Human Biomonitoring of T-2 Toxin, T-2 Toxin-3-Glucoside and Their Metabolites in Urine through High-Resolution Mass Spectrometry

The metabolic profile of T-2 toxin (T-2) and its modified form T-2-3-glucoside (T-2-3-Glc) remain unexplored in human samples. Therefore, the present study aimed to investigate the presence of T-2, T-2-3-Glc and their respective major metabolites in human urine samples (n = 300) collected in South Italy through an ultra-high performance liquid chromatography (UHPLC) coupled to Q-Orbitrap-HRMS methodology. T-2 was quantified in 21% of samples at a mean concentration of 1.34 ng/mg Crea (range: 0.22–6.54 ng/mg Crea). Almost all the major T-2 metabolites previously characterized in vitro were tentatively found, remarking the occurrence of 3′-OH-T-2 (99.7%), T-2 triol (56%) and HT-2 (30%). Regarding T-2-3-Glc, a low prevalence of the parent mycotoxin (1%) and its metabolites were observed, with HT-2-3-Glc (17%) being the most prevalent compound, although hydroxylated products were also detected. Attending to the large number of testing positive for T-2 or its metabolites, this study found a frequent exposure in Italian population.

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Phytochemical Study and In Vitro Screening Focusing on the Anti-Aging Features of Various Plants of the Greek Flora

Antioxidants ◽

10.3390/antiox10081206 ◽

2021 ◽

Vol 10 (8) ◽

pp. 1206

Author(s):

Aimilia D. Sklirou ◽

Maria T. Angelopoulou ◽

Aikaterini Argyropoulou ◽

Eliza Chaita ◽

Vasiliki Ioanna Boka ◽

...

Keyword(s):

Plant Species ◽

High Performance ◽

High Resolution Mass Spectrometry ◽

Ultra Performance Liquid Chromatography ◽

Skin Aging ◽

Rosa Damascena ◽

Phytochemical Study ◽

Age Related

Skin health is heavily affected by ultraviolet irradiation from the sun. In addition, senile skin is characterized by major changes in the collagen, elastin and in the hyaluronan content. Natural products (NPs) have been shown to delay cellular senescence or in vivo aging by regulating age-related signaling pathways. Moreover, NPs are a preferable source of photoprotective agents and have been proven to be useful against the undesirable skin hyperpigmentation. Greek flora harvests great plant diversity with approximately 6000 plant species, as it has a wealth of NPs. Here, we report an extensive screening among hundreds of plant species. More than 440 plant species and subspecies were selected and evaluated. The extracts were screened for their antioxidant and anti-melanogenic properties, while the most promising were further subjected to various in vitro and cell-based assays related to skin aging. In parallel, their chemical profile was analyzed with High-Performance Thin-Layer Chromatography (HPTLC) and/or Ultra-Performance Liquid Chromatography High-Resolution Mass Spectrometry (UPLC-HRMS). A variety of extracts were identified that can be of great value for the cosmetic industry, since they combine antioxidant, photoprotective, anti-melanogenic and anti-aging properties. In particular, the methanolic extracts of Sideritis scardica and Rosa damascena could be worthy of further attention, since they showed interesting chemical profiles and promising properties against specific targets involved in skin aging.

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Chemical Constituents of Stems and Leaves of Tagetespatula L. and Its Fingerprint

Molecules ◽

10.3390/molecules24213911 ◽

2019 ◽

Vol 24 (21) ◽

pp. 3911 ◽

Cited By ~ 2

Author(s):

Yu-Meng Wang ◽

Xiao-Ku Ran ◽

Muhammad Riaz ◽

Miao Yu ◽

Qian Cai ◽

...

Keyword(s):

High Performance ◽

High Resolution Mass Spectrometry ◽

Chemical Constituents ◽

Human Gastric Cancer ◽

Chemical Structures ◽

Yellow Color ◽

Ic50 Values ◽

Gastric Cancer Cell Lines ◽

Stems And Leaves

Tagetespatula L. is a widely cultivated herbal medicinal plant in China and other countries. In this study, two new 2, 3-dihydrobenzofuran glucosides (1, 2) and fourteen known metabolites (3–16) were isolated from the stems and leaves of T. patula (SLT). The chemical structures of the isolated compounds were characterized comprehensively based on one- and two-dimensional NMR spectroscopy and high resolution mass spectrometry. Absolute configurations of compounds 1 and 2 were determined by ECD calculations. Compounds 1 and 2 exhibited moderate in vitro inhibitory activities against human gastric cancer cell lines (AGS) with IC50 values of 41.20 μmol/L and 30.43 μmol/L, respectively. The fingerprint profiles of stems and leaves of T. patula with three color types of flowers (Janie Yellow Bright, Jinmen Orange, Shouyao Red and Yellow color) were established by high-performance liquid chromatography (HPLC). Ten different batches of stems and leaves were examined as follow: Shouyao Red and Yellow color (1, 2, 3), Janie Yellow Bright (4, 5, 6, 7) and Jinmen Orange (8, 9, 10). Twenty-two common peaks were identified with similarity values ranging from 0.910 to 0.977. Meanwhile, the average peak area of SLT in the three types of flowers was different and it was the highest in Janie Yellow Bright.

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Hepatoprotective activity of a purified methanol extract and saponins from the roots of Chenopodium bonus-henricus L.

Zeitschrift für Naturforschung C ◽

10.1515/znc-2019-0002 ◽

2019 ◽

Vol 74 (11-12) ◽

pp. 329-337 ◽

Cited By ~ 2

Author(s):

Zlatina Kokanova-Nedialkova ◽

Paraskev Nedialkov ◽

Magdalena Kondeva-Burdina ◽

Rumyana Simeonova

Keyword(s):

High Performance ◽

High Resolution Mass Spectrometry ◽

Antioxidant Activities ◽

Rat Hepatocytes ◽

Hepatoprotective Activity ◽

Cellular Damage ◽

Medicagenic Acid ◽

Hepatoprotective Agents

Abstract An ultra-high-performance liquid chromatography-high-resolution mass spectrometry based profiling of a purified MeOH extract (PME) from the roots of Chenopodium bonus-henricus L. (Amaranthaceae) tentatively identified 15 saponins of six sapogenins. The PME exerts hepatoprotective and antioxidant activities comparable to those of flavonoid complex silymarin in in vitro (1 and 10 μg/mL) and in vivo (200 mg/kg/daily for 7 days) models of hepatotoxicity, induced by CCl4. The main constituents of PME, respectively saponins bonushenricoside A (1), 3-O-β-D-glucuronopyranosyl-bayogenin-28-O-β-D-glucopyranosyl ester (2), 3-O-β-D-glucuronopyranosyl-medicagenic acid-28-O-β-D-xylopyranosyl (1→4)-α-L-rhamnopyranosyl(1→2)-α-L-arabinopyranosyl ester (3), 3-O-β-D-glucuronopyranosyl-2β-hydroxygypsogenin-28-O-β-D-glucopyranosyl ester (4), 3-O-α-L-rabinopyranosyl-bayogenin-28-O-β-D-glucopyranosyl ester (6) and bonushenricoside B (8) (3 μg/mL each), compared to silymarin (5 and 50 μg/mL), significantly reduced the cellular damage caused by CCl4 in rat hepatocytes, preserved cell viability and glutathione level, decreased lactate dehydrogenase leakage and reduced lipid damage. The experimental data suggest that the glycosides of phytolaccagenin, bayogenin, medicagenic acid, 2β-hydroxygypsogenin, 2β-hydroxyoleanoic acid and oleanoic acid are a promising and safe class of hepatoprotective agents.

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Antifungal Activity of Saponins from the Fruit Pericarp of Sapindus mukorossi against Venturia inaequalis and Botrytis cinerea

Plant Disease ◽

10.1094/pdis-06-17-0906-re ◽

2018 ◽

Vol 102 (5) ◽

pp. 991-1000 ◽

Cited By ~ 7

Author(s):

Franziska M. Porsche ◽

Daniel Molitor ◽

Marco Beyer ◽

Sophie Charton ◽

Christelle André ◽

...

Keyword(s):

Liquid Chromatography ◽

Antifungal Activity ◽

Botrytis Cinerea ◽

Fungal Pathogens ◽

High Performance ◽

High Resolution Mass Spectrometry ◽

Venturia Inaequalis ◽

Field Trials ◽

Fruit Pericarp

The antifungal activity of an aqueous extract (AE) and the solid fraction of a chloroform-methanol fruit pericarp extract (CME) of Sapindus mukorossi resolved in water was tested for the first time against Venturia inaequalis and Botrytis cinerea—two important fungal pathogens worldwide. In the greenhouse, a CME (1% vol/vol) spray significantly reduced V. inaequalis symptoms and sporulation (99%) on apple seedling leaves (P ≤ 0.05). In field trials, applications of AE (1% vol/vol) reduced the disease severity of B. cinerea on grape, on average, by 63%. Extracts were fractionated by high-performance liquid chromatography and the bioefficacy of the fractions was tested in vitro. Some components of the most fungicidal fraction were identified by liquid chromatography-high resolution mass spectrometry as saponins: sapindoside B (accounting for ≥98% of the total constituents), hederagenin-pentosylhexoside, and oleanolic acid-hexosyl-deoxyhexosyl-hexoside. This fraction inhibited the mycelial growth of V. inaequalis and B. cinerea by 45 and 43%, respectively.

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Mapping the lipid metabolites in follicular fluid from patients with infertility issues across ages

10.21203/rs.2.24602/v1 ◽

2020 ◽

Author(s):

Xingxing Zhang ◽

Tianqi Wang ◽

Jingyan Song ◽

Jifeng Deng ◽

Zhengao Sun

Keyword(s):

Follicular Fluid ◽

High Performance ◽

High Resolution Mass Spectrometry ◽

Age Groups ◽

Follicular Development ◽

Principal Component ◽

Scientific Basis ◽

Vitro Fertilization ◽

Lipid Metabolites

Abstract Background: Follicular fluid is an important external environment for the growth and development of oocytes. A thorough identification of specific components in follicular fluid can better the existing understand of intracellular signal transduction and reveal potential biomarkers of oocyte health in women undergoing assisted reproductive therapy. To study the biomarkers that affect the development of oocytes, we have adopted a new method of SWATH to MRM( the sequential window acquisition of all theoretical fragment-ion spectra to multiple reaction monitor)metabolomics to provide extensive coverage and excellent quantitative data. This was done to investigate the differences in follicular fluid of patients undergoing in vitro fertilization (IVF) and embryo transfer in different age groups and to further explore the relationship between follicular fluid, age and reproductive function.Method: A combination of Ultra-high-performance liquid chromatography and high resolution mass spectrometry techniques were used to analyze the follicular fluid of 230 patients enrolled for the IVF cycle. The patients were of different ages grouped into two groups:the younger and older patients.The obtained multidimensional chromatographic data were processed by principal component analysis (PCA) and partial least squares discriminant analysis (PLS-DA). The charge ratios and mass numbers enabled for the identification of different fragments in the samples. Matching information obtained through database search and the fragment information obtained by fragment ion scan structurally identified substances in the samples. This was used to determine the differential compounds.Results: The quality and quantity of oocytes decline with age. This in caused by changes in follicular fluid metabolites. The main differences were in lipid metabolites. Some were up-regulated : Arachidonate, LysoPC(16:1), LysoPC(20:4) and LysoPC(20:3) while others were down-regulated: LysoPC(18:3) and LysoPC(18:1).Conclusions: Metabolomic analysis of follicular fluid revealed that with the increase in age, several differential metabolites are at play. Among these metabolites, lipid metabolism undergoes significant changes that affect the development of oocytes thus causing reduced fertility in older women. These differential metabolites related to follicular development may provide possible detection and treatment targets for promoting oocyte health, and provide scientific basis for understanding the environment of oocyte development.

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A Cup of Hemp Coffee by Moka Pot from Southern Italy: An UHPLC-HRMS Investigation

Foods ◽

10.3390/foods9081123 ◽

2020 ◽

Vol 9 (8) ◽

pp. 1123

Author(s):

Simona Piccolella ◽

Giuseppina Crescente ◽

Marialuisa Formato ◽

Severina Pacifico

Keyword(s):

High Performance ◽

High Resolution Mass Spectrometry ◽

Economic Problem ◽

Added Value ◽

Industrial Sectors ◽

Current Maximum ◽

Solid Liquid ◽

Industrial Hemp

After a long period defined by prohibition of hemp production, this crop has been recently re-evaluated in various industrial sectors. Until now, inflorescences have been considered a processing by-product, not useful for the food industry, and their disposal also represents an economic problem for farmers. The objects of the present work are coffee blends enriched with shredded inflorescences of different cultivars of industrial hemp that underwent solid/liquid extraction into the Italian “moka” coffee maker. The obtained coffee drinks were analyzed by Ultra-High-Performance Liquid Chromatography-High Resolution Mass Spectrometry (UHPLC-HRMS) tools for their quali-quantitative phytocannabinoid profiles. The results showed that they are minor constituents compared to chlorogenic acids and caffeine in all samples. In particular, cannabidiolic acid was the most abundant among phytocannabinoids, followed by tetrahydrocannabinolic acid. Neither Δ9-tetrahydrocannabinol (THC) nor cannabinol, its main oxidation product, were detected. The percentage of total THC never exceeded 0.04%, corresponding to 0.4 mg/kg, far below the current maximum limits imposed by the Italian Ministry of Health. This study opens up a new concrete possibility to exploit hemp processing by-products in order to obtain drinks with high added value and paves the way for further in vitro and in vivo investigations aimed at promoting their benefits for human health.

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Implication of Opioid Receptors in the Antihypertensive Effect of a Novel Chicken Foot-Derived Peptide

Biomolecules ◽

10.3390/biom10070992 ◽

2020 ◽

Vol 10 (7) ◽

pp. 992

Author(s):

Anna Mas-Capdevila ◽

Lisard Iglesias-Carres ◽

Anna Arola-Arnal ◽

Gerard Aragonès ◽

Begoña Muguerza ◽

...

Keyword(s):

Mass Spectrometry ◽

High Performance Liquid Chromatography ◽

Liquid Chromatography ◽

Opioid Receptors ◽

High Performance ◽

Antihypertensive Effect ◽

High Resolution Mass Spectrometry ◽

Liquid Chromatography Tandem Mass

The peptide AVFQHNCQE demonstrated to produce nitric oxide-mediated antihypertensive effect. This study investigates the bioavailability and the opioid-like activity of this peptide after its oral administration. For this purpose, in silico and in vitro approaches were used to study the peptide susceptibility to GI digestion. In addition, AVFQHNCQE absorption was studied both in vitro by using Caco-2 cell monolayers and in vivo evaluating peptide presence in plasma from Wistar rats by ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) and by ultra-high performance liquid chromatography-high resolution mass spectrometry (UHPLC-HRMS). Both in vivo and in vitro experiments demonstrated that peptide AVFQHNCQE was not absorbed. Thus, the potential involvement of opioid receptors in the BP-lowering effect of AVFQHNCQE was studied in the presence of opioid receptors-antagonist Naloxone. No changes in blood pressure were recorded in rats administered Naloxone, demonstrating that AVFQHNCQE antihypertensive effect is mediated through its interaction with opioid receptors. AVFQHNCQE opioid-like activity would clarify the antihypertensive properties of AVFQHNCQE despite its lack of absorption.

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Characterization of lacosamide metabolites by UHPLC–ESI–HRMS method

Acta Chromatographica ◽

10.1556/1326.2019.00591 ◽

2020 ◽

Vol 32 (2) ◽

pp. 107-116

Author(s):

Maciej Gawlik ◽

Robert Skibiński ◽

Łukasz Komsta

Keyword(s):

Human Liver ◽

High Performance ◽

High Resolution Mass Spectrometry ◽

Parent Compound ◽

Liver Microsomes ◽

Complementary Technique ◽

Polar Metabolite ◽

Simulation Techniques

In this study, the in vitro phase I metabolism of lacosamide was characterized with the use of ultra-high-performance liquid chromatography combined with high-resolution mass spectrometry (quadrupole time-of-flight). The use of two metabolism simulation techniques (photocatalysis and human liver microsomes) allowed the characterization of a polar metabolite of parent compound, not yet described. The experiment with the participation of HLM gave the ability to describe the full liver metabolic pathway of lacosamide. It has been proven that this molecule undergoes deacetylation, demethylation, and during liver tissue metabolism. Photocatalysis with the use of a TiO2 catalyst was proved to be a complementary technique in mimicking in vitro drug metabolism.

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Study on follicular fluid metabolomics components at different ages based on lipid metabolism

10.21203/rs.2.24602/v2 ◽

2020 ◽

Author(s):

xingxing zhang ◽

tianqi wang ◽

jingyan song ◽

jifeng deng ◽

Zhengao Sun

Keyword(s):

Lipid Metabolism ◽

Follicular Fluid ◽

High Performance ◽

High Resolution Mass Spectrometry ◽

Age Groups ◽

Principal Component ◽

Vitro Fertilization ◽

Different Ages

Abstract Background: Follicular fluid is an important external environment for the growth and development of oocytes. A thorough identification of specific components in follicular fluid can better the existing understand of intracellular signal transduction and reveal potential biomarkers of oocyte health in women undergoing assisted reproductive therapy. To study on follicular fluid metabolomics components at different ages based on lipid metabolism, we have adopted a new method of SWATH to MRM( the sequential window acquisition of all theoretical fragment-ion spectra to multiple reaction monitor)metabolomics to provide extensive coverage and excellent quantitative data. This was done to investigate the differences in follicular fluid of patients undergoing in vitro fertilization (IVF) and embryo transfer in different age groups and to further explore the relationship between follicular fluid, age and reproductive function.Method: A combination of Ultra-high-performance liquid chromatography and high resolution mass spectrometry techniques were used to analyze the follicular fluid of 230 patients enrolled for the IVF cycle. The patients were of different ages grouped into two groups:the younger and older patients.The obtained multidimensional chromatographic data were processed by principal component analysis (PCA) and partial least squares discriminant analysis (PLS-DA). The charge ratios and mass numbers enabled for the identification of different fragments in the samples. Matching information obtained through database search and the fragment information obtained by fragment ion scan structurally identified substances in the samples. This was used to determine the differential compounds.Results:The quality of oocytes decline with age,and the lipid composition in follicular fluid also changes,The lipid metabolism that changes with age may be related to the quality of oocytes.The main differences were in lipid metabolites. Some were up-regulated : Arachidonate, LysoPC(16:1), LysoPC(20:4) and LysoPC(20:3) while others were down-regulated: LysoPC(18:3) and LysoPC(18:1).Conclusions: Metabolomic analysis of follicular fluid revealed that with the increase in age, several differential metabolites are at play. Among these metabolites, lipid metabolism undergoes significant changes that affect the development of oocytes thus causing reduced fertility in older women. These differential metabolites related to follicular development may provide possible detection and treatment targets for promoting oocyte health, and provide scientific basis for understanding the environment of oocyte development.

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Changes in the Organosulfur and Polyphenol Compound Profiles of Black and Fresh Onion during Simulated Gastrointestinal Digestion

Foods ◽

10.3390/foods10020337 ◽

2021 ◽

Vol 10 (2) ◽

pp. 337

Author(s):

Alicia Moreno-Ortega ◽

José Luis Ordóñez ◽

Rafael Moreno-Rojas ◽

José Manuel Moreno-Rojas ◽

Gema Pereira-Caro

Keyword(s):

High Performance ◽

High Resolution Mass Spectrometry ◽

Methionine Sulfoxide ◽

Organosulfur Compounds ◽

Gastrointestinal Digestion ◽

Digestion Process ◽

Simulated Gastrointestinal Digestion ◽

Positive Effect ◽

Cysteine Sulfoxide

This study aims to determine the changes in, and bioaccessibility of, polyphenols and organosulfur compounds (OSCs) during the simulated gastrointestinal digestion of black onion, a novel product derived from fresh onion by a combination of heat and humidity treatment, and to compare it with its fresh counterpart. Fresh and black onions were subjected to in-vitro gastrointestinal digestion, and their polyphenol and OSC profiles were determined by ultra-high-performance liquid chromatography coupled with high-resolution mass spectrometry (UHPLC-HRMS). Although to a lesser extent than in the fresh onion, the phenolic compounds in the black variety remained stable during the digestion process, presenting a higher bioaccessibility index (BI) with recovery corresponding to 41.1%, compared with that of fresh onion (23.5%). As for OSCs, apart from being more stable after the digestion process, with a BI of 83%, significantly higher quantities (21 times higher) were found in black onion than in fresh onion, suggesting that the black onion production process has a positive effect on the OSC content. Gallic acid, quercetin, isorhamnetin, and ɣ-glutamyl-S-(1-propenyl)-L-cysteine sulfoxide were the most bioaccessible compounds in fresh onion, while isorhamnetin, quercetin-diglucoside, ɣ-glutamyl-S-methyl-L-cysteine sulfoxide and methionine sulfoxide were found in black onion. These results indicate that OSCs and polyphenols are more bioaccessible in black onion than in fresh onion, indicating a positive effect of the processing treatment.

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