolution/accuracy Fourier transform mass spectrometry (RPC-ESI-FTMS) and chemometrics were exploited to evaluate the influence of horizontal centrifugation by two- or three-phase decanters on the content of major phenolic secoiridoids in extravirgin olive oils (EVOOs). Despite the occurrence of other potential sources of variability typical of commercial olive oils, horizontal centrifugation was found to play a primary role, with a general increase of secoiridoid content occurring when two-phase decanters were used. As emphasized by principal component analysis (PCA), the increase involved preferentially oleacin and oleocanthal, when oxidative deterioration was purposely minimized during and/or after production, and oleuropein and ligstroside aglycones, when no vertical centrifugation was performed at the end of the productive cycle.