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Excess molar volume, excess isentropic compressibility, deviation in viscosity, and excess Gibbs free energy of activation for viscous flow for binary mixtures of N-Methyl benzyl amine (NMBA) with 2-Methyl-2-butanol (2M2B), 2-Methyl-1-butanol (2M1B), and 3-Methyl-1-butanol (3M1B) were determined from measured densities (ρ), viscosities (η) and speeds of sound (u) at 303.15 K to 313.15 K. Influence Structural disparities on excess properties is discussed concerning intermolecular forces. The Prigogine – Flory – Patterson (PFP) theory identifies predominant molecular interactions, and the Jouyban – Acree model correlates density, speed of sound, and viscosity with composition. Thermodynamic activation parameters were calculated using the Eyring equation to study viscous flow thermodynamics. FT-IR and 1H NMR spectra of equimolar binary mixtures were analysed to confirm experimental findings through absorption bands (cm−1) and chemical shifts. [ABSTRACT FROM AUTHOR]

As a salt-type compound, mosapride citrate's metabolism and side effects are correlated with its salt-forming ratio. Several techniques were developed in this work to compare various quantitative nuclear magnetic resonance (qNMR) methodologies and to quantitatively examine the content of raw materials. Among the qNMR techniques, methods for 1H NMR and 19F NMR were developed. Appropriate solvents were chosen, and temperature, number of scans, acquisition time, and relaxation delay parameter settings were optimized. Maleic acid was chosen as the internal standard in 1H NMR, and the respective characteristic signals of mosapride and citrate were selected as quantitative peaks. The internal standard in 19F NMR analysis was 4,4′-difluoro diphenylmethanone, and the distinctive signal peak at −116.15 ppm was utilized to quantify mosapride citrate. The precision, repeatability, linearity, stability, accuracy, and robustness of the qNMR methods were all validated according to the ICH guidelines. By contrasting the outcomes with those from high-performance liquid chromatography (HPLC), the accuracy of qNMR was assessed. As a result, we created a quicker and easier qNMR approach to measure the amount of mosapride citrate and evaluated several qNMR techniques to establish a foundation for choosing quantitative peaks for the qNMR method. Concurrently, it is anticipated that various selections of distinct quantitative objects will yield the mosapride citrate salt-forming ratio. [ABSTRACT FROM AUTHOR]

Introduction: Breeding for oil palm resistance against basal stem rot caused by Ganoderma boninense is challenging and time-consuming. Advanced oil palm gene pools are very limited, hence it is assumed that parental palms have experienced genetic drift and lost their resistance genes against Ganoderma. High-throughput selection criteria should be developed. Metabolomic analysis using 1H nuclear magnetic resonance (NMR) spectroscopy is easy, and the resulting metabolite can be used as a diagnostic tool for detecting disease in various host-pathogen combinations. Objectives: The objective of this study was to identify metabolite variations in Dura (D) and Pisifera (P) parental palms with different resistance levels against Ganoderma and moderately resistant DxP using 1H NMR analysis. Methods: Leaf tissues of seven different oil palm categories consisting of: resistant, moderate, and susceptible Dura (D); moderate and susceptible Pisifera (P); resistant Tenera/Pisifera (T/P) parental palms; and moderately resistant DxP variety progenies, were sampled and their metabolites were determined using NMR spectroscopy. Results: Twenty-nine types of metabolites were identified, and most of the metabolites fall in the monosaccharides, amino acids, and fatty acids compound classes. The PCA, PLS-DA, and heatmap multivariate analysis indicated two identified groups of resistance based on their metabolites. The first group consisted of resistant T/P, moderate P, resistant D, and moderately resistant DxP. In contrast, the second group consisted of susceptible P, moderate D, and susceptible D. Glycerol and ascorbic acid were detected as biomarker candidates by OPLS-DA to differentiate moderately resistant DxP from susceptible D and P. The pathway analysis suggested that glycine, serine, and threonine metabolism and taurine and hypotaurine metabolism were involved in the oil palm defense mechanism against Ganoderma. Conclusion: A metabolomic study with 1H NMR was able to describe the metabolite composition that could differentiate the characteristics of oil palm resistance against basal stem rot (BSR) caused by G. boninense. These metabolites revealed in this study have enormous potential to become support tools for breeding new oil palm varieties with higher resistance against BSR. [ABSTRACT FROM AUTHOR]

This study aimed to assess the applicability of solution-state 1H NMR for molecular-level characterization of siRNA-loaded lipid nanoparticles (LNP). Dilinoleylmethyl-4-dimethylaminobutyrate (DLin-MC3-DMA, MC3) was used as an ionizable lipid, and siRNA-loaded LNPs were prepared by pre-mixing and post-mixing methods. The pre-mixing method involved mixing an acidic solution containing siRNA with an ethanolic lipid solution using a microfluidic mixer. The pre-mixed LNP was prepared by dialyzing the mixed solution into the phosphate buffered saline (PBS, pH 7.4). The post-mixed LNP was prepared by mixing the siRNA solution with empty LNP in an acidic condition with and without ethanol, resulting in post-mixed LNP (A) and (B), respectively. Both pre-mixed and post-mixed LNPs formed LNP particles with an average diameter of approximately 50 nm. Moreover, the ratio of encapsulated siRNA to lipid content in each LNP particle remained constant regardless of the preparation method. However, small-angle X-ray scattering measurements indicated structural variations in the siRNA-MC3 stacked bilayer structure formed in the LNPs, depending on the preparation method. Solution-state 1H NMR analysis suggested that the siRNA was incorporated uniformly into the LNP core for pre-mixed LNP compared to post-mixed LNPs. In contrast, the post-mixed LNPs contained siRNA-empty regions with local enrichment of siRNA in the LNP core. This heterogeneity was more pronounced in post-mixed LNP (B) than in post-mixed LNP (A), suggesting that ethanol facilitated the homogeneous mixing of siRNA with LNP lipids. The silencing effect of each siRNA-loaded LNP was reduced in the order of pre-mixed LNP, post-mixed LNP (A), and post-mixed LNP (B). This suggested that the heterogeneity of the siRNA-loaded LNP could cause a reduction in the silencing effect of the incorporated siRNA inside LNPs. The present study highlighted that NMR-based characterization of siRNA-loaded LNP can reveal the molecular-level heterogeneity of siRNA-loaded LNP, which helps to optimize the preparation conditions of siRNA-loaded LNP formulations. [Display omitted] [ABSTRACT FROM AUTHOR]

Global exploration of nanoparticles as nano-fertilizers/nano-fungicides to optimize crop production has attracted greater attention. Among metal oxide nano-formulations, the increasing application and discharge of copper oxide nanoparticles (CuO-NPs) into the environment requires urgent attention due to their toxic and stimulatory impact on plants, including vegetables. This study aimed at the bio-fabrication of CuO-NPs from Rosa indica petal extracts and to assess their nanotoxicity on germination and biological and biochemical growth of tomato plants. The morphological characterization of phytofabricated CuO-NPs by microscopic (SEM/TEM) and spectroscopic (XRD/FTIR) techniques revealed its nanostructure, spherical shape ranging in size between 23 and 47 nm exhibiting different functional groups. Furthermore, tomato-CuO-NPs interactions resulted in reduced germination percentage and plant biomass. At the biochemical level, the chlorophyll content decreased consistently, while malonaldehyde and proline content in tomato foliage enhanced substantially with increasing concentrations of CuO-NPs. Size, lycopene content (71 % reduction), and fruit quality (metabolites like sugars, amino acids, and organic acids) assessed by 1H NMR declined after CuO-NPs exposure in a dose-dependent manner. Further in situ experiments revealed deformation in a stomatal aperture in leaves and accumulation of CuO-NPs in roots, suggesting toxicity under SEM. In summation, this study highlights the toxicity of biosynthesized CuO-NPs to tomato plants paving the way to develop novel strategies to mitigate its toxicity to vegetable crops, particularly tomato under real field conditions. [Display omitted] • Copper oxide nanoparticles (CuO-NPs) exhibit toxic and stimulatory effects on plants. • Biogenic synthesized CuO-NPs from Rosa indica petal extract shows phytotoxicity to tomato plants. • Exposure to CuO-NPs reduces germination percentage, plant biomass, and fruit quality. • Metal oxide nanoparticles increase malondialdehyde and proline content after CuO-NPs exposure. • Strategies need to be developed to counteract nano-CuO toxicity. [ABSTRACT FROM AUTHOR]

Mitomycin C (MMC) has an antitumor effect and is considered as a broad‐spectrum antibiotic. Sijunzi Decoction (SJZD), a well‐known ancient Chinese prescription, is widely used in the treatment of cancer when combined with chemotherapy drugs. Studies have shown that SJZD can be combined with other drugs to enhance the therapeutic effect against cancer and inhibit the toxicity of chemotherapy drugs, but the specific mechanism is not clear. Thus, we hope to further explore the antitumor mechanism of combined SJZD and MMC. 3‐(4,5‐Dimethyl‐2‐thiazolyl)‐2, 5‐diphenyl‐2‐H‐tetrazolium bromide assay, flow cytometry, western blot, 1H NMR and HPLC–MS were used to study the mechanism at the cellular level. The results show that the combined administration can have a more significant effect on inhibiting the proliferation of cancer cells, promoting their apoptosis. Based on metabolomics, 38 biomarkers were found in the MMC group and 43 biomarkers were found in the combined administration group. Among them, 18 unique biomarkers were discovered in the combined administration group. Studies have shown that the antitumor mechanism of combined administration is related to amino acid metabolism, energy metabolism, lipid metabolism and nucleotide metabolism, among which amino acid metabolism is the most important. In addition, SJZD achieves the effect of toxin reduction and efficiency enhancement by improving the body's immunity and improving the oxidative stress environment. [ABSTRACT FROM AUTHOR]

Traditional Mexican medicine commonly uses infusions of Ternstroemia spp. to treat insomnia, injuries, and infections. The antibacterial activities of Ternstroemia dentisepala and Ternstroemia lineata were evaluated for the first time against a panel of Gram-positive and Gram-negative bacteria that have implications for human health, including Enterococcus faecalis, Streptococcus agalactiae, Streptococcus pyogenes, Salmonella typhi, Pseudomonas aeruginosa, and Vibrio parahaemolyticus. Furthermore, the scavenging potential of the hydroalcoholic (HAEs) and total phenolic extracts (TPEs) from the leaves of both plants by a 2,2'-azino-bis(3-ethylbenzothiazoline-6-sulfonic acid) assay (ABTS•+) was determined. Also, the total phenolic contents of the HAEs using the Folin–Ciocalteu reagent were assayed. T. dentisepala HAE and TPE were active against all bacterial strains tested, with a minimum inhibitory concentration between 1.0 and 6.0 mg/mL, with the last one being the most active. However, the T. lineata extracts only demonstrated effectiveness against S. typhi and P. aeruginosa. The TPEs from T. dentisepala and T. lineata improved the activity by approximately 30% in all bacteria tested in comparison with the HAEs. The T. dentisepala HAE had a higher total phenolic content than the T. lineata extract, which was consistent with its ABTS•+-scavenging activity. The two HAEs had different chemical profiles, mostly because of the types and amounts of phenolic compounds they contained. These profiles were obtained using thin-layer chromatography (TLC), high-performance liquid chromatography (HPLC), and proton nuclear magnetic resonance (1H NMR) experiments. [ABSTRACT FROM AUTHOR]

Abstract Background Schizophrenia (SCZ) is a severe mental disorder of multifactorial origin in which the role of amino acids is relatively unknown. Based on the hypothesis that there is an imbalance in amino acid levels in individuals with SCZ compared with healthy controls (HCs), the aim of this study was to identify the 20 proteinogenic amino acids involved in protein synthesis. Methods This study included 43 sex‐ and age‐matched individuals: 20 HCs and 23 with SCZ diagnosed using the Diagnostic and Statistical Manual of Mental Disorders criteria. Using proton nuclear magnetic resonance, we identified the serum levels of the 20 amino acids proteinogenic. We perform multivariate statistical exploratory analyzes to identify compounds, quantify, and identify the main biomarkers of SCZ. Results We identified the serum levels of 19 of the 20 amino acids. Cysteine, the main precursor of glutathione, was not detected. Multivariate exploratory analysis identified lysine, Tryptophan (TRP), and glutamate as possible biomarkers of SCZ. Both lysine and TRP levels were lower and glutamate levels were higher in individuals with SCZ than in HCs. The observed reduction in plasma TRP levels in SCZ was attributed to the activation of the kynurenine pathway and has implications for serotonin synthesis. A strong positive correlation was observed between lysine and TRP, and a weak negative correlation between lysine and glutamate. This result is consistent with the lysine catalysis process because lysine degradation generates glutamate and favors an increase in dopamine. Conclusions The results are consistent with the lysine catalysis process because lysine degradation generates glutamate and favors an increase in dopamine. We were unable to identify any studies suggesting a relationship between lysine catabolism and SCZ pathophysiology, but we recognize this association as innovative.

Freezing is essential for the stability of biological drug substances and products, particularly in frozen solution formulations and during the primary drying of lyophilized preparations. However, the unfrozen segment within the frozen matrix can alter solute concentration, ionic strength, and stabilizer crystallization, posing risks of increased biophysical instability and faster chemical degradation. While quantifying the unfrozen water content is important for designing stable biopharmaceuticals, there is a lack of analytical techniques for in situ quantitative measurements. In this study, we introduce a 1H magic angle spinning NMR technique to identify the freezing point (T ice) and quantify mobile water content in frozen biologics, applying this method to analyze the freezing of a commercial high-concentration drug product, Dupixent®. Our results demonstrate that water freezing is influenced by buffer salt properties and formulation composition, including the presence of sugar cryoprotectants and protein concentration. Additionally, the 1H chemical shift can probe pH in the unfrozen phase, potentially predicting the microenvironmental acidity in the frozen state. Our proposed methodology provides fresh insights into the analysis of freeze-concentrated solutions, enhancing our understanding of the stability of frozen and lyophilized biopharmaceuticals. [Display omitted] [ABSTRACT FROM AUTHOR]

The present study was undertaken to extract chitin and chitosan from crab shell waste and investigate the chemical structure and antioxidant abilities by in vitro assays. Chitin was extracted, chitosan conversion was performed by chemical methods, and the yield was found to be 21%. Several active functional groups, NH primary and secondary amines, amides, and acetyl groups with different bond stretching were conformed in FT-IR spectral analysis. In the proton NMR, N-acetyl glucosamine and H-2 proton of glucosamine (GlcN) residues were identified in chitosan. The antioxidant activities were realized by dose dependent and the maximum activity was found 62, 71, and 58% in higher concentrations of DPPH, hydroxyl, and ferrous ion chelating effects. The derived chitosan is a nontoxic polymer with high chelating capability a good source for functional foods from sustainable source of marine waste. [ABSTRACT FROM AUTHOR]

Early NMR studies of several heterohelicenes containing an annular nitrogen atom and a thiophene ring in their structure suggested the possibility of the lengthening of the carbon–carbon bonds in the interior of the helical turn of the molecule based on the progressive upfield shift of 13C resonances toward the center of the helical turn. We now report a comprehensive analysis of the optimized geometry and a comparison of the calculated vs. observed 1H and 13C NMR chemical shifts of nineteen representative benzothienoquinoline heterohelicenes. As was initially hypothesized on the basis of the progressive upfield shift of carbon resonances toward the center of the interior helical turn, the present computational study has demonstrated that carbon–carbon bonds indeed have more sp3 character and are longer than normal sp2 bonds to accommodate the helical twist of the molecule, as expected. [ABSTRACT FROM AUTHOR]

Herein, the classic organic chemistry experiment titled "Determination of Ethyl Acetoacetate Tautomers by 1H Nuclear Magnetic Resonance" was redesigned to enhance its scope and depth. This new experiment goes beyond simply recognizing the keto-enol tautomeric phenomenon. It delves into the kinetics, the impact of substituents, and the influence of solvents on the keto-enol tautomerization. It's worth noting that the hydrogen-deuterium exchange phenomenon can be observed, providing valuable insights into the ketone-enol tautomeric mechanism. This wellcrafted experiment is designed for senior undergraduate students pursuing chemistry-related majors. It not only deepens their comprehension of ketone properties but also fosters expertise in utilizing nuclear magnetic resonance spectroscopy in the field of organic chemistry. This, in turn, solidifies their theoretical knowledge in organic chemistry and instrumental analysis and hones their problem-solving and analytical skills. [ABSTRACT FROM AUTHOR]

In most cases, the number of honeybee stings received by the body is generally small, but honeybee stings can still cause serious allergic reactions. This study fully simulated bee stings under natural conditions and used 1H Nuclear Magnetic Resonance (1H NMR) to analyze the changes in the serum metabolome of Sprague–Dawley (SD) rats stung once or twice by honeybees to verify the impact of this mild sting on the body and its underlying mechanism. The differentially abundant metabolites between the blank control rats and the rats stung by honeybees included four amino acids (aspartate, glutamate, glutamine, and valine) and four organic acids (ascorbic acid, lactate, malate, and pyruvate). There was no separation between the sting groups, indicating that the impact of stinging once or twice on the serum metabolome was similar. Using the Principal Component Discriminant Analysis (PCA-DA) and Variable Importance in Projection (VIP) methods, glucose, lactate, and pyruvate were identified to help distinguish between sting groups and non-sting groups. Metabolic pathway analysis revealed that four metabolic pathways, namely, the tricarboxylic acid cycle, pyruvate metabolism, glutamate metabolism, and alanine, aspartate, and glutamate metabolism, were significantly affected by bee stings. The above results can provide a theoretical basis for future epidemiological studies of bee stings and medical treatment of patients stung by honeybees. [ABSTRACT FROM AUTHOR]

Lipid oxidation deteriorates the sensory and nutritional quality of food emulsions containing polyunsaturated fatty acids. Classically, different extraction solvents are used as a first step to measure lipid oxidation in emulsions. However, it is unclear how the applied extraction method influences the measured lipid oxidation values. In this work, we systematically examined the performance of common solvent mixtures such as chloroform, methanol, and hexane (or isooctane)–isopropanol on lipid extraction from emulsions stabilized with different emulsifiers (Tween 20 (T20), whey proteins, and pea proteins) and oxidation levels, and how this, in turn, affected the measured hydroperoxide concentrations. Chloroform–methanol was the most effective solvent (lipid yield >93 wt.%). When using hexane–isopropanol, extraction yields were consistently high for T20‐ and pea protein‐based emulsions (>60 wt.%), but in whey protein‐based emulsions, values as low as 26 wt.% were measured. In case of incomplete extraction, hydroperoxide concentrations measured by colorimetric methods need to be corrected for this effect. When using 1H NMR to assess lipid oxidation, the actual amount of extracted lipids is intrinsically taken into account. This highlights not only the importance of the extraction method in determining lipid oxidation in emulsions but also that of the actual analysis method. Practical application: This study highlights that the lipid extraction yield can vary depending not only on the emulsion composition (e.g., type of emulsifier) but also on the oxidative state of the emulsion and the extraction solvent used. If this is overlooked, errors can be made in the hydroperoxide determination. Although these effects can be corrected for, this is not standard procedure, which implies that awareness on this matter should be increased. It is also important to point out that depending on the solvent used, the different lipid classes (including various lipid oxidation products) may be extracted at different levels. Chloroform–methanol should be preferred for extraction of all lipid and lipid oxidation‐derived molecules, including aldehydes. [ABSTRACT FROM AUTHOR]

Background: Malignant pleural effusion (MPE) is a common complication of non-small cell lung cancer (NSCLC). Patients with NSCLC exhibit a high rate of epidermal growth factor receptor (EGFR) mutations. The detection of EGFR mutations is usually time-consuming and costly. This study aimed at identifying potential biomarkers of EGFR mutations in MPE of NSCLC patients by metabolomics. Methods: In total, 58 MPE samples from 30 EGFR mutant and from 28 wild-type NSCLC patients were collected and analyzed by using hydrogen nuclear magnetic resonance (1H NMR) based metabolomics and UPLC-MS/MS based amino acid analysis. Results: Our 1H NMR study showed a significant increase in the lysine levels but a significant decrease in the alanine levels in MPE of NSCLC patients with EGFR-mutant. Twelve amino acids in MPE were further determined by UPLC-MS/MS. It showed that alanine in MPE (6.34 ± 1.88 vs. 8.73 ± 3.68) were significantly decreased and leucine (3.13 ± 0.57 vs. 2.22 ± 0.13), lysine (2.19 ± 0.50 vs. 1.53 ± 0.40), and tyrosine (2.69 ± 0.71 vs. 1.89 ± 0.46) were increased in the EGFR mutation group; leucine (2.19 ± 0.50 vs. 1.53 ± 0.40), methionine (2.19 ± 0.50 vs. 1.53 ± 0.40), and threonine (2.19 ± 0.50 vs. 1.53 ± 0.40) in MPE were significantly lower in the EGRF 19 mutation compared with 21 mutation patients. The area under the receiver operating characteristic curve of 0.851 and 0.931 would be achieved by the logistic model for classification of EGFR-mutant patients from the wild-type controls or the exon 19 from exon 21 mutant patients. Conclusions: Amino acids in MPE are significantly altered and helpful in the diagnosis of EGFR-mutant patients from the wild-type controls or the exon 19 from exon 21 mutant patients with high accuracy, which is worthy of further study. [ABSTRACT FROM AUTHOR]

Polyacrylamide (PAM) is one of the widely used flocculant of cement-based materials, and its degradation products are potentially toxic to the environment. However, few studies have explored the degradation and leakage behavior. Here, these experiments on the total organic carbon, 1H nuclear magnetic resonance, infrared spectroscopy, gel permeation chromatography and gas chromatography–mass spectrometry were carried out to insight into this behavior. The results show that the leakage ratio of PAM from cement paste decreases with the extension of cement hydration time. This flocculant exhibits degradation behavior, the molecular weight of leaked PAM decreases and its amide group and carboxyl group reduce with the prolongation of hydration time. The degradation products of PAM in cement after 70 d contain a variety of small molecular weight organic compounds, such as aldehydes, alcohols, phenols and esters. PAM can definitely degrade and leak from cement-based materials, and the degradation products may contain potentially toxic organics, thus the PAM potential environmental pollution cannot be ignored. [ABSTRACT FROM AUTHOR]

The metabolic profiles of seed extracts from two cultivars of avocado (Hass var. and Criollo var., thereafter Hass and Criollo) were obtained using FTIR and 1H NMR spectroscopies. The extracts can be regarded as a rich source of bioactive compounds with significant antioxidant and antimicrobial properties. The extraction yields was 25.5% for Hass and 17.5% for Criollo. Total phenolic content and antioxidant activity were higher for Hass (287.41 ± 1.36 mg GAE/g dry extract and 1329.48 ± 6.89 μmol Fe + 2/g dry seed) as compared to Criollo (207.01 ± 1.38 mg GAE/g dry extract and 1276.18 ± 6.4 μmol Fe + 2/g dry seed). Also, the composition of the extracts was determined by using UPLC-ESI-QTOF-MS/MS. Eleven compounds were identified in both extracts, which included mainly phenolic acids, epicatechin derivatives and flavonoids. These compounds were correlated to the profiles obtained with FTIR and 1H NMR. A higher inhibition growth of S. aureus was observed for Hass extracts. The results obtained here suggest that avocado seeds from Hass variant are a substantial source of bioactive compounds, which may have significant potential in the food industry. [ABSTRACT FROM AUTHOR]

Two untargeted metabolomics approaches (LC-HRMS and 1H NMR) were combined to classify Amarone wines based on grape withering time and yeast strain. The study employed a multi-omics data integration approach, combining unsupervised data exploration (MCIA) and supervised statistical analysis (sPLS-DA).The results revealed that the multi-omics pseudo-eigenvalue space highlighted a limited correlation between the datasets (RV-score = 16.4%), suggesting the complementarity of the assays. Furthermore, the sPLS-DA models correctly classified wine samples according to both withering time and yeast strains, providing a much broader characterization of wine metabolome with respect to what was obtained from the individual techniques. Significant variations were notably observed in the accumulation of amino acids, monosaccharides, and polyphenolic compounds throughout the withering process, with a lower error rate in sample classification (7.52%).In conclusion, this strategy demonstrated a high capability to integrate large omics datasets and identify key metabolites able to discriminate wine samples based on their characteristics.

The use of biochar can have several effects on plant germination, depending on raw material, preparation method and application dose. However, the molecular mechanisms that lead to those results have yet to be elucidated. The aim of this research was to improve the understanding of these mechanisms by characterizing the metabolic effects of sugarcane bagasse biochar on soybean germination. Three types of biochars were prepared by pyrolysis at 300 ​°C (SCB300), 400 ​°C (SCB400) and 600 ​°C (SCB600). Then, each one was mixed into sand at 1%, 3%, 5% (w/w) dose, respectively. The experiment was performed in 8 days of incubation, when the number of germinated seeds and the average radicle length were determined. To evaluate the metabolome, the dry biomass (DB) was subjected to extraction with a mixture of methanol-d4 and D2O (1:1 v/v). The extracts were submitted to metabolomics analysis by Proton Nuclear Magnetic Resonance. The Relative Germination, Relative Average Radicle Growth and Germination Index increased in all treatments compared to control. On the other hand, the DB increased in all treatments, except for SCB300, at doses of 1% and 3% w/w. Seven metabolites (alanine, asparagine, acetic acid, citric acid, glycerol, fatty acids and sucrose) were identified and quantified in DB extracts as the most influential finding for the separation of treatments. Taken together, these results strongly suggested that biochars accelerated the catabolism of triacylglycerols to sucrose and induced a slight osmotic stress.

Abstract Background The new trend demanding for “natural” agri-food products has encouraged the application of more sustainable and eco-friendly farming methods, which limit or avoid the use of synthetic chemicals. This approach is increasing in viticulture, one of the sectors with the highest commercial value since grapes and derived products are largely consumed foodstuffs, with appreciated nutritional and sensory features. In this work, 1H Nuclear Magnetic Resonance spectroscopy (1H NMR) was applied for the metabolic profiling of cv. Italia table grapes samples, from the same origin area, cultivated with different treatments (biodynamic, organic and integrated) and collected in three subsequent vintages. Multivariate statistical analysis was performed on NMR-data with the aim of comprehensively researching the possible influences on metabolites due to the use of diverse agricultural practices. Results Both inter-annual variability (2020, 2021 and 2022 vintages) and different vineyard treatments (biodynamic, organic and integrated) resulted as significant drivers for samples differentiation in the preliminary unsupervised analysis of the (1H NMR spectra derived) metabolic profile data. Nevertheless, supervised data analyses showed that inter-vineyards variability, due to application of diverse farming methods, had a comparable discriminating effect with respect to harvesting years. Ethanol, sugars (as α-/β-glucose), organic acids (as malate) and amino acids (as arginine, leucine, glutamine) resulted the most viticultural practices-dependent metabolites. Interestingly, results from pairwise comparisons between treatments indicated the biodynamic samples with respect to the organic ones as the best-observed differentiation. This was followed by the biodynamic vs integrated and organic vs integrated samples comparisons, in decreasing discrimination order, as confirmed by the descriptiveness and predictive ability parameters of the corresponding pairwise OPLS-DA models. Conclusions Results highlighted that metabolites’ composition in cv. Italia table grapes juice is significantly affected by the use of different kinds of vineyard managements (biodynamic, organic and integrated, here investigated). Metabolomics study, here employing 1H NMR spectroscopy combined with multivariate statistical analysis, offers powerful tools to elucidate the metabolic differences among classes of samples. Graphical Abstract

The primary objective of this investigation was to explore the electrochemical oxidation behavior of Sorbitan monolaurate (Span 20) under high-voltage environments. We designed and prepared working electrodes using a mixture containing Span 20 and conductive carbon black as an electron transport material. Linear sweep voltammetry (LSV) served as the technique to monitor the reactions undergone by Span 20. The oxidative products were subjected to analysis using X-ray photoelectron spectroscopy (XPS) and nuclear magnetic resonance hydrogen spectrum (1H NMR). LSV reveals the decomposition of Span 20 occurring at voltages exceeding 4.2 V, involving two distinct reactions. Further insights from XPS and 1H NMR demonstrated that Span 20 underwent a two-electron-two-proton electrochemical reaction, producing triketone and 1, 3-diketone with a hydroxyl group positioned at the 2 position. To elucidate these results, a reasoning mechanism was proposed. [ABSTRACT FROM AUTHOR]

Polycystic ovary syndrome (PCOS) is a common systemic disorder related to endocrine disorders, affecting the fertility of women of childbearing age. It is associated with glucose and lipid metabolism disorders, altered gut microbiota, and insulin resistance. Modern treatments like pioglitazone, metformin, and spironolactone target specific symptoms of PCOS, while in Chinese medicine, moxibustion is a common treatment. This study explores moxibustion’s impact on PCOS by establishing a dehydroepiandrosterone (DHEA)-induced PCOS rat model. Thirty-six specific pathogen-free female Sprague-Dawley rats were divided into four groups: a normal control group (CTRL), a PCOS model group (PCOS), a moxibustion treatment group (MBT), and a metformin treatment group (MET). The MBT rats received moxibustion, and the MET rats underwent metformin gavage for two weeks. We evaluated ovarian tissue changes, serum testosterone, fasting blood glucose (FBG), and fasting insulin levels. Additionally, we calculated the insulin sensitivity index (ISI) and the homeostasis model assessment of insulin resistance index (HOMA-IR). We used 16S rDNA sequencing for assessing the gut microbiota, 1 H NMR spectroscopy for evaluating metabolic changes, and Spearman correlation analysis for investigating the associations between metabolites and gut microbiota composition. The results indicate that moxibustion therapy significantly ameliorated ovarian dysfunction and insulin resistance in DHEA-induced PCOS rats. We observed marked differences in the composition of gut microbiota and the spectrum of fecal metabolic products between CTRL and PCOS rats. Intriguingly, following moxibustion intervention, these differences were largely diminished, demonstrating the regulatory effect of moxibustion on gut microbiota. Specifically, moxibustion altered the gut microbiota by increasing the abundance of UCG-005 and Turicibacter, as well as decreasing the abundance of Desulfovibrio. Concurrently, we also noted that moxibustion promoted an increase in levels of short-chain fatty acids (including acetate, propionate, and butyrate) associated with the gut microbiota of PCOS rats, further emphasizing its positive impact on gut microbes. Additionally, moxibustion also exhibited effects in lowering FBG, testosterone, and fasting insulin levels, which are key biochemical indicators associated with PCOS and insulin resistance. Therefore, these findings suggest that moxibustion could alleviate DHEA-induced PCOS by regulating metabolic levels, restoring balance in gut microbiota, and modulating interactions between gut microbiota and host metabolites. [ABSTRACT FROM AUTHOR]

Late-season varieties of mandarin (Citrus reticulata Blanco) have a high economic value, so their study, characterization, and comparison among different commercial varieties is of great interest for agriculture. Detailed metabolomic analysis of mandarin leaves can provide valuable information on agronomic characteristics, vegetative development, and tree response to abiotic and biotic stresses. In this study, an analysis of the main metabolites presents in the leaves of three late-season mandarin orange varieties ('Afourer', 'Orri' and 'Tango'), cultivated under homogeneous conditions, was carried out using nuclear magnetic resonance (1H NMR) and multivariate statistical analysis techniques. The results show that organic acids and sugars are the metabolites with the highest presence in mandarin leaves, especially malate and sucrose. Ten amino acids and other metabolites such as choline and trigonelline were also detected. Metabolites such as asparagine and isoleucine were widely implicated in the metabolic pathways of the detected compounds. The 'Orri' variety showed significantly more differences in metabolite concentrations compared to the other two varieties studied. Malate and sucrose were shown to be the metabolites with the greatest significant differences between the varieties compared. From an agronomic point of view, the 'Orri' variety differs from the other two varieties because it has concentrations of metabolites that provide good resistance to abiotic and biotic stresses and fruits of higher quality and sweetness. [ABSTRACT FROM AUTHOR]

Background: The new trend demanding for "natural" agri-food products has encouraged the application of more sustainable and eco-friendly farming methods, which limit or avoid the use of synthetic chemicals. This approach is increasing in viticulture, one of the sectors with the highest commercial value since grapes and derived products are largely consumed foodstuffs, with appreciated nutritional and sensory features. In this work, 1H Nuclear Magnetic Resonance spectroscopy (1H NMR) was applied for the metabolic profiling of cv. Italia table grapes samples, from the same origin area, cultivated with different treatments (biodynamic, organic and integrated) and collected in three subsequent vintages. Multivariate statistical analysis was performed on NMR-data with the aim of comprehensively researching the possible influences on metabolites due to the use of diverse agricultural practices. Results: Both inter-annual variability (2020, 2021 and 2022 vintages) and different vineyard treatments (biodynamic, organic and integrated) resulted as significant drivers for samples differentiation in the preliminary unsupervised analysis of the (1H NMR spectra derived) metabolic profile data. Nevertheless, supervised data analyses showed that inter-vineyards variability, due to application of diverse farming methods, had a comparable discriminating effect with respect to harvesting years. Ethanol, sugars (as α-/β-glucose), organic acids (as malate) and amino acids (as arginine, leucine, glutamine) resulted the most viticultural practices-dependent metabolites. Interestingly, results from pairwise comparisons between treatments indicated the biodynamic samples with respect to the organic ones as the best-observed differentiation. This was followed by the biodynamic vs integrated and organic vs integrated samples comparisons, in decreasing discrimination order, as confirmed by the descriptiveness and predictive ability parameters of the corresponding pairwise OPLS-DA models. Conclusions: Results highlighted that metabolites' composition in cv. Italia table grapes juice is significantly affected by the use of different kinds of vineyard managements (biodynamic, organic and integrated, here investigated). Metabolomics study, here employing 1H NMR spectroscopy combined with multivariate statistical analysis, offers powerful tools to elucidate the metabolic differences among classes of samples. [ABSTRACT FROM AUTHOR]

The use of biochar can have several effects on plant germination, depending on raw material, preparation method and application dose. However, the molecular mechanisms that lead to those results have yet to be elucidated. The aim of this research was to improve the understanding of these mechanisms by characterizing the metabolic effects of sugarcane bagasse biochar on soybean germination. Three types of biochars were prepared by pyrolysis at 300 ℃ (SCB300), 400 ℃ (SCB400) and 600 ℃ (SCB600). Then, each one was mixed into sand at 1%, 3%, 5% (w/w) dose, respectively. The experiment was performed in 8 days of incubation, when the number of germinated seeds and the average radicle length were determined. To evaluate the metabolome, the dry biomass (DB) was subjected to extraction with a mixture of methanol-d4 and D2O (1:1 v/v). The extracts were submitted to metabolomics analysis by Proton Nuclear Magnetic Resonance. The Relative Germination, Relative Average Radicle Growth and Germination Index increased in all treatments compared to control. On the other hand, the DB increased in all treatments, except for SCB300, at doses of 1% and 3% w/w. Seven metabolites (alanine, asparagine, acetic acid, citric acid, glycerol, fatty acids and sucrose) were identified and quantified in DB extracts as the most influential finding for the separation of treatments. Taken together, these results strongly suggested that biochars accelerated the catabolism of triacylglycerols to sucrose and induced a slight osmotic stress. [ABSTRACT FROM AUTHOR]

The chitosan films were prepared from shrimp, squid, and crab to corroborate that regardless of the source of the chitosan, it was possible to measure the degree of deacetylation. In this work, the degree of deacetylation of chitosan was evaluated via UV, FTIR and 1H NMR spectrophotometry methodologies. Values in a range of 74 to 99% degree of deacetylation (DD) were obtained and varied depending on the method used and the source of chitosan. The spectrophotometric method is one of the most commonly used for this determination; however, it has the limitation that D-glucosamine and N-acetylglucosamine share similar wavelengths. All three methods were simple and provided rapid analysis; however, NMR, in particular, was expensive due to its equipment specifications. For this reason, its important to select the simplest method than can be routinely used. • The simplest used technique to determine the degree of deacetylation is infrared spectroscopy. • The degree of acetylation of chitosan is related to its physicochemical properties; its determination is an important parameter due to its association with chitosan applications in different industrial areas. • The 1H NMR method is very precise and requires expensive equipment and trained personal. Thus, it cannot be used routinely to determine the degree of deacetylation.

As a salt-type compound, mosapride citrate’s metabolism and side effects are correlated with its salt-forming ratio. Several techniques were developed in this work to compare various quantitative nuclear magnetic resonance (qNMR) methodologies and to quantitatively examine the content of raw materials. Among the qNMR techniques, methods for 1H NMR and 19F NMR were developed. Appropriate solvents were chosen, and temperature, number of scans, acquisition time, and relaxation delay parameter settings were optimized. Maleic acid was chosen as the internal standard in 1H NMR, and the respective characteristic signals of mosapride and citrate were selected as quantitative peaks. The internal standard in 19F NMR analysis was 4,4′-difluoro diphenylmethanone, and the distinctive signal peak at −116.15 ppm was utilized to quantify mosapride citrate. The precision, repeatability, linearity, stability, accuracy, and robustness of the qNMR methods were all validated according to the ICH guidelines. By contrasting the outcomes with those from high-performance liquid chromatography (HPLC), the accuracy of qNMR was assessed. As a result, we created a quicker and easier qNMR approach to measure the amount of mosapride citrate and evaluated several qNMR techniques to establish a foundation for choosing quantitative peaks for the qNMR method. Concurrently, it is anticipated that various selections of distinct quantitative objects will yield the mosapride citrate salt-forming ratio.

High-resolution 1H nuclear magnetic resonance (1H NMR) was advanced to determine both epoxy value and iodine value (IV) of vegetable oils that occur during their epoxidation. For calibration, rather than using a series of diluted stock samples, epoxidized soybean oils with a range of IV and epoxy value synthesized using entrapped peroxophosphotungstate as the catalyst under different reaction conditions were used. During the epoxidation reaction, IV and epoxy value were tracked with respect to time using 1H NMR and conventional volumetric methods. The integrated peak area of the olefinic hydrogens (5.3–5.5 ppm) was used to calculate the absolute number of double-bonded protons. By comparison of IV obtained by 1H NMR and the traditional Wijs-cyclohexane methods, the correlation coefficient was R2 = 0.9997 for the regression equation y = 1.1314x + 1.0035, where x was the result given by 1H NMR. The average integrated peak areas related to the hydrogens of the epoxide groups located at chemical shifts of 2.9 ppm (monoepoxide) and 3.1 ppm (diepoxide) were used to determine the epoxy value. The quantification of the number of epoxides was carried out by 1H NMR and the values obtained were correlated with epoxide content determined by the hydrochloric acid/acetone method. As a consequence, the correlation coefficient was R2 = 0.9991 for the regression equation y = 0.0052x + 1.7258, where x was the average integrated peak areas related to the hydrogens of the epoxide groups by 1H NMR. The novelty of our study lies in the simultaneous correlation between IV and epoxy value obtained from conventional titrations, the integrated peak area related to olefinic protons, and the average integrated peak area located at the hydrogen of epoxide group, calculated using 1H NMR. This approach is used to monitor and optimize the epoxidation reaction. [ABSTRACT FROM AUTHOR]

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Background: Cystic echinococcosis (CE) is a parasitic zoonosis caused by the tapeworm Echinococcus granulosus. Over the past few years, a lot of research has been done on liver illnesses using metabolomics techniques to identify biomarkers which could identify the diseases in its early stages. The present study was done to explore biomarkers in serum, urine, and cystic fluid which would help in differentiating, staging, and assessing fertility of intra-abdominal hydatid cyst by using proton nuclear magnetic resonance (1H NMR) metabolomics. Materials and methods: In the study, 28 subjects (16 cases and 12 controls) were enrolled. Staging of hydatid cysts was performed using ultrasonography. In patients complying with case and control definition, blood, urine, and cystic fluid were collected for complete blood count, urine culture, Echinococcus IgG enzyme-linked immunosorbent assay (ELISA), and metabolomic analysis. The 17, 15, and 11 metabolites in serum, urine, and cystic fluid samples were quantified, respectively, to differentiate between case and control group. Results: In this study, we observed that there was a significant downregulation of succinate metabolite in urine samples of cases, down-regulation of five metabolites (isoleucine, valine, histidine, tyrosine and formate) and upregulation of alanine in cystic fluid of cases. Conclusion: Current study demonstrates that metabolomics can be used non-invasively for rapid diagnosis of CE. This is one of the very few studies, which used 1H NMR spectroscopy, to analyze the profile of metabolites in serum, urine, and cystic fluid in cases of CE and controls. [ABSTRACT FROM AUTHOR]

One‐dimensional (1D) proton‐nuclear magnetic resonance (1H‐NMR) spectroscopy is an established technique for the deconvolution of complex biological sample types via the identification/quantification of small molecules. It is highly reproducible and could be easily automated for small to large‐scale bioanalytical, epidemiological, and in general metabolomics studies. However, chemical shift variability is a serious issue that must still be solved in order to fully automate metabolite identification. Herein, we demonstrate a strategy to increase the confidence in assignments and effectively predict the chemical shifts of various NMR signals based upon the simplest form of statistical models (i.e., linear regression). To build these models, we were guided by chemical homology in serum/plasma metabolites classes (i.e., amino acids and carboxylic acids) and similarity between chemical groups such as methyl protons. Our models, built on 940 serum samples and validated in an independent cohort of 1,052 plasma‐EDTA spectra, were able to successfully predict the 1H NMR chemical shifts of 15 metabolites within ~1.5 linewidths (Δv1/2) error range on average. This pilot study demonstrates the potential of developing an algorithm for the accurate assignment of 1H NMR chemical shifts based solely on chemically defined constraints. [ABSTRACT FROM AUTHOR]

Nuclear magnetic resonance (NMR) spectral analysis of biofluids can be a time‐consuming process, requiring the expertise of a trained operator. With NMR becoming increasingly popular in the field of metabolomics, there is a growing need to change this paradigm and to automate the process. Here we introduce MagMet, an online web server, that automates the processing and quantification of 1D 1H NMR spectra from biofluids—specifically, human serum/plasma metabolites, including those associated with inborn errors of metabolism (IEM). MagMet uses a highly efficient data processing procedure that performs automatic Fourier Transformation, phase correction, baseline optimization, chemical shift referencing, water signal removal, and peak picking/peak alignment. MagMet then uses the peak positions, linewidth information, and J‐couplings from its own specially prepared standard metabolite reference spectral NMR library of 85 serum/plasma compounds to identify and quantify compounds from experimentally acquired NMR spectra of serum/plasma. MagMet employs linewidth adjustment for more consistent quantification of metabolites from higher field instruments and incorporates a highly efficient data processing procedure for more rapid and accurate detection and quantification of metabolites. This optimized algorithm allows the MagMet webserver to quickly detect and quantify 58 serum/plasma metabolites in 2.6 min per spectrum (when processing a dataset of 50–100 spectra). MagMet's performance was also assessed using spectra collected from defined mixtures (simulating other biofluids), with >100 previously measured plasma spectra, and from spiked serum/plasma samples simulating known IEMs. In all cases, MagMet performed with precision and accuracy matching the performance of human spectral profiling experts. MagMet is available at http://magmet.ca. [ABSTRACT FROM AUTHOR]

We report the development of a software program, called MagMet‐F, that automates the processing and quantification of 1D 1H NMR of human fecal extracts. To optimize the program, we identified 82 potential fecal metabolites using 1D 1H NMR of six human fecal extracts using manual profiling and a literature review of known fecal metabolites. We acquired pure versions of those metabolites and then acquired their 1D 1H NMR spectra at 700 MHz to generate a fecal metabolite spectral library for MagMet‐F. The fitting of these metabolites by MagMet‐F was iteratively optimized to replicate manual profiling. We validated MagMet‐F's automated profiling using a test set of six fecal extracts. It correctly identified 80% of the compounds and quantified those within <20% of the values determined by manual profiling using Chenomx. We also compared MagMet‐F's profiling performance to two other open‐access NMR profiling tools, Bayesil and Batman. MagMet‐F outperformed both. Bayesil repeatedly overestimated metabolite concentrations by 10% to 40% while Batman was unable to properly quantify any compounds and took 10–20× longer. We have implemented MagMet‐F as a freely accessible web server to enable automated, fast and convenient 1D 1H NMR spectral profiling of fecal samples. MagMet‐F is available at https://www.magmet.ca. [ABSTRACT FROM AUTHOR]

Tetrahydrobiopterin (BH4) is an essential biological cofactor and a derivative of pterin which is considered potent anticancer agents. In continuation of our previous study on the identification of BH4 from cyanide‐degrading Bacillus pumilus, the present study focuses on evaluating the anticancer properties of BH4 on A549, a human lung adenocarcinoma. Anticancer activity analysis shows that BH4 inhibited A549 cell growth after 24 h of incubation with 0.02 mg/mL. In acridine orange/ethidium bromide staining, BH4‐treated A549 cells showed apoptotic morphology. BH4 treatment caused cell cycle arrest at G0/G1 phase compared to control cells. BH4 augmented p53 expression in alveolar cancer cells by downregulating MDM2 levels. There was downregulation of casp‐3 and upregulation of iNOS gene in BH4‐treated A549 cells. Further, docking studies indicated that BH4 had significant interactions with the above proteins affirming the apoptosis mechanism. Thus, BH4 could be considered a potential anticancer drug. [ABSTRACT FROM AUTHOR]

Introduction: Idiopathic acquired aplastic anemia (AA) is a bone marrow failure disorder where aberrant T-cell functions lead to depletion of hematopoietic stem and progenitor cells in the bone marrow (BM) microenvironment. T-cells undergo metabolic rewiring, which regulates their proliferation and differentiation. Therefore, studying metabolic variation in AA patients may aid us with a better understanding of the T-cell regulatory pathways governed by metabolites and their pathological engagement in the disease. Objective: To identify the differential metabolites in BM plasma of AA patients, AA follow-up (AAF) in comparison to normal controls (NC) and to identify potential disease biomarker(s). Methods: The study used 1D 1H NMR Carr–Purcell–Meiboom–Gill (CPMG) spectra to identify the metabolites present in the BM plasma samples of AA (n = 40), AAF (n = 16), and NC (n = 20). Metabolic differences between the groups and predictive biomarkers were identified by using multivariate analysis and receiver operating characteristic (ROC) module of Metaboanalyst V5.0 tool, respectively. Results: The AA and AAF samples were well discriminated from NC group as per Principal Component analysis (PCA). Further, we found significant alteration in the levels of 17 metabolites in AA involved in amino-acid (Leucine, serine, threonine, phenylalanine, lysine, histidine, valine, tyrosine, and proline), carbohydrate (Glucose, lactate and mannose), fatty acid (Acetate, glycerol myo-inositol and citrate), and purine metabolism (hypoxanthine) in comparison to NC. Additionally, biomarker analysis predicted Hypoxanthine and Acetate can be used as a potential biomarker. Conclusion: The study highlights the significant metabolic alterations in the BM plasma of AA patients which may have implication in the disease pathobiology. [ABSTRACT FROM AUTHOR]

Inspiratory muscle training (IMT) is known to promote physiological benefits and improve physical performance in endurance sports activities. However, the metabolic adaptations promoted by different IMT prescribing strategies remain unclear. In this work, a longitudinal, randomized, double-blind, sham-controlled, parallel trial was performed to investigate the effects of 11 weeks (3 days·week−1) of IMT at different exercise intensities on the serum metabolomics profile and its main regulated metabolic pathways. Twenty-eight healthy male recreational cyclists (30.4 ± 6.5 years) were randomized into three groups: sham (6 cm·H2O of inspiratory pressure, n = 7), moderate-intensity (MI group, 60% maximal inspiratory pressure (MIP), n = 11) and high-intensity (HI group, 85–90% MIP, n = 10). Blood serum samples were collected before and after 11 weeks of IMT and analyzed by 1H NMR and UHPLC-HRMS/MS. Data were analyzed using linear mixed models and metabolite set enrichment analysis. The 1H NMR and UHPLC-HRMS/MS techniques resulted in 46 and 200 compounds, respectively. These results showed that ketone body metabolism, fatty acid biosynthesis, and aminoacyl-tRNA biosynthesis were upregulated after IMT, while alpha linolenic acid and linoleic acid metabolism as well as biosynthesis of unsaturated fatty acids were downregulated. The MI group presented higher MIP, Tryptophan, and Valine levels but decreased 2-Hydroxybutyrate levels when compared to the other two studied groups. These results suggest an increase in the oxidative metabolic processes after IMT at different intensities with additional evidence for the upregulation of essential amino acid metabolism in the MI group accompanied by greater improvement in respiratory muscle strength. [ABSTRACT FROM AUTHOR]

Kurzfassung: Die Carbonatisierung von Beton und der damit einhergehende Verlust der Passivierung der Stahlbewehrung stellt jeher eine Herausforderung hinsichtlich der Dauerhaftigkeit von Stahlbetonbauwerken dar. Um eine Schädigung infolge der Korrosion der Bewehrung zu vermeiden und Instandsetzungsmaßnahmen zum Erhalt der Passivierung rechtzeitig durchzuführen, gilt es die Carbonatisierungstiefe des Betons zu bestimmen. Die Bestimmung der Carbonatisierungstiefe mithilfe des pH‐Indikators Phenolphthalein stellt diesbezüglich den Stand der Technik dar, wird hierbei jedoch nur indirekt die Carbonatisierung des Betons auf Grundlage des pH‐Werts bestimmt. Eine direkte Messung der mit der Carbonatisierung einhergehenden strukturellen Änderungen, welche ebenfalls eine Änderung der Transporteigenschaften des Betons hervorruft, wird mithilfe des Phenolphthaleintests nicht erfasst. Mithilfe der einseitigen Wasserstoffkernspinresonanz (1H NMR) ist eine tiefenabhängige Untersuchung der Gefügestruktur möglich. Erste Ergebnisse zeigen, dass eine Ableitung des Carbonatisierungsfortschritts anhand der NMR‐Untersuchungen an Mörtel möglich ist. Mithilfe der Korrelation weiterer Untersuchungsmethoden kann ein umfassendes Verständnis des Carbonatisierungsprozesses gewonnen werden. [ABSTRACT FROM AUTHOR]

Self‐leveling underlayments (SLU) are used for smoothing and levelling sub‐floors before any flexible flooring is applied. Though being comparatively simple in its requirements, commercial SLUs have become one of the most complex cementitious mixtures in dry‐mortar technology. By using ternary binders, most SLUs are designed to be self‐drying, binding most of the mixing water in crystalline cementitious phases, allowing a fast work progress. In this study, the simultaneous hydration and drying of a commercial SLU are monitored with single‐sided 1H nuclear magnetic resonance (NMR). This technique allows the quantification of chemically bound water and water in different pore environments with superior time and depth resolution. The technique is combined with conventional testing techniques enabling a more comprehensive view on the processes at hand. Results allow quantification of hydration and self‐drying, superimposed by physical drying effects over time. Additionally, the drying of a PVC adhesive through water absorption into a well‐dried SLU are visualized with this technique. The results are discussed in the context of moisture transport processes and floor‐laying readiness of the material. [ABSTRACT FROM AUTHOR]

The study sought to investigate the impact of a holistic high-power microwave technology during all stages of the extraction on the quality, time of extraction, and degree of deacetylation (DD) of shrimp chitosan (SC) and crab chitosan (KC). The demineralization and deproteinization stages took 7 and 8 min, at 750 and 875 W, respectively. The deacetylation process was conducted at two powers, 875 W and 1250 W, for 10, 15, and 20 min. It only took 25 min at 875 W to successfully prepare chitosan with a high DD and 30 min to reach the maximum DD. The highest DDs by the potentiometric titration method, FTIR, and 1H NMR of SC were 86.6%, 86.7%, and 83%, compared to 83.8%, 82.7%, and 80% for KC, respectively. Extracted SC had 79% solubility, 14.125 kDa, a 46.57% crystallinity index, 705.40% WBC, and 434.60% FBC, against 74.5%, 16.982 kDa, 74.14%, 689.82%, and 413.20% for KC, respectively. The study proved that 30 min of holistic high-power microwave at 875 W produced low-molecular-weight chitosan with relatively high deacetylation and low content of viscosity, crystallinity, and protein residue. The technique can provide a feasible alternative to the commercial production of low-molecular-weight chitosan in less time and energy.Article Highlights: High-power (875 W) microwave irradiation at 15 min-deacetylation produced Chitosan’s maximum deacetylation degree (DD). Holistic microwave irradiation (MW) can successfully produce high DD chitosan, and low molecular weight in 30 min. The chemical structure of MW-extracted chitosan was confirmed by FTIR and 1H NMR and low crystallinity by X-ray. [ABSTRACT FROM AUTHOR]

Wine maturation in oak barrels is a well-known winemaking practice that, among other things, brings roundness and complexity to wine. Studying wine evolution during barrel maturation is crucial to ensure wine quality. Red wines produced in a wine growing estate of the Bordeaux region were monitored after one and twelve months of maturation in oak barrels in the estate’s cellar. Wines were kept in oak casks from three different manufacturers. The evolution of the wine constituents during maturation was monitored by 1H NMR-based metabolomics combined with multivariate statistical analysis. NMR spectra were submitted to targeted and untargeted approaches. The wine maturation effects were thereby monitored and the discriminant metabolites identified. The wines analysed after one month of maturation exhibit higher contents of amino acids, catechin and epicatechin, acetoin and choline than the wines analysed twelve months after maturation; for their part, the latter wines showed higher contents of acetic acid, ethyl lactate, arabinose and glucose. In addition, significant differences were observed between the wines depending on the barrel manufacturers.

Abstract The study sought to investigate the impact of a holistic high-power microwave technology during all stages of the extraction on the quality, time of extraction, and degree of deacetylation (DD) of shrimp chitosan (SC) and crab chitosan (KC). The demineralization and deproteinization stages took 7 and 8 min, at 750 and 875 W, respectively. The deacetylation process was conducted at two powers, 875 W and 1250 W, for 10, 15, and 20 min. It only took 25 min at 875 W to successfully prepare chitosan with a high DD and 30 min to reach the maximum DD. The highest DDs by the potentiometric titration method, FTIR, and 1H NMR of SC were 86.6%, 86.7%, and 83%, compared to 83.8%, 82.7%, and 80% for KC, respectively. Extracted SC had 79% solubility, 14.125 kDa, a 46.57% crystallinity index, 705.40% WBC, and 434.60% FBC, against 74.5%, 16.982 kDa, 74.14%, 689.82%, and 413.20% for KC, respectively. The study proved that 30 min of holistic high-power microwave at 875 W produced low-molecular-weight chitosan with relatively high deacetylation and low content of viscosity, crystallinity, and protein residue. The technique can provide a feasible alternative to the commercial production of low-molecular-weight chitosan in less time and energy.

Extracellular DNA (exDNA) can be actively released by living cells and different putative functions have been attributed to it. Further, homologous exDNA has been reported to exert species-specific inhibitory effects on several organisms. Here, we demonstrate by different experimental evidence, including 1H-NMR metabolomic fingerprint, that the growth rate decline in Saccharomyces cere-visiae fed-batch cultures is determined by the accumulation of exDNA in the medium. Sequencing of such secreted exDNA represents a portion of the en-tire genome, showing a great similarity with extrachromosomal circular DNA (eccDNA) already reported inside yeast cells. The recovered DNA molecules were mostly single strands and specifically associated to the yeast metabolism displayed during cell growth. Flow cytometric analysis showed that the ob-served growth inhibition by exDNA corresponded to an arrest in the S phase of the cell cycle. These unprecedented findings open a new scenario on the func-tional role of exDNA produced by living cells.

Bile acids are the main body of enterohepatic circulation in vivo. They have essential functions such as emulsifying fat, bacteriostasis and regulating multiple metabolic pathways as signal molecules. However, the assignments of NMR signals for some low-concentration bile acids are still needed. This study combined 1D nuclear magnetic resonance (NMR) and 2D NMR techniques including 1H–1H correlation spectroscopy (COSY), 1H–1H total correlation spectroscopy (TOCSY), 1H J-resolved spectroscopy (J-Res), 1H–13C heteronuclear single quantum coherence spectroscopy (HSQC), and 1H–13C heteronuclear multiple bond correlation spectroscopy (HMBC) to assign the 1H and 13C signals of six bile acids in aqueous solution at physiological pH (∼7.4) and nine bile acids in methanol. These data are of importance to the NMR-based studies on lipid digestion, absorption, and metabolism.

Early NMR studies of several heterohelicenes containing an annular nitrogen atom and a thiophene ring in their structure suggested the possibility of the lengthening of the carbon–carbon bonds in the interior of the helical turn of the molecule based on the progressive upfield shift of 13C resonances toward the center of the helical turn. We now report a comprehensive analysis of the optimized geometry and a comparison of the calculated vs. observed 1H and 13C NMR chemical shifts of nineteen representative benzothienoquinoline heterohelicenes. As was initially hypothesized on the basis of the progressive upfield shift of carbon resonances toward the center of the interior helical turn, the present computational study has demonstrated that carbon–carbon bonds indeed have more sp3 character and are longer than normal sp2 bonds to accommodate the helical twist of the molecule, as expected.

In most cases, the number of honeybee stings received by the body is generally small, but honeybee stings can still cause serious allergic reactions. This study fully simulated bee stings under natural conditions and used 1H Nuclear Magnetic Resonance (1H NMR) to analyze the changes in the serum metabolome of Sprague–Dawley (SD) rats stung once or twice by honeybees to verify the impact of this mild sting on the body and its underlying mechanism. The differentially abundant metabolites between the blank control rats and the rats stung by honeybees included four amino acids (aspartate, glutamate, glutamine, and valine) and four organic acids (ascorbic acid, lactate, malate, and pyruvate). There was no separation between the sting groups, indicating that the impact of stinging once or twice on the serum metabolome was similar. Using the Principal Component Discriminant Analysis ( PCA-DA) and Variable Importance in Projection (VIP) methods, glucose, lactate, and pyruvate were identified to help distinguish between sting groups and non-sting groups. Metabolic pathway analysis revealed that four metabolic pathways, namely, the tricarboxylic acid cycle, pyruvate metabolism, glutamate metabolism, and alanine, aspartate, and glutamate metabolism, were significantly affected by bee stings. The above results can provide a theoretical basis for future epidemiological studies of bee stings and medical treatment of patients stung by honeybees.

Aconitum pendulum, a member of the Aconitum genus within the Ranunculaceae family, is known for its remarkable anti-inflammatory, anti-tumor, and analgesic properties. However, the application of Aconitum pendulum in traditional medicine is often restricted by its inherent toxicity, necessitating specific processing methods to ensure safe usage. Tibetan medicine utilizes distinctive processing techniques such as the barley wine, Hezitang, and zanba frying systems to render the herb safe for medicinal use. Despite the known pharmacological importance, scant research exists on how these processing methods affect the phytochemical profile of Aconitum pendulum, indicating a necessity for comparative analysis of the resulting concoctions. In this study, we employed 1H nuclear magnetic resonance (1H NMR) spectroscopy and ultra-performance liquid chromatography coupled with quadrupole time of flight mass spectrometry (UPLC-Q-TOF-MS) to explore the metabolomic variations among different processed products of Aconitum pendulum. Multivariate data analysis techniques, including pattern recognition, allowed us to investigate the intricacies of the compound profiles. To discover signature chemical markers that can differentiate the various processed products, we conducted paired t-tests and generated heat maps highlighting the detected differences. Our integrated analysis of the 1H NMR and UPLC-Q-TOF-MS data revealed distinct chemical signatures unique to each method of Aconitum pendulum processing. By employing chemometric analysis with variable importance in projection (VIP) scores greater than 1.0, and coupled with the statistical rigor of paired t-tests (P

The present study investigated the physico-chemical characteristics of whole-meal flours from three wild chickpea varieties (white chickpea – WC, red rough chickpea – RRC, red smooth chickpea – RSC) compared to a modern chickpea variety (MC) and their bread-making performances in 30% (w/w flour) substituted GF breads. Wild chickpea flours showed the highest ash, total dietary fiber (TDF), and total antioxidant capacity (6.3%, 13.4%, and 9.5% increase for WC, RRC, and RSC flour compared to MC flour) values compared to MC sample, and red varieties (RRC- and RSC-samples) showed the highest total phenolic content (15.5% and 17.0% increase compared to MC flour). Significant differences were also found in protein content and techno-functional properties. Bread specific volume and crumb hardness were significantly affected by chickpea variety, with red varieties (RRC- and RSC-samples) revealing the lowest impact. 1H NMR proton molecular mobility significantly changed as a function of chickpea variety, and these differences might be associated to the different macroscopic bread quality. Overall, the tested wild chickpea flours revealed valuable chemical composition, and differed in the techno-functional and bread-making performances, with red varieties showing the most promising results to improve GF breads.