LC-QTOF MS Research Articles

Effect of In Vitro Gastrointestinal Digestion on the Polyphenol Bioaccessibility and Bioavailability of Processed Sorghum (Sorghum bicolor L. Moench).

Sorghum is a significant source of polyphenols, whose content, antioxidant properties and bioaccessibility may be modulated by digestion. Studies have reported sorghum polyphenol changes after simulated digestion. However, the effects of simulated digestion on processed, pigmented sorghum are unknown. This study investigated the bioaccessibility and bioavailability of black (BlackSs and BlackSb), red (RedBa1, RedBu1, RedBa2, RedBu2) and white (WhiteLi2 and White Li2) sorghum samples using a Caco-2 in vitro model. Ultra high performance liquid chromatography-online 2,2'-azino-bis (3-ethylbenzothiazoline-6-sulfonic acid) (UHPLC-online ABTS)-and quadrupole time-of-flight liquid chromatography mass spectra (QTOF LC-MS) facilitated the identification of digested and transported compounds. Simulated digestion showed increased bioaccessibility and total phenolic content (TPC) for BlackSs by 2-fold. BlackSs and BlackSb exhibited high antioxidant capacities, with variations dependent on processing in other varieties. Kaempferol-3-O-xyloside exhibited a 4-fold increase in TPC following digestion of processed BlackSs and BlackSb but was absent in the others. BlackSs, BlackSb, and RedBu1 revealed twelve bioaccessible and Caco-2 transported compounds not previously reported in sorghum, including trans-pinostilbene, tryptophan and maackin a. This study demonstrates that in vitro digestion increases the bioaccessiblity of sorghum polyphenols through the process of cellular biotransformation, possibly improving transport and bioactivity in vivo.

Phenols, flavonoids and anthocyanins in Solanum lasiocarpum from Borneo: In vitro antioxidant activity and phytochemical profiling via LCMS Q-TOF

Phenols, flavonoids, and anthocyanins are compounds that reported play important roles in plant defence mechanism system. Antioxidant activity is mostly derived from these phytochemical groups, which have a wide range of pharmaceutical properties, including antimicrobial, antitumor, anti-inflammatory, antipyretic, anti-allergy, anti-fertility, hypoglycemic, anti-histamine, antioxidant, antiviral, analgesic, anti-ulcerogenic, nephroprotective, antidiabetic, immuno-secretory, cardiovascular, anti-platelet aggregation, antibacterial, anticancer, and hepatoprotective activities. However, these compounds in Solanum lasiocarpum from Borneo areas are remaining unclear. In this experiment, we performed comprehensive evaluation on effect of extraction solvents on phenols, flavonoids, and anthocyanin's contents and further on the scavenging activity (2,2-diphenyl-1-picrylhydrazyl-hydrate, DPPH; 2,2′-azino-bis(3-ethylbenzthiazoline-6-sulphonic acid), ABTS; and ferric-reducing antioxidant power, FRAP). High phenolic, flavonoid and anthocyanin contents be found in low polar solvent. Antioxidant assay showed acetone was higher activity with IC50 of 6.36 mg/mL compared to methanol (12.1 mg/mL) and hexane (17.8 mg/mL). Furthermore, liquid chromatography mass spectrometry quadrupole-time of flight (LCMS Q-TOF) mass spectrometer detected N-Acryloylglycine, butoctamide hydrogen succinate, eruberin B, emmotin A and N-Cyclohexanecarbonylpentadecylamine that important in natural polymers, serve as sleep disorders treatment agents, anti-fibrotic property, immunomodulatory activity, and act as differentiator between N-palmitoylethanolamine-hydrolyzing acid amidase (NPAA) compared to fatty acid amide hydrolase (FAAH), respectively. The limitation of this research is the assessment of antioxidant properties related to the polarity of the extraction solvent. Polar solvents may exhibit high scavenging activity, but phenolic compounds, flavonoids, and anthocyanins are found in higher concentrations in non-polar solvents. We encourage further investigation into phytochemical profiles due to the abundance from non-polar solvents.

Impact of Processing on the Phenolic Content and Antioxidant Activity of Sorghum bicolor L. Moench.

Sorghum, a cereal grain rich in nutrients, is a major source of phenolic compounds that can be altered by different processes, thereby modulating their phenolic content and antioxidant properties. Previous studies have characterised phenolic compounds from pigmented and non-pigmented varieties. However, the impact of processing via the cooking and fermentation of these varieties remains unknown. Wholegrain flour samples of Liberty (WhiteLi1 and WhiteLi2), Bazley (RedBa1 and RedBa2), Buster (RedBu1 and RedBu2), Shawaya black (BlackSb), and Shawaya short black 1 (BlackSs) were cooked, fermented, or both then extracted using acidified acetone. The polyphenol profiles were analysed using a UHPLC-Online ABTS and QTOF LC-MS system. The results demonstrated that combining the fermentation and cooking of the BlackSs and BlackSb varieties led to a significant increase (p < 0.05) in total phenolic content (TPC) and antioxidant activities, as determined through DPPH, FRAP, and ABTS assays. The 2,2'-azino-bis (3-ethylbenzothiazoline-6-sulfonic acid) (ABTS) radical scavenging activity of WhiteLi1, BlackSb, RedBu2, and BlackSs increased by 46%, 32%, 25%, and 10%, respectively, post fermentation and cooking. Conversely, fermentation only or cooking generally resulted in lower phenolic content and antioxidant levels than when samples were fully processed compared to raw. Notably, most of the detected antioxidant peaks (53 phenolic compounds) were only detected in fermented and cooked black and red pericarp varieties. The phenolic compounds with the highest antioxidant activities in pigmented sorghum included 3-aminobenzoic acid, 4-acetylburtyic acid, malic acid, caffeic acid, and luteolin derivative. Furthermore, the growing location of Bellata, NSW, showed more detectable phenolic compounds following processing compared to Croppa Creek, NSW. This study demonstrates that sorghum processing releases previously inaccessible polyphenols, making them available for human consumption and potentially providing added health-promoting properties.

Simultaneous Detection Method of 11 Respiratory Drug Substances Including Theobromine, Oxymetazoline, etc. in Adulterated Dietary Supplements Using Liquid Chromatography–Electrospray Ionization–Tandem Mass Spectrometry and Liquid Chromatography–Quadrupole Time-of-Flight Mass Spectrometry Analysis

Abstract Recently, the demand for respiratory disease-related products has surged due to the influence of coronavirus disease 2019, prompting warnings about illegal dietary supplements containing unauthorized substances. Additionally, adulterated dietary supplements are continuously detected in open markets, posing significant public health safety problem. In this study, we developed and validated an analytical method for 11 respiratory drug substances using liquid chromatography–electrospray ionization–tandem mass spectrometry (LC–ESI–MS/MS) and proposed optimal conditions for LC–quadrupole time-of-flight MS (LC–QTOF-MS) to determine the fragmentation patterns of each substance. This method underwent thorough validation considering specificity, linearity, limits of detection and quantification, accuracy, precision, matrix effect, stability, etc. All results met international guidelines. These validated methods were applied to 52 dietary supplements advertised for treating respiratory diseases and enhancing respiratory function, among which one sample was found to contain 313.7 mg/g of theobromine. This determination was made by comparing the product ion ratios with the standards and subsequent quantification. To re-confirm the detected substances, their fragmentation patterns were compared with those of the standards using LC–QTOF-MS. In conclusion, the mass-based information, coupled with the LC–ESI–MS/MS method development, can be successfully applied to rapidly identify 11 respiratory drug substances in illegal dietary supplements used for respiratory disease treatment. The developed simultaneous detection method contributes to public health and safety improvements.

EXPLORING THE HAEMOSTATIC POTENTIAL OF PANCHAVALKALA KASHAYA AND PANCHAVALKALA AQUEOUS EXTRACT: AN IN VITRO STUDY

Acharya Susrutha under the context of Rakthasthambhanopaya (methods of haemostasis) has explained about the different methods to attain Rakthasthambhana or haemostasis. which include Skandana (clotting of blood), Santhana (uniting), Pachana (ripening or digestive measures) and Dahana (thermal cauterisation). Acharya Susrutha while explaining about agantuja vrana chikitsa (treatment of wound) has explained that ‘Pittavat sheeta kriya’ should be done prior to santhana to mitigate the ‘Kshatoshmana’. So, from this it is evident the primary method of management should be done with sheeta (cold) followed by Kashaya rasa dravya (astringent taste drugs) for Santhana. Panchavalkala is a group drug with sheeta veerya (cold potency) and Kashaya rasa (astringent taste) mentioned in Dalhana commentary for Skandana. This study investigates the haemostatic effect of Panchavalkala Kashaya and Panchavalkala aqueous extract by in vitro method. Preliminary phytochemical screening of both trial drugs was done. A total of 10 samples of healthy human platelet poor plasma were mixed in trial drugs, Prothrombin and Activated Partial Thromboplastin time were determined. Data was analysed using Kruskal Wallis test. Phytochemical analysis confirmed that the Panchavalkala kashaya contain alkaloids, tannins, glycosides and saponins. Panchavalkala aqueous extract sample consist of flavonoids, alkaloids, glycosides, tannins and saponins. LCMS Q-TOF analysis shows the presence of compounds Gallic acid, Epicatechin, Leucocynidin and Procyanidin B1. And the HPLC study confirmed that Gallic acid is an active phytoconstituent present in the Panchavalkala aqueous extract. In the present study the trial group Panchavalkala aqueous extract showed more desirable haemostatic effect than Panchavalkala Kashaya on comparison.

Bacteria-mediated green synthesis of silver nanoparticles and their antifungal potentials against Aspergillus flavus.

The best biocontroller Bacillus subtilis produced silver nanoparticles (AgNPs) with a spherical form and a 62 nm size through green synthesis. Using UV-vis spectroscopy, PSA, and zeta potential analysis, scanning electron microscopy, and Fourier transform infrared spectroscopy, the properties of synthesized silver nanoparticles were determined. Silver nanoparticles were tested for their antifungicidal efficacy against the most virulent isolate of the Aspergillus flavus fungus, JAM-JKB-BHA-GG20, and among the 10 different treatments, the treatment T6 [PDA + 1 ml of NP (19: 1)] + Pathogen was shown to be extremely significant (82.53%). TG-51 and GG-22 were found to be the most sensitive groundnut varieties after 5 and 10 days of LC-MS QTOF infection when 25 different groundnut varieties were screened using the most toxic Aspergillus flavus isolate JAM- JKB-BHA-GG20, respectively. In this research, the most susceptible groundnut cultivar, designated GG-22, was tested. Because less aflatoxin (1651.15 g.kg-1) was observed, treatment T8 (Seed + Pathogen + 2 ml silver nanoparticles) was determined to be much more effective. The treated samples were examined by Inductively Coupled Plasma Mass Spectrometry for the detection of metal ions and the fungicide carbendazim. Ag particles (0.8 g/g-1) and the fungicide carbendazim (0.025 g/g-1) were found during Inductively Coupled Plasma Mass Spectrometry analysis below detectable levels. To protect plants against the invasion of fungal pathogens, environmentally friendly green silver nanoparticle antagonists with antifungal properties were able to prevent the synthesis of mycotoxin by up to 82.53%.

Leaf extract of Garcinia atroviridis promotes anti-heat stress and antioxidant effects in Caenorhabditis elegans.

Introduction: Garcinia atroviridis has been used for traditional medicines, healthy foods and tea. The chemical compositions and biological activities of fruit, stem bark and root have been widely studied. However, the phytochemical components and the biological activities in Garcinia atroviridis leaves (GAL) are limited. This research aims to study the phytochemical components and the stress resistance effects of GAL in Caenorhabditis elegans (C. elegans). Methods: To investigate the chemical components and antioxidant activities of GAL extract, the ethanol extract was characterized by liquid chromatography-quadrupole time-of-flight mass spectrometry (LC-QTOF MS) analysis and C. elegans was used to evaluate the effects of GAL extracts on longevity and stress resistance. Results and discussion: The results revealed that the ethanol extract of GAL possesses free radical scavenging activities. Furthermore, GAL extract increased the lifespan of C. elegans by 6.02%, 15.26%, and 12.75% at concentrations of 25, 50, and 100μg/mL, respectively. GAL extract exhibited improved stress resistance under conditions of heat and hydrogen peroxide-induced stress. The survival rates of GAL extract-treated worms were significantly higher than those of untreated worms, and GAL extract reduced reactive oxygen species (ROS) accumulation. Additionally, GAL extract treatment upregulated the expression of stress resistance-associated genes, including gst-4, sod-3, skn-1, and hsp16.2. GAL extract supplementation alleviated stress and enhanced longevity by inducing stress-related genes in C. elegans. The observed effects of GAL extracts may be attributed to the stimulation of oxidant enzymes mediated through DAF-16/FOXO and SKN-1/NRF2, as well as the enhancement of thermal defense in C. elegans. Collectively, this study provides the first evidence of the antioxidant activities of GAL and elucidates the underlying mechanisms of stress resistance.

The mixture of Ganoderma lucidum and Cordyceps militaris: Chemical composition and protective effect against oxidative stress

There is a growing demand for the consumption of medicinal mushrooms and their products. Ganoderma lucidum and Cordyceps militaris are two important medicinal mushrooms with significant pharmacological activities. In this study, we aim to develop a preparation of the extracts of these two mushrooms, and investigate its composition, antioxidant activities, and protective effects against oxidative damage. Liquid chromatography equipped with quadrupole time-of-flight mass spectrometry (LC-QTOF MS) was employed to analyze the chemical profiles of the mixture. A total of 94 compounds were identified as belonging to phenolic acids, flavonoids, triterpenes, and nucleosides. In addition, HPLC-DAD was used to quantify major compounds. Ferulic and cinnamic acids were predominant in the phenolic acid groups, with corresponding concentrations of 0.41 and 0.29 mg/g. The concentration of ganoderic acid A was 0.08 mg/g, and the contents of adenosine and cordycepin were 0.53 and 0.14 mg/g, respectively. The mixture could scavenge free radicals and reduce ferric ions in vitro. The preparation also showed nontoxic but proliferative effects on human fibroblast cells. In addition, it could protect fibroblasts against oxidative stress, reducing 21–22% of cell death in the presence of H2O2. These findings provide more information on the applications of medicinal mushrooms in the functional food and pharmaceutical industries.

Biodegradable Mulch Films and Bioformulations Based on Trichoderma sp. and Seaweed Extract Differentially Affect the Metabolome of Industrial Tomato Plants.

The use of biostimulants and biofilms in agriculture is constantly increasing, as they may support plant growth and productivity by improving nutrient absorption, increasing stress resilience and providing sustainable alternatives to chemical management practices. In this work, two commercial products based on Trichoderma afroharzianum strain T22 (Trianum P®) and a seaweed extract from Ascophyllum nodosum (Phylgreen®) were tested on industrial tomato plants (Solanum lycopersicum var. Heinz 5108F1) in a field experiment. The effects of single and combined applications of microbial and plant biostimulants on plants grown on two different biodegradable mulch films were evaluated in terms of changes in the metabolic profiles of leaves and berries. Untargeted metabolomics analysis by LC-MS Q-TOF revealed the presence of several significantly accumulated compounds, depending on the biostimulant treatment, the mulch biofilm and the tissue examined. Among the differential compounds identified, some metabolites, belonging to alkaloids, flavonoids and their derivatives, were more abundant in tomato berries and leaves upon application of Trichoderma-based product. Interestingly, the biostimulants, when applied alone, similarly affected the plant metabolome compared to control or combined treatments, while significant differences were observed according to the mulch biofilm applied.

Characterization of Levan Fructan Produced by a Gluconobacter japonicus Strain Isolated from a Sugarcane Processing Facility.

During raw sugarcane processing, a significant portion of lost sucrose is attributable to microbial degradation. Sucrose consumption by many bacteria is also linked to the production of exopolysaccharides (EPS) such as dextrans and fructans. These resulting EPS cause operational challenges during raw sugar manufacturing. Here, we report the characterization of EPS from a fructan-forming Gluconobacter japonicus bacterium that we previously isolated from a Louisiana sugarcane factory. The genome sequencing revealed the presence of two encoded levansucrase genes, lsrA and lsrB. One levansucrase, LsrB, was detected in the secreted protein fraction of G. japonicus LASM12 by QTOF LC-MS. The spotting assays indicated that G. japonicus produces EPS using sucrose and raffinose as substrates. The G. japonicus EPS correlated with levan fructan commercial standards by 1H-NMR, and with the characteristic carbohydrate fingerprint region for FTIR spectra, confirming that the G. japonicus EPS is levan fructan. The glycosyl composition and glycosyl linkage analysis revealed a linear β-2,6-fructofuranosyl polysaccharide with occasional (5.7%) β-2,1-fructofuranosyl branches. The gel permeation chromatography of the levan fructan EPS showed two main peaks at 4.5 kDa and 8 kDa and a very minor peak at 500 kDa. G. japonicus was identified as a producer of levan fructan. These findings will be useful for future studies aimed at evaluating the impact of levan fructans on sugar crop processing, which have been historically underestimated in industry.

Retention time-independent strategy for screening pesticide residues in herbs based on a fingerprint database and all ion fragmentation acquisition with LC-QTOF MS.

A retention time (RT)-independent strategy for nontargeted screening of pesticide residues in herbs was exploited using liquid chromatography-quadrupole time-of-flight mass spectrometry (LC-QTOF MS). The core of this strategy is a fingerprint database coupled with a data-independent acquisition (DIA) scan mode of all ion fragmentation (AIF). In the fingerprint database, a total of 150 pesticides with quasimolecular ions and fragment ions at five-level collision energies were collected as qualified ions for screening. During the data acquisition, the AIF scan was performed via real unbiased full-spectrum MS/MS acquisition. Six herb matrices spiked with 30 banned pesticides were used to evaluate the applicability of the strategy in real samples. The use of the narrow ion mass extraction window (10 mDa) and the narrow RT window (0.1 min) enabled the effective extraction of spectra from noisy backgrounds and the discovery of suspected pesticides via similarity matching of filtered qualified ions. On average, more than 11/30 of pesticides at 1 ng mL-1 and more than 23/30 of pesticides at 10 ng mL-1 or lower could be screened out in each matrix using at least two qualified ions. In addition, the AIF mode exhibited superior anti-interference capability compared to data-dependent acquisition (DDA) and sequential window acquisition of all theoretical mass spectra (SWATH), as determined by comparing the limits of screening (LOSs) of 30 banned pesticides spiked into Isatidis Folium. Finally, the developed strategy was applied to screen pesticide residues in extracts of Ganoderma and Foeniculi Fructus. Phorate-sulfone and phorate-sulfoxide were found in Ganoderma, as well as terbufos-sulfone and terbufos-sulfoxide were found in Foeniculi Fructus. In conclusion, the developed RT-independent strategy based on a fingerprint database and AIF acquisition with LC-QTOF MS seems to be one of the most efficient tools for the analysis of nontargeted pesticide residues in complicated matrices.

Metabolites from a Pleurotus tuber-regium collected in Madagascar

Pleurotus tuber-regium was isolated from a dead trunk of Raphia farinifera (Arecaceae) in a lowland moist forest in Antsohihy, Madagascar, and the species was confirmed by molecular analysis and morphological observations. The main bioactive metabolites of the mycelium extracts were identified by mass spectrometry techniques. Five structural diverse metabolites, tryptophol, pyroglutamic acid, prolyldiketopiperazine B, sporol and RKS-1778, were characterised by LC-MS qTOF analysis of the hydro-alcoholic extract. GC-MS analysis of both chloroform and ethyl acetate extracts revealed the presence of several saturated and ­unsaturated fatty acids and their esters derivatives.

Reaction mechanism, degradation pathway and toxicity assessment of NH4+ enhanced potassium ferrate removal of levofloxacin

Considering that ammonium ion (NH4+) was widely distributed in natural water and many sewage, it was of great practical significance to study NH4+ enhanced potassium ferrate (Fe(VI)) to rapid removal of levofloxacin (LEV) from water. In this experiment, firstly, the reaction kinetic of NH4+ enhanced Fe(VI) removal of LEV was studied, and the results showed that the enhanced removal reaction conformed to the second-order kinetic equation. When pH ≤ 9, the second-order rate constant kapp was linearly related to NH4+ dosage, but when pH= 10, the above linear relationship was broken, and the slope of the fitting line would change toward a smaller trend. Subsequently, tert-butanol (TBA) and Methyl phenyl sulfoxide (PMSO) were used as probes for·OH and high-valent iron-based intermediate (Fe(V)/Fe(IV)) respectively, which further revealed the reaction mechanism that NH4+ enhanced Fe(VI) to remove LEV as follows: NH4+ could promote Fe(VI) to produce a large amount of Fe(V)/Fe(IV), thus accelerating the degradation of LEV. In addition, 10 degradation intermediates of LEV were identified by quadrupole time-of-flight tandem ultra-performance liquid chromatography mass spectrometer (Q-TOF LC-MS), and then combined with density functional theory (DFT) calculation, two possible degradation pathways were inferred. Through the luminescence inhibition experiment of Vibrio fischeri and the toxicity evaluation of ECOSAR, it could be concluded that in the process of NH4+ enhancing Fe(VI) to remove LEV, the toxicity of the solution showed a trend of increasing first and then decreasing, and its toxicity was effectively improved and reduced after full oxidation. Finally, the experiments in actual water showed that it was feasible to use NH4+ in actual water to enhance Fe(VI) for rapid removal of LEV.

Extracting Structural Information from Physicochemical Property Measurements Using Machine Learning─A New Approach for Structure Elucidation in Non-targeted Analysis.

Non-targeted analysis (NTA) has made critical contributions in the fields of environmental chemistry and environmental health. One critical bottleneck is the lack of available analytical standards for most chemicals in the environment. Our study aims to explore a novel approach that integrates measurements of equilibrium partition ratios between organic solvents and water (KSW) to predictions of molecular structures. These properties can be used as a fingerprint, which with the help of a machine learning algorithm can be converted into a series of functional groups (RDKit fragments), which can be used to search chemical databases. We conducted partitioning experiments using a chemical mixture containing 185 chemicals in 10 different organic solvents and water. Both a liquid chromatography quadrupole time-of-flight mass spectrometer (LC-QTOF MS) and a LC-Orbitrap MS were used to assess the feasibility of the experimental method and the accuracy of the algorithm at predicting the correct functional groups. The two methods showed differences in log KSW with the QTOF method showing a mean absolute error (MAE) of 0.22 and the Orbitrap method 0.33. The differences also culminated into errors in the predictions of RDKit fragments with the MAE for the QTOF method being 0.23 and for the Orbitrap method being 0.31. Our approach presents a new angle in structure elucidation for NTA and showed promise in assisting with compound identification.

Unique green chromatographic method for the qualitative and quantitative analysis of ketoconazole, its impurities and preservatives from ketoconazole cream formulation: Identification of degradants by Q-ToF LCMS and Robustness by Design of Experiments

Current research portrays a simultaneous determination method for the qualitative and quantitative analysis of Ketoconazole, its impurities and preservatives from Ketoconazole cream formulation. The unique method was developed using the RP-UPLC technique with a gradient elution mode. The separation of isomeric preservative components was achieved on the Waters Acquity UPLC BEH C18 column using phosphate buffer as mobile phase A and a mixture of phosphate buffer and acetonitrile, 30:70 (v/v) as mobile phase B. The set flow rate, injection volume, column oven temperature, and detector wavelengths were 0.5 mL/min, 2.0 μL, 30 °C, and 225 nm, respectively. The method's stability indicating nature was achieved through forced degradation studies. The active drug was prone to acidic and oxidative conditions. The attained acidic and peroxide degradant peaks were identified using Q-ToF LCMS. The developed method was validated per regulatory guidelines, and the data showed superior precision with a %RSD of 0.7 for Ketoconazole, 0.8 for preservatives, and 1.6 for impurities. All the components showed excellent linearity (r > 0.999) within the 50–150% range for Ketoconazole and preservatives and from LOQ to 150% for impurities. The mean accuracy data resulted from 99.4% to 99.9% for Ketoconazole, 99.9%–106.0% for impurities, and 100.3%–101.4% for butylated hydroxyanisole. The robust method conditions were evaluated by the Design of Experiments. The greenness and eco-friendliness of the method were demonstrated by modern tools such as the analytical eco scale, GAPI and AGREE. The final UPLC method is specific and suitable for determining the preservatives, drug content and impurities of Ketoconazole simultaneously from its cream formulation, which saves analysis time and solvent consumption supporting towards the green chemistry principles.

Identification of isomeric labdane diterpenoids from rhizomes of Alpinia purpurata by Q-TOF LCMS

The hexane and dichloromethane sub-fractions prepared from extracts of Alpinia purpurata (Vieill.) K. SCHUM rhizomes using Vacuum Liquid Chromatography (VLC) and Radial Chromatography (RC) were subjected to qualitative LCMS analysis. A total of thirteen labdane diterpenoid compounds with various pharmacological activities were identified through correlation of their molecular ion peaks at m/z [M + H] +, retention time and molecular formula with those labdane diterpenoids isolated from another Zingiberaceae plant. The result of the LCMS analysis indicated that A. purpurata rhizome has more labdane diterpenoid compounds other than those few reported.

Classifying micropollutants by environmental risk in groundwater using screening analysis associated to a hybrid multicriteria method combining (Q)SAR tools, fuzzy AHP and ELECTRE

This study aimed to evaluate and monitor pesticides in groundwater of the Serra Geral aquifer, located in the Paraná Basin 3 (southern Brazil), using Liquid Chromatography coupled with a Quadrupole-Time-of-Flight Mass Spectrometer (LC-QTOF MS). A total of 117 samples, collected in three different moments, were analyzed over 36 months. Groundwater samples from 35 wells and four surface water points were monitored in each sampling campaign. A pesticide screening methodology was proposed with the tentative identification of 1607 pesticides and pesticide metabolites. The application of the proposed methodology resulted in the verification of 29 pesticides and pesticide metabolites, 7 as confirmed analytes and 22 as suspect compounds. (Q)SAR in silico predictions and GUS index calculation provided data on the potential environmental risk of the identified compounds, with eight endpoints considered. After in silico predictions, an alternative hybrid multicriteria method was applied, combining the weighting of endpoints of fuzzy AHP and micropollutants classification by environmental risk using ELECTRE. The fuzzy AHP results indicated the greatest importance of mutagenicity among the eight evaluated indicators, while the scarce influence of the physicochemical properties on the environmental risk suggested their exclusion from the model. Accordingly, the ELECTRE results highlighted the prevalence of thiamethoxam and carbendazim as the most dangerous for the environment. The application of the proposed method enabled the selection of the compounds that must be monitored, considering mutagenicity and toxicity predictions for environmental risk analysis.

Optimization of a Green Microwave-Assisted Extraction Method to Obtain Multifunctional Extracts of Mentha sp.

A microwave-assisted extraction (MAE) procedure has been optimized to simultaneously provide multifunctional extracts of Mentha sp. leaves with improved antioxidant properties and, for the first time, with optimal antimicrobial activity. Among the solvents evaluated, water was selected as the extractant in order to develop a green procedure and also for its improved bioactive properties (higher TPC and Staphylococcus aureus inhibition halo). MAE operating conditions were optimized by means of a 3-level factorial experimental design (100 °C, 14.7 min, 1 g of dry leaves/12 mL of water and 1 extraction cycle), and further applied to the extraction of bioactives from 6 different Mentha species. A comparative LC-Q MS and LC-QToF MS analysis of these MAE extracts was carried out for the first time in a single study, allowing the characterization of up to 40 phenolics and the quantitation of the most abundant. Antioxidant, antimicrobial (Staphylococcus aureus, Escherichia coli and Salmonella typhimurium) and antifungal (Candida albicans) activities of MAE extracts depended on the Mentha species considered. In conclusion, the new MAE method developed here is shown as a green and efficient approach to provide multifunctional Mentha sp. extracts with an added value as natural food preservatives.

The Predictive Ability of Total Genotype Score and Serum Metabolite Markers in Power-Based Sports Performance Following Different Strength Training Intensities — A Pilot Study

Muscular power is one of the factors that contribute to an athlete’s performance. This study aimed to explore the predictive ability of total genotype score (TGS) and serum metabolite markers in power-based sports performance following different strength training (ST) intensities. We recruited 15 novice male field hockey players (age = 16.27 ± .12 years old, body mass index = 22.57 ± 2.21 kg/m2) and allocated them to; high-intensity strength training (HIST, n=5), moderate intensity strength (MIST, n=5), and control group (C, n=5). Both training groups completed an eight-week ST intervention. Pre- and post-training muscular power (vertical jump) was measured. The participants were genotyped for; ACE (rs1799752), ACTN3 (rs1815739), ADRB3 (rs4994), AGT (rs699), BDKRB2 (rs1799722), PPARA (rs4253778), PPARGC1A (rs8192678), TRHR (rs7832552), and VEGF (rs1870377). TGS was calculated to annotate for strength-power (STP) and endurance (END) qualities. Subsequently, serum metabolomics analysis was conducted using Liquid chromatography-mass spectrometry Quadrupole-Time-of-Flight (LC-MS QTOF) to profile differentially expressed metabolite changes induced by training. Multiple regression analysis was conducted to explore the ability of TGS and differentially expressed metabolite markers to predict muscular power changes following the intervention. Multiple Regression revealed that only TGS STP might be a significant predictor of muscular power changes following MIST (adjusted R2=.906, p&lt;.05). Additionally, ST also resulted in significant muscular power improvement (p&lt;.05) and perturbation of the sphingolipid metabolism pathway (p&lt;.05). Therefore, selected gene variants may influence muscular power. Therefore, STP TGS might be able to predict muscular power changes following MIST.

Novel Plant-Protein (Quinoa) Derived Bioactive Peptides with Potential Anti-Hypercholesterolemic Activities: Identification, Characterization and Molecular Docking of Bioactive Peptides

Hypercholesterolemia remains a serious global public health concern. Previously, synthetic anti-hypercholesterolemic drugs were used for ameliorating this condition; however, long-term usage presented several side-effects. In this regard, natural products as an adjunct therapy has emerged in recent times. This study aimed to produce novel bioactive peptides with anti-hypercholesterolemic activity (cholesterol esterase (CEase) and pancreatic lipase (PL)) from quinoa protein hydrolysates (QPHs) using three enzymatic hydrolysis methods (chymotrypsin, protease and bromelain) at 2-h hydrolysis intervals (2, 4, and 6 h). Chymotrypsin-generated hydrolysates showed higher CEase (IC50: 0.51 mg/mL at 2 h) and PL (IC50: 0.78 mg/mL at 6 h) inhibitory potential in comparison to other derived hydrolysates and intact quinoa proteins. Peptide profiling by LC-MS QTOF and in silico interaction with target enzymes showed that only four derived bioactive peptides from QPHs could bind in the active site of CEase, whereas twelve peptides could bind in the active site of PL. Peptides QHPHGLGALCAAPPST, HVQGHPALPGVPAHW, and ASNLDNPSPEGTVM were identified to be potential CEase inhibitors, and FSAGGLP, QHPHGLGALCAAPPST, KIVLDSDDPLFGGF, MFVPVPH, and HVQGHPALPGVPAHW were identified as potential PL inhibitors on the basis of the maximum number of reactive residues in these bioactive peptides. In conclusion, QPHs can be considered as an alternative therapy for the treatment of hypercholesterolemia.