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Colquhounia root tablets (CRT) and Tripterygium hypoglaucum hutch tablets (THHT), two major Tripterygium hypoglaucum hutch (THH) commercial preparations, have been used to treat chronic kidney diseases or rheumatic diseases. However, there have been no reports on the chemical comparison between CRT and THHT, greatly hindering the understanding of their pharmacological difference as well as their rational application in clinical practice. In the present study, ultra‐high‐performance liquid chromatography coupled with quadrupole time‐of‐flight tandem mass spectrometry combined with automated data analysis by MS‐DIAL software and MS‐FLO website was employed to systematically screen and characterize the components in CRT and THHT. Multivariate statistical analysis was used to compare the differences between these two preparations. As a result, up to 92 components were tentatively identified, and 17 of them were characterized for the first time in THH preparations. According to the criteria of variable importance in projection (VIP) >1, p < 0.05, and fold change (FC) > 1.2, 46 components could be screened as major differential chemical components. Among them, phenolic acids, organic acids, amino acids, and diterpenoids were higher in CRT, while the sesquiterpene alkaloids were relatively higher in THHT. This study clarified the chemical material basis and the difference between CRT and THHT, providing a valuable reference for quality control and clinical rational use of THH preparations. [ABSTRACT FROM AUTHOR]

Rationale: Rapid, accurate, and easy‐to‐perform diagnostic assays are required to address the current need for the diagnosis of resistant pathogens. That is particularly the case for mycobacteria, such as the human pathogen Mycobacterium tuberculosis, which requires up to 2 weeks for the determination of the drug susceptibility profile using the conventional broth microdilution method. To address this challenge, we investigated the incorporation of deuterium, the stable isotope of hydrogen, into lipids as a read out of the drug susceptibility profile. Methods: Deuterium is incorporated into newly synthesized proteins or lipids in place of hydrogen as bacterial cells grow, increasing the mass of the macromolecules, which can then be observed via matrix‐assisted laser desorption ionization time of flight mass spectrometry (MALDI‐TOF MS). As proof‐of‐concept, we used the non‐pathogenic Mycobacterium smegmatis mc2155 strain, which is susceptible to the aminoglycoside antibiotic kanamycin, and M. smegmatis mc2155 containing the empty vector pVV16, which is kanamycin‐resistant. Bacteria were incubated in a culture medium containing 50% of deuterium oxide (D2O) and either 1 or 2 times the minimal inhibitory concentration (MIC50) of kanamycin. Lipids were then analyzed using the MBT lipid Xtract matrix combined with routine MALDI mass spectrometry in the positive ion mode to evaluate the changes in the lipid profile. Results: Using this approach, we were able to distinguish susceptible from resistant bacteria in less than 5 h, a process that would take 72 h using the conventional broth microdilution method. Conclusions: We therefore propose a solution for the rapid determination of drug susceptibility profiles using a phenotypic assay combining D2O stable isotope labelling and lipid analysis by routine MALDI mass spectrometry. [ABSTRACT FROM AUTHOR]

Objective Methods Results Significance Epilepsy surgery is a treatment option for patients with seizures that do not respond to pharmacotherapy. The histopathological characterization of the resected tissue has an important prognostic value to define postoperative seizure outcome in these patients. However, the diagnostic classification process based on microscopic assessment remains challenging, particularly in the case of focal cortical dysplasia (FCD). Imaging mass spectrometry is a spatial omics technique that could improve tissue phenotyping and patient stratification by investigating hundreds of biomolecules within a single tissue sample, without the need for target‐specific reagents.An in situ proteomic technique called matrix‐assisted laser desorption/ionization mass spectrometry imaging (MALDI‐MSI) is here investigated as a potential new tool to expand conventional diagnosis on standard paraffin brain tissue sections. Unsupervised and region of interest‐based MALDI‐MSI analyses of sections from 10 FCD type IIb (FCDIIb) cases were performed, and the results were validated by immunohistochemistry.MALDI‐MSI identified distinct histopathological features and the boundaries of the dysplastic lesion. The capability to visualize the spatial distribution of well‐known diagnostic markers enabling multiplex measurements on single tissue sections was demonstrated. Finally, a fingerprint list of potential discriminant peptides that distinguish FCD core from peri‐FCD tissue was generated.This is the first study that explores the potential application of MALDI‐MSI in epilepsy postsurgery fixed tissue, by utilizing the well‐characterized FCDIIb features as a model. Extending these preliminary analyses to a larger cohort of patients will generate spectral libraries of molecular signatures that discriminate tissue features and will contribute to patient phenotyping. [ABSTRACT FROM AUTHOR]

The conducting two‐dimensional electron gas (2DEG) behavior in LaAlO3 (LAO)/SrTiO3 (STO) and their associated mechanisms from various aspects have brought tremendous attention in the concerned area of research. To correlate the 2DEG behavior with their compositions, we have performed time of flight secondary ion mass spectrometry (TOF‐SIMS) depth profile analysis of thin films of Cr‐doped LAO/STO system as LaAl1‐xCrxO3 (x = 0, 0.2, 0.6 and 1) deposited over TiO2 terminated STO substrate, which includes two parent compounds LAO/STO (metallic) and LCO/STO (insulating). The uniform decrease of La and Al concentration at the interface of LAO/STO (metallic) system and in the contrary the nonuniformity of La and Cr concentration in LCO/STO (insulating) system have been highlighted. The uniform variation of ionic concentration at the interface of LAO/STO may increase the career concentrations to make the system metallic. The upward and downward diffusion at the interfaces of intermediate compositions varies differently from their parent ones due to the mixing of Al and Cr. Our results may help to understand the conducting nature of LAO/STO system for future developments and applications in such system. [ABSTRACT FROM AUTHOR]

Summary: The increased consumption of minimally processed vegetables (MPV) in various countries is related to the continued interest of consumers in seeking practical and healthy food items. Due to multiple processing steps, MPV can be contaminated by several foodborne pathogens that pose significant health risks to consumers. The use of rapid techniques to detect pathogens in ready‐to‐eat (RTE) foods such as MPV is therefore essential to provide high quality and safe products. This review aims to provide a comprehensive description of molecular‐based techniques for rapid detection of pathogenic bacteria in MPV, and their occurrence reported in studies published in the last 10 years. The main pathogens detected using rapid methods were Salmonella spp., Escherichia coli, Listeria monocytogenes, Staphylococcus aureus, Shigella spp., and Campylobacter jejuni. Molecular‐based techniques included real‐time polymerase chain reaction (PCR), multiplex PCR, matrix‐assisted laser desorption ionisation time of flight mass spectrometry (MALDI‐TOF MS), and denaturing gradient gel electrophoresis (DGGE). The data indicate high incidences of pathogenic bacteria in MPV, stressing the need for their rapid detection in these products to prevent associated health risks. Further studies should be carried out to increase the sensitivity of molecular‐based techniques and prevent false positives due to undesirable non‐specific PCR amplifications. [ABSTRACT FROM AUTHOR]

Rational: Aconiti Lateralis Radix Praeparata (AC) is a traditional Chinese medicine with a long history of use. However, the current research on the material basis of AC and its processed products is still not comprehensive, especially the changes in lipo‐diterpenoid alkaloids (LDAs) that can be hydrolyzed into diester‐diterpenoid alkaloids in AC before and after processing. This study aimed to provide material basis guidance for the clinical use of AC and its processed products by comprehensively analyzing the changes in substances between AC and its processed products. Methods: An ultra‐high‐performance liquid chromatography with quadrupole time‐of‐flight mass spectrometry (UHPLC/Q‐TOF‐MS/MS) approach was optimized to chemical profiling. The MS data were processed using molecular networking combined with the in‐house library database to fast characterize the compounds. Multivariate statistical methods were adopted to determine the dissimilarities of components in AC and its processed products. Results: A total of 310 compounds were tentatively identified from AC, including 109 potential new alkaloids, of which 98 were potential novel LPAs. A metabolomics approach was applied to find the characteristic marker components. As a result, 52 potential chemical markers were selected to distinguish the AC samples of different extraction methods and 42 potential chemical markers for differentiating between AC and its processed products were selected. Conclusion: The results indicate that UHPLC/Q‐TOF‐MS/MS and Global Natural Products Social Molecular Networking coupled with multivariate analysis strategies was a powerful tool to rapidly identify and screen the chemical markers of alkaloids between the AC samples and its processed products. These results also indicate that the toxicity of water extracts of AC and its processed products were decreased. This research not only guides the clinical safe use of AC and its processed products, but also extends the application of the molecular networking strategy in traditional herbal medicine. [ABSTRACT FROM AUTHOR]

Rationale: This study developed a method for the rapid classification and identification of the chemical composition of Qingyan dropping pills (QDP) to provide the theoretical basis and data foundation for further in‐depth research on the pharmacological substance basis of the formula and the selection of quality control indexes. Methods: Ultra‐high performance liquid chromatography‐quadrupole time‐of‐flight mass spectrometry (UHPLC‐Q‐TOF‐MS) and data postprocessing technology were used to analyze the chemical composition of QDP. The fragmentation information on possible characteristic fragments and related neutral losses was summarized based on the literature and was compared with the MS data obtained from the assay, and thus a rapid classification and identification of chemical components in QDP could be achieved. Results: A total of 73 compounds were identified, namely 24 flavonoids, 14 terpenoids, 30 organic acids and their esters, 3 alkaloids, and 2 phenylpropanoids. Conclusions: In this study, UHPLC‐Q‐TOF‐MS and data postprocessing technology were used to realize the rapid classification and identification of the chemical constituents of QDP, which provided a comprehensive, efficient, and fast qualitative analysis method, a basis for further quality control and safe medication of QDP. [ABSTRACT FROM AUTHOR]

Rationale: Cloxacillin and flucloxacillin are prone to degradation and polymerization in humid and hot environments, and their polymers have long been recognized to trigger allergic manifestations. A series of the degradation and polymerized impurities in cloxacillin and flucloxacillin were separated and characterized to ensure safe use of these drugs by the public. Methods: By studying the chromatographic behavior of the degradation impurities and polymerized impurities in reversed‐phase high‐performance liquid chromatography (RP‐HPLC) gradient elution, the impurities in cloxacillin and flucloxacillin were effectively separated and eluted. RP‐HPLC tandem ion trap/time‐of‐flight mass spectrometry (MS) was applied to characterize the structures of unknown impurities eluted from the RP‐HPLC methods for cloxacillin and flucloxacillin. The mechanisms of formation of the impurities in cloxacillin and flucloxacillin were also investigated. Results: The structures of 10 unknown impurities in cloxacillin and 8 unknown impurities in flucloxacillin were elucidated based on the high‐resolution MSn data at positive and negative modes, respectively. Six polymerized impurities were found and characterized, of which three were from the polymerization of cloxacillin and three were from the polymerization of flucloxacillin. Conclusions: The study on the impurity profiles of cloxacillin and flucloxacillin provided a scientific basis for improving their production processes and quality control. [ABSTRACT FROM AUTHOR]

BACKGROUND: Rice‐based distillers' spent cake (RDSC), a by‐product of the Chinese liquor (Baijiu) industry, is a potential source of angiotensin‐converting enzyme (ACE) inhibitory peptide. Since ACE plays a crucial role in controlling hypertension, inhibition of ACE has been widely emphasized. The ACE inhibitory active peptide derived from by‐products of food has been recognized as a safer and cheaper inhibitor. RESULTS: Aimed to discover ACE‐inhibiting active peptides in RDSC. Hydrolysis of RDSC by alcalase for 4 h followed by ultrafiltration yielded low‐molecular‐weight (< 3 kDa) fractions. Subsequently, a comprehensive method using a combination of liquid chromatography quadrupole time‐of‐flight mass spectrometry (LC‐Q‐TOF‐MS) and LC‐Q‐Exactive‐MS to identify the novel short peptides (3–5 amino acids residues; n = 7) and medium‐sized peptides (more than 6 amino acids residues; n = 6). In vitro activity assay showed that the peptides KPFFPGL, GFPRPLL, GPPGVF, and VGK exhibited the highest activity with inhibitory concentration of 50% (IC50) of 11.63, 12.34, 19.55, and 33.54 μmol L−1. Molecular docking reveal that the active and inactive sites (Glu123, Asp121, Arg522, and Lys118) play important roles in enhancing the ACE inhibitory activity of peptides. CONCLUSION: Here we report a comprehensive method that effectively extracted and identified the bioactive peptides from RDSC. Four highly active novel peptides may be the most promising candidates for functional foods against hypertension, provide significant information for enhancing value of rice‐based distilled by‐products. © 2024 Society of Chemical Industry. [ABSTRACT FROM AUTHOR]

We evaluated the performance of Zybio EXS2600 matrix‐assisted laser desorption ionization time‐of‐flight mass spectrometry (MALDI‐TOF MS) (Zybio Inc., Chongqing, China) for the identification of bacteria from positive blood culture (BC) bottles using Blood Culture Positive Sample Pretreatment Kit (Zybio Inc., Chongqing, China) in comparison to an in‐house saponin method. Following a positive signal by the BACTEC™ FX system, confirmation of identification was achieved using subcultured growing biomass used for MALDI‐TOF MS analysis. A total of 94 positive BC bottles with 97 bacterial isolates were analyzed. The overall identification rates at the genus and species levels for the saponin method were 89.7% (87/97) and 74.2% (72/97), respectively. With the Zybio Kit, 88.7% (86/97) and 80.4% (78/97) of microorganisms were correctly identified to the genus and species levels, respectively. The saponin method identified 65.3% (32/49) of Gram‐positive bacteria at the species level, whereas the Zybio Kit achieved a higher species‐level identification rate of 79.6% (39/49) (p = 0.1153). The saponin method with additional on‐plate formic acid extraction showed a significantly higher overall identification rate in comparison to the saponin method without that step for both genus (87.6% [85/97] vs. 70.1% [68/97], p = 0.0029) and species level (70.1% [68/97] vs. 46.4% [45/97], p = 0.0008). Identification rates of Gram‐negative bacteria showed a higher identification rate, however, not statistically significant with additional Zybio Kit protocol step on both genus (85.4% [41/48] vs. 81.3% [39/48], p = 0.5858) and species level (77.1% [37/48] vs. 75% [36/48], p = 0.8120). Zybio Kit could offer an advantage in species‐level identification, particularly for Gram‐positive bacteria. The inclusion of on‐plate formic acid extraction in the saponin method notably enhanced identification at both genus and species levels for Gram‐positive bacteria. The extended protocol provided by the Zybio Kit could potentially offer an advantage in the identification of Gram‐negative bacteria at both genus and species levels. Enhancements to the Zybio EXS2600 MALDI‐TOF instrument software database are necessary. [ABSTRACT FROM AUTHOR]

Rationale: Despite decades of implementation, the selection of optimal sample preparation conditions for matrix-assisted laser desorption/ionization (MALDI) imaging is still ambiguous due to the lack of a universal and comprehensive evaluation methodology. Thus, numerous experiments with different matrix application conditions accompany a translation of the method to novel sample types and matrices. Methods: Mouse brain tissues were covered with 9-aminoacridine through sublimation, followed by recrystallization in vapors of 5% (v/v) methanol solution in water. The samples were analyzed by MALDI time-of-flight mass spectrometry, and the efficiency of lipid and small-molecule ionization was evaluated with different metrics. Results: We first investigate the dependency of matrix density and recrystallization conditions on the thickness of an analyte-empty matrix layer to roughly evaluate the laser shot number required to obtain an intense signal with minimal noise. Then, we introduce metrics for the analysis of small imaging datasets (small sample regions) of model samples based on median quantity of peaks in spectra (medQP) and weighted median signal-to-noise ratio (wmSNR). The evaluation of small regions and taking median values for metrics help overcome the sample heterogeneity and allow for the simultaneous comparison of different acquisition parameters. Conclusions: Here, we propose a methodology based on gradual laser ablation of small regions of sample and further implementation of weighted signal-to-noise ratio to assess various matrix application conditions. The proposed approach helps reduce the number of test samples required to determine optimal sample preparation conditions and improve the overall quality of images. [ABSTRACT FROM AUTHOR]

Rationale: Alkylresorcinols (AR) are cereal-specific biomarkers and have recently been found in archaeological pots. However, their low concentrations and high susceptibility to degradation make them difficult to detect using conventional gas chromatography mass spectrometry (GC/MS). Here we describe the development of a more sensitive liquid chromatography mass spectrometry (LC/MS) method to detect these compounds. Method: A method based on the use of ultra-high-performance liquid chromatography (UHPLC) coupled to an Orbitrap mass analyser was established and validated for the detection of low-concentration ARs in pottery. During the preliminary experiments, UHPLC-Q/Orbitrap MS (ultra-high-performance liquid chromatography-quadrupole/Orbitrap mass spectrometry) was demonstrated to be more sensitive, and a wide range of AR homologues in cereal extracts were detected, unlike UHPLC-QTOFMS (ultra-high-performance liquid chromatography-quadrupole time-of-flight mass spectrometry) and GC/MS. The developed method was utilised to profile AR homologue distribution in modern cereal samples and reanalyse AR-containing pots from the archaeological site of Must Farm. Results: A highly sensitive LC/MS method with a limit of detection (LOD) of 0.02 µg/g and a limit of quantification (LOQ) of 0.06 µg/g was used to profile ARs in five modern cereal grains. The obtained LOD is 250 times lower than that obtained using the conventional GC/MS approach. AR 21:0 was the most abundant homologue in all four Triticum spp.--einkorn, emmer, Khorasan wheat and common wheat. Meanwhile, AR 25:0 was the predominant homologue in barley, potentially enabling differentiation between wheat and barley. The developed LC/MS-based method was successfully used to analyse ARs extracted from Must Farm potsherds and identified the cereal species most likely processed in the pots--emmer wheat. Conclusion: The described method offers an alternative and more sensitive approach for detecting and identifying ARs in ancient pottery. It has been successfully utilised to detect AR homologues in archaeological samples and discriminate which cereal species--wheat and barley--were processed in the pots. [ABSTRACT FROM AUTHOR]

An efficient calculation tool for rigorously optimizing the instrument parameters of matrix‐assisted laser desorption/ionization time‐of‐flight mass spectrometry (MALDI‐TOF MS) is demonstrated in this work. Optimization of MALDI‐TOF MS has been an experience‐based, time‐consuming process without a rigorous theoretical principle. Based on the comprehensive calculation model reported previously, we developed a software tool, MAXTOF, to rapidly determine instrument parameters providing ultimate mass resolving power (MRP). The software conducts big data analysis of most instrument parameters to predict the MRP, including instrument dimensions, voltages, mass‐to‐charge ratio of ions, and ion extraction delay. It can complete the calculation in seconds, providing parameters that serve as the starting point for subsequent optimization that greatly accelerates the optimization process. Experimental validation using a commercial instrument demonstrates MAXTOF's efficacy in predicting optimal parameters and enhancing MRP. The predicted ion extraction delays for bradykinin fragment, P14R polypeptide, and insulin chain B ions were within 5% of the values observed through long‐term optimization. The observed MRP of those ions ranged from 2800 to 4500. Results show that the method and software are highly advantageous for fast and precise measurements. [ABSTRACT FROM AUTHOR]

BACKGROUND: Mangifera indica L. (mango), a medicinal plant rich in biologically active compounds, has potential to be used in disease‐preventing and health‐promoting products. The present investigation reveals and uncovers bioactive metabolites with remarkable therapeutic efficiency from mango (family: Anacardiaceae) seeds. RESULTS: Biological activity was determined by antimicrobial, antioxidant and anticancer assays, and metabolite profiling was performed on gas chromatography coupled to quadrupole time‐of‐flight mass spectrometry (GC‐QTOF‐MS) and liquid chromatography coupled to quadrupole time‐of‐flight mass spectrometry (LC‐QTOF‐MS) platforms. Validation of active metabolites was carried out by in silico molecular docking (Molinspiration Cheminformatics Server and PASS). Extracted and identified metabolites were screened; 54 compounds associated with various groups were selected for the in silico interaction study. CONCLUSIONS: Molecular docking revealed lead molecules with a potential binding energy score, efficacy and stable modulation with a selected protein domain. Investigation, directed by in vitro and in silico analysis, confirms mango seeds as an excellent source of potential metabolites as a therapeutic agent. © 2024 Society of Chemical Industry. [ABSTRACT FROM AUTHOR]

Oxalyl chloride, (ClCO)2$\text{(ClCO)}_2$, is widely used as a photolytic source of Cl atoms in reaction kinetics studies. (ClCO)2$\text{(ClCO)}_2$ photolysis is typically assumed to produce Cl atoms with an overall yield of 2 via three‐body dissociation, (ClCO)2+hν→Cl+CO+ClCO∗$\text{(ClCO)}_2 + h\nu \rightarrow \text{Cl} + \text{CO} + \text{ClCO}^*$, followed by fast subsequent ClCO unimolecular decomposition of either the energetically excited ClCO∗${\rm ClCO}^*$ fragment, ClCO∗→Cl+CO$\text{ClCO}^* \rightarrow \text{Cl} + \text{CO}$, or the thermalized ClCO radical, ClCO+M→Cl+CO+M$\text{ClCO} + \text{M} \rightarrow \text{Cl} + \text{CO} + \text{M}$. However, a study by Huang et al. (J. Phys. Chem. A 121 (2017) 2888–2895) found that UV photolysis of (ClCO)2$\text{(ClCO)}_2$ at 248nm$248\ {\rm nm}$ directly yields Cl2${\rm Cl}_2$ with a photolysis quantum yield of ϕ(Cl2)>14%$\phi (\text{Cl}_2) > 14\%$. This new product pathway may complicate the use of (ClCO)2$\text{(ClCO)}_2$ as a clean source of Cl atoms and challenges the previously accepted photodissociation scheme. The purpose of the present work was 2‐fold. Firstly, the unimolecular decomposition of ClCO∗${\rm ClCO}^*$ and ClCO radicals has been investigated in (ClCO)2$\text{(ClCO)}_2$/C2H6/Ar$\text{C}_{2}\text{H}_6{\rm {/Ar}}$ gas mixtures after UV photolysis at 266$266\ {\rm }$ and 355nm$355\ {\rm nm}$. Cl atoms were captured by C2H6$\text{C}_{2}\text{H}_6$ added in excess such that concentration‐time profiles of HCl measured by means of mid‐infrared frequency modulation spectroscopy reflect the temporally separated Cl formation pathways. The low‐pressure thermal ClCO decomposition rate constant was determined to be k=(1.79±0.17)×10−14cm3molecule−1s−1$k = (1.79 \pm 0.17)\times 10^{-14}\ \text{cm}^{3}\ \text{molecule}^{-1}\ \text{s}^{-1}$ at 295K$295\ {\rm K}$, which is in very good agreement with previously reported literature values. Secondly, the photolysis quantum yield of direct Cl2${\rm Cl}_2$ formation from (ClCO)2$\text{(ClCO)}_2$ photofragmentation was studied with time‐of‐flight mass spectrometry using a photoelectron photoion coincidence setup. Calibrated Cl2${\rm Cl}_2$ concentration‐time profiles were recorded and analyzed using kinetic simulations accounting for both direct and secondary formation of Cl2${\rm Cl}_2$ from photolysis and reactions involving Cl, ClCO, and (ClCO)2$\text{(ClCO)}_2$, respectively. Direct Cl2${\rm Cl}_2$ formation could be confirmed, where wavelength‐dependent quantum yields of ϕ(Cl2)=(5.0±1.6)%$\phi (\text{Cl}_2) = (5.0 \pm 1.6)\%$, (10.0±3.3)%$(10.0 \pm 3.3)\%$, and (5.6±2.0)%$(5.6 \pm 2.0)\%$ at 213nm$213\ {\rm nm}$, 266nm$266\ {\rm nm}$, and 355nm$355\ {\rm nm}$ were determined. Complementary quantum‐chemical calculations of the potential energy diagram for ground‐state photodissociation reveal a low‐lying energy barrier for the formation of phosgene, Cl2CO${\rm Cl}_2{\rm CO}$. We suggest that subsequent Cl2${\rm Cl}_2$ and Cl formation from energetically excited Cl2CO${\rm Cl}_2{\rm CO}$ may actually play a role for the overall photodissociation of (ClCO)2$\text{(ClCO)}_2$. [ABSTRACT FROM AUTHOR]

This document is a compilation of articles that discuss the field of laser materials processing and its applications in various industries. It emphasizes Europe's role in this field and provides an overview of a symposium held during the 2023 Spring Meeting of the European Materials Research Society. The articles cover topics such as laser nanostructuring, up-scaling processing rates, laser direct writing, laser texturing, and surface engineering. The authors provide detailed experimental observations and analysis of their findings, and their biographies highlight their expertise in laser processing. [Extracted from the article]

Rationale: This study overcomes traditional biomass analysis limitations by introducing a pioneering matrix‐free laser desorption/ionization (LDI) approach in mass spectrometry imaging (MSI) for efficient lignin evaluation in wood. The innovative acetic acid–peracetic acid (APA) treatment significantly enhances lignin detection, enabling high‐throughput, on‐site analysis. Methods: Wood slices, softwood from a conifer tree (Japanese cypress) and hardwood from a broadleaf tree (Japanese beech), were analyzed using MSI with a Fourier transform ion cyclotron resonance mass spectrometer. The developed APA treatment demonstrated effectiveness for MSI analysis of biomass. Results: Our imaging technique successfully distinguishes between earlywood and latewood and enables the distinct visualization of lignin in these and other wood tissues, such as the radial parenchyma. This approach reveals significant contrasts in MSI. It has identified intense ions from β‐O‐4‐type lignin, specifically in the radial parenchyma of hardwood, highlighting the method's precision and utility in wood tissue analysis. Conclusions: The benefits of matrix‐free LDI include reduced peak overlap, consistent sample quality, preservation of natural sample properties, enhanced analytical accuracy, and reduced operational costs. This innovative approach is poised to become a standard method for rapid and precise biomass evaluation and has important applications in environmental research and sustainable resource management and is crucial for the effective management of diverse biomass, paving the way towards a sustainable, circular society. [ABSTRACT FROM AUTHOR]

Rationale: With the development of matrix‐assisted laser desorption/ionisation (MALDI) mass spectrometry (MS) in spatial localisation omics research on small molecules, the detection sensitivity of the matrix must increase. However, the types of matrices suitable for detecting acidic small molecules in (−) MALDI‐MS mode are very limited and are either not sensitive enough or difficult to obtain. Methods: More than 10 commercially available benzimidazole and benzothiazole derivatives were selected as MALDI matrices in negative ion mode. MALDI‐MS analysis was performed on 38 acidic small molecules and mouse serum, and the matrix effects were compared with those of the common commercial matrices 9‐aminoacridine (9AA), 1,5‐naphthalenediamine (DAN) and 3‐aminoquinoline (3AQ). Moreover, the proton affinity (PA) of the selected potential matrix was calculated, and the relationships among the compound structure, PA value and matrix effect were discussed. Results: In (−) MALDI‐MS mode, a higher PA value generally indicates a better matrix effect. Amino‐substituted 2‐phenyl‐1H‐benzo[d]imidazole derivatives had well‐defined matrix effects on all analytes and were generally superior to the commonly used matrices 9AA, DAN and 3AQ. Among them, 2‐(4‐(dimethylamino‐phenyl)‐1H‐benzo[d]imidazole‐5‐amine (E‐4) has the best sensitivity and versatility for detecting different analytes and has the best ability to detect fatty acids in mouse serum; moreover, the limit of detection (LOD) of some analytes can reach as low as ng/L. Conclusions: Compared to 9AA, DAN and 3AQ, matrix E‐4 is more effective at detecting low‐molecular‐weight acidic compounds in (−) MALDI‐MS mode, with higher sensitivity and better versatility. In addition, there is a clear correlation between compound structure, PA and matrix effects, which provides a basis for designing more efficient matrices. [ABSTRACT FROM AUTHOR]

Rationale: Solvent‐free sample preparation offers some advantages over solvent‐based techniques, such as improved accuracy, reproducibility and sensitivity, for matrix‐assisted laser desorption/ionization (MALDI) analysis. However, little or no information is available on the application of solvent‐free techniques for the MALDI analysis of polymer blends. Methods: Solvent‐free sample preparation by ball milling was applied with varying sample‐to‐matrix ratios for MALDI time‐of‐flight mass spectrometry analysis of various polymers, including polystyrenes, poly(methyl methacrylate)s and poly(ethylene glycol)s. The peak intensity ratios were compared with those obtained after using the conventional dried droplet sample preparation method. In addition, solvent‐assisted milling was also applied to improve sample homogeneities. Results: Depending on the sample preparation method used, different peak intensity ratios were found, showing varying degrees of suppression of the signal intensities of higher mass polymers. Ball milling for up to 30 min was required to achieve constant intensity ratios indicating homogeneous mixtures. The use of wet‐assisted grinding to improve the homogeneity of the blends was found to be disadvantageous as it caused partial degradation and mass‐dependent segregation of the polymers in the vials. Conclusions: The results clearly show that solvent‐free sample preparation must be carefully considered when applied to synthetic polymer blends, as it may cause additional problems with regard to homogeneity and stability of the blends. [ABSTRACT FROM AUTHOR]

Rationale: As per International Council for Harmonization (ICH) drug stability test guideline Q1A(R2), inherent stability characteristics of a drug should be studied. This work was designed to investigate inherent degradation characteristics of the drug idelalisib under ICH prescribed stress conditions, identify its degradation products, and postulate their corresponding degradation pathways. Methods: Idelalisib was subjected to the ICH prescribed conditions of hydrolytic (neutral, acidic, and alkaline), photolytic, oxidative, and thermal stress according to ICH guideline Q1A(R2). An ultrahigh‐performance liquid chromatography with photodiode array (UHPLC‐PDA) method was developed to adequately resolve the drug from its degradation products, validated as per the ICH guidelines, and subsequently extended to UHPLC with electrospray ionization quadrupole time‐of‐flight mass spectrometry (ESI‐QTOFMS) studies to identify the degradation products. Results: Significant degradation was noted under conditions of acidic/alkaline hydrolysis, acid photolysis, and oxidative stress. The UHPLC/ESI‐QTOFMS studies revealed the generation of four degradation products (I–IV), which were satisfactorily resolved from the drug by UHPLC on a Kinetex® C18 (100 × 4.6 mm; 2.6 μm) column by the developed isocratic elution method. Detection wavelength was selected as 270 nm. All the degradation products (I–IV) could be identified and characterized from their mass spectral data. The degradation pathways for the generation of various products from the drug were postulated. Conclusions: A UHPLC‐PDA method was developed and validated for idelalisib. Four degradation products of idelalisib were revealed through UHPLC/ESI‐QTOFMS studies, and corresponding degradation pathways were postulated for the same. [ABSTRACT FROM AUTHOR]

Rationale: Atmospheric pressure interface multi‐reflection time‐of‐flight mass spectrometry (API‐MRTOF‐MS) has the potential to be a rapid and high‐resolution analytical tool for versatile applications in chemistry, biology, environmental science, and medicine. Methods: The ions were reflected in a mass analyzer via electrostatic mirrors and folded flight path. Therefore, flight distances were significantly increased. The ion flight path of the API‐MRTOF‐MS was extended from meters to over 1 km, and the mass resolution was increased. Furthermore, the mass analysis could be completed at around 10 ms due to the rapid response of TOF‐MS. Results: A high‐resolution API‐MRTOF‐MS approach is successfully developed in this study. The mass resolution could achieve 116 050 (full widths at half maximum [FWHM]) for Cs+ ions using an atmospheric pressure electrospray ionization within a total TOF of only 18 ms. An ion transmission efficiency of over 50% was achieved after 600 cycles. Conclusions: The analytical performance of the newly developed API‐MRTOF‐MS demonstrated that it is suitable for high resolution and rapid analysis in many fields. [ABSTRACT FROM AUTHOR]

SrTiO3 (STO) is a well‐known perovskite oxide often used, among others, as a crystalline substrate for epitaxial deposition. However, its indirect bandgap of 3.25 eV is too high for solar applications. Tentative experiments to reduce its bandgap are very welcome. To this end, sulfurization of STO substrates using ion implantation is performed. The simulated profile is controlled by time‐of‐flight secondary‐ion mass spectrometry. S is at least partially inserted into the STO lattice, as evidenced by X‐ray diffraction and X‐ray photoelectron spectroscopy. UV–vis spectroscopy indicates a drastic reduction of the bandgap of S:STO from 3.25 eV (indirect) down to 2.14 eV for 10% S:STO, a trend also observed by spectroscopic ellipsometry. The results are confronted to ab initio calculations. Besides bandgap, the valence band level, that is the ionization energy, is determined by ambient‐pressure photoemission spectroscopy so that the complete energy diagrams could be plotted. This work paves the way for tuning the bandgap of perovskites in a highly controlled manner for solar energy applications. [ABSTRACT FROM AUTHOR]

Taibai ginseng (roots of Pedicularis decora Franch.) has been reported to possess anti‐Alzheimer's disease (anti‐AD) activity and can be potentially used for treating AD. However, the chemical constituents of taibai ginseng have not yet been elucidated because of the paucity of relevant studies, which hinders further research on the pharmacological mechanism and utilization of taibai ginseng. In this study, a rapid and efficient method for comprehensively analyzing the chemical constituents of taibai ginseng was established for the first time. We used ultra‐high performance liquid chromatography‐quadrupole time of flight mass spectrometry in combination with the UNIFI data‐processing platform to automatically characterize and identify the chemical profile of taibai ginseng. As a result, more than 76 compounds were detected, and their structures were characterized. These compounds include 24 iridoid glycosides, 24 phenylethanol glycosides, 15 terpenoids, and 13 other components. More than fifty of these compounds from taibai ginseng were reported for the first time. Our results provide a reference for the quality control of taibai ginseng and establish a higher quality standard for pharmacodynamic research. Appropriate modification of the method reported herein can enable its use for the screening and characterization of taibai ginseng and other compounds from the Pedicularis genus. [ABSTRACT FROM AUTHOR]

Summary: Fermentation of yellow maize using different inocula yields mahewu products with varying compositions. Comprehensive analysis of the metabolites influencing distinctive characteristics of mahewu from sorghum malt (YMSM); wheat (YMW), malted millet (YMMM) and malted yellow maize (YMYM) inocula was investigated using an untargeted gas chromatography high‐resolution time‐of‐flight mass spectrometry (GC‐HRTOF‐MS)‐based metabolomics. Metabolites in mahewu from different inocula included phenols, fatty acid methyl ester (FAME), benzenes, amides, amines, cyclic compounds, fatty acid ethyl esters (FAEEs), esters, ketones and vitamins which differentiated metabolites identified in raw yellow maize (RYM). Principal component analysis (PCA) showed that the mahewu and related inocula were distinguished across PC1 and PC2. The OPLS‐DA result further intensifies the significant (P ≤ 0.05) metabolite causing variations among samples. This study serves as the first report into the metabolome of yellow maize mahewu from different inocula, serving as a foundation for the quality control of mahewu products for further research. [ABSTRACT FROM AUTHOR]

Piper longum L. (long pepper) is an economically and industrially important medicinal plant. However, the characterization of its volatiles has only been analyzed by gas chromatography–mass spectrometry (GC–MS). In the present study, precise characterization of P. longum fruit volatiles has been performed for the first time through advanced two‐dimensional gas chromatography–time‐of‐flight spectrometry (GC×GC–TOFMS). A total of 146 constituents accounting for 93.79% were identified, of which 30 were reported for the first time. All these constituents were classified into alcohols (4.5%), alkanes (8.9%), alkenes (6.71%), esters (6.15%), ketones (0.58%), monoterpene hydrocarbons (1.64%), oxygenated monoterpenes (2.24%), sesquiterpene hydrocarbons (49.61%), oxygenated sesquiterpenes (13.03%), phenylpropanoid (0.23%), and diterpenes (0.2%). Among all the classes, sesquiterpene hydrocarbons were abundant, with germacrene‐D (2.87% ± 0.01%) as the major one, followed by 8‐heptadecene (2.69% ± 0.03%), β‐caryophyllene (2.43% ± 0.03%), n‐heptadecane (2.4% ± 0.04%), n‐pentadecane (2.11% ± 0.05%), and so forth. Further, 20 constituents were observed to be coeluted and separated precisely in the two‐dimensional column. The investigation provides an extensive metabolite profiling of P. longum fruit volatiles, which could be helpful to improve its therapeutic potential. [ABSTRACT FROM AUTHOR]

Hua‐ju‐hong (HJH) is a Chinese medicinal material obtained from Citrus grandis 'Tomentosa' (CGT) and Citrus grandis (L.) Osbeck (CG) with various commercial specifications. It is known for relieving cough and dispelling phlegm. To reveal the quality marker for distinguishing the various HJH, 215 batches of commercial HJH were studied systematically using multidimensional chemical analysis. Ten major components were identified by high‐performance liquid chromatography coupled with quadrupole‐time‐of‐flight mass spectrometry and quantified via high‐performance liquid chromatography coupled with diode array detection. In this study, a rapid, efficient, and low‐cost chromatographic method was established. Total coumarin‐hemiterpene and total coumarin‐monoterpene were first classified and analyzed in HJH. The result indicated that the main component, naringin, was not the quality marker for differentiating CGT from CG. For reflecting the unique medicinal and food value of HJH, coumarins should be the more potential quality markers. Flavonoids were the possible quality markers for distinguishing two growth stages of fruit‐exocarp and young fruit. For the first time, two chemotypes of HJH were identified in CG. This study provides a convenient yet reliant chromatographic method and novel yet systematic strategies for overall quality control of commercial HJH. [ABSTRACT FROM AUTHOR]

Objectives: Cold storage is being implemented as an alternative to conventional room‐temperature storage for extending the shelf‐life of platelet components beyond 5–7 days. The aim of this study was to characterise the lipid profile of platelets stored under standard room‐temperature or cold (refrigerated) conditions. Methods: Matched apheresis derived platelet components in 60% PAS‐E/40% plasma (n = 8) were stored at room‐temperature (20–24°C with agitation) or in the cold (2–6°C without agitation). Platelets were sampled on day 1, 5 and 14. The lipidome was assessed by ultra‐pressure liquid chromatography ion mobility quadrupole time of flight mass spectrometry (UPLC IMS QToF). Changes in bioactive lipid mediators were measured by ELISA. Results: The total phospholipid and sphingolipid content of the platelets and supernatant were 44 544 ± 2915 μg/mL and 38 990 ± 10 880 μg/mL, respectively, and was similar over 14 days, regardless of storage temperature. The proportion of the procoagulant lipids, phosphatidylserine (PS) and phosphatidylethanolamine (PE), increased by 2.7% and 12.2%, respectively, during extended cold storage. Cold storage for 14 days increased sphingomyelin (SM) by 4.1% and decreased ceramide by 1.6% compared to day 1. Further, lysophosphatidylcholine (LPC) species remained unchanged during cold storage for 14 days. The concentration of 12‐ and 15‐hydroxyeicosatetraenoic acid (HETE) were lower in the supernatant of cold‐stored platelets than room‐temperature controls stored for 14 days. Conclusion: The lipid profile of platelets was relatively unchanged during storage for 5 days, regardless of temperature. However, during extended cold storage (14 days) the proportion of the procoagulant lipids, PS and PE, increased, while LPC and bioactive lipids were stable. [ABSTRACT FROM AUTHOR]

Context: Qi‐dan‐dihuang decoction (QDD) has been used to treat diabetic kidney disease (DKD), but the underlying mechanisms are poorly understood. Objective: This study reveals the mechanism by which QDD ameliorates DKD. Materials and Methods: The compounds in QDD were identified by high‐performance liquid chromatography and quadrupole‐time‐of‐flight tandem mass spectrometry (HPLC‐Q‐TOF‐MS). Key targets and signaling pathways were screened through bioinformatics. Nondiabetic Lepr db/m mice were used as control group, while Lepr db/db mice were divided into model group, dapagliflozin group, 1% QDD‐low (QDD‐L), and 2% QDD‐high (QDD‐H) group. After 12 weeks of administration, 24 h urinary protein, serum creatinine, and blood urea nitrogen levels were detected. Kidney tissues damage and fibrosis were evaluated by pathological staining. In addition, 30 mmol/L glucose‐treated HK‐2 and NRK‐52E cells to induce DKD model. Cell activity and migration capacity as well as protein expression levels were evaluated. Results: A total of 46 key target genes were identified. Functional enrichment analyses showed that key target genes were significantly enriched in the phosphatidylinositol 3‐kinase (PI3K)/protein kinase B (AKT) and mitogen‐activated protein kinase (MAPK) signaling pathways. In addition, in vivo and in vitro experiments confirmed that QDD ameliorated renal fibrosis in diabetic mice by resolving inflammation and inhibiting the epithelial‐mesenchymal transition (EMT) via the p38MAPK and AKT‐mammalian target of rapamycin (mTOR) pathways. Discussion and Conclusion: QDD inhibits EMT and the inflammatory response through the p38MAPK and AKT/mTOR signaling pathways, thereby playing a protective role in renal fibrosis in DKD. [ABSTRACT FROM AUTHOR]

A 6-year-old 21.5 kg castrated male Siberian Husky was presented for acute onset of lethargy, vomiting, hemorrhagic diarrhea, and inappetence. Physical examination revealed marked discomfort upon abdominal palpation and 5%–7% dehydration. The CBC and biochemical profile revealed changes consistent with mild to moderate inflammation, dehydration, and gastrointestinal (GI) disease. Despite aggressive gastrointestinal support, anorexia persisted, and an upper GI endoscopy was performed in conjunction with esophagostomy tube placement. Endoscopy revealed abnormal gastric mucosa characterized by moderately well-demarcated areas of blue-black discoloration. Impression smears of a gastric biopsy revealed abundant extracellular yeasts with morphology most consistent with Candida spp. and frequent extracellular cocci. Similar yeast and bacteria, in lower numbers, were observed on cytologic analysis of a direct smear of the rectal mucosa. A rectal swab submitted for fungal culture yielded pure growth of fungal yeasts identified as Diutina (formerly Candida) rugosa by matrix-assisted laser desorption-ionization time-of-flight mass spectrometry. The dog's clinical signs improved with fluconazole, and he was discharged. Follow-up fungal culture of a rectal swab showed no growth of D. rugosa. To the authors' knowledge, this is the first case report that describes the clinical, hematologic, cytologic, and gross findings of enteric colonization by D. rugosa in a dog. [ABSTRACT FROM AUTHOR]

With the ongoing mutation of severe acute respiratory syndrome coronavirus 2 (SARS‐CoV‐2) leading to various variants, there is an urgent need for new diagnostic methods for SARS‐CoV‐2 infection. The existing nucleic acid test and antigen test suffer from long assay time and low sensitivity, respectively. Matrix‐assisted laser desorption/ionization time‐of‐flight mass spectrometry (MALDI‐TOF MS)‐based nasal swabs analysis have been demonstrated as a promising technique in SARS‐CoV‐2 infection screening. However, the applicability of the technique in the different variants of SARS‐CoV‐2 is uncertain. Given the prevalence of the Omicron variant since 2022, we developed a MALDI‐TOF‐based diagnosis method with nasal swab samples to detect the infection by this variant. We collected 325 SARS‐CoV‐2‐positive and 221 SARS‐CoV‐2‐negative nasal swab samples, and the molecular mass fingerprints were acquired from the samples by MALDI‐TOF MS. Using a random forest machine learning classification model to analyze the molecular mass fingerprints MALDI‐TOF mass spectra, the accuracy of 97%, false negative rate of 0%, and false positive rate of 7.6% were achieved for the diagnosis of SARS‐CoV‐2 infection. Combining the MALDI‐TOF analysis with top‐down proteomics, we identified four potential protein biomarkers, that is, humanin‐like 4, thymosin beta‐10, thymosin beta‐4 and statherin, in the nasal swab for the diagnosis of coronavirus disease 2019. It was further found that the four protein biomarkers can also differentiate the SARS‐CoV‐2 original strains infection and Omicron strains infection. These results suggest that the MALDI‐TOF MS‐based nasal swab analysis holds effective diagnostic capabilities of SARS‐CoV‐2 infection, and shows promising potential for global application and extension to other infectious diseases. [ABSTRACT FROM AUTHOR]

Objective: Acute mortality with clinical symptoms of streptococcal‐like infections was observed in red tilapia Oreochromis sp. cultured in floating cages in Prachin Buri Province, Thailand, during May 2023. Herein, we identified an emerging pathogen, Lactococcus garvieae, as the etiological agent. Methods: After bacterial isolation from the brain and kidney of diseased fish, identification was performed using matrix‐assisted laser desorption/ionization time‐of‐flight mass spectrometry and the VITEK 2 system. Sequencing of the 16S ribosomal RNA (rRNA) gene and phylogenetic analysis were applied to confirm bacterial species. Antimicrobial susceptibility testing was conducted. Histopathological findings in the brain, kidney, spleen, liver, and heart were evaluated. Result: From 20 fish samples, L. garvieae (n = 18 isolates) and Streptococcus agalactiae (n = 2 isolates) were identified. A phylogenetic tree of the 16S rRNA gene revealed that Thai isolates of either L. garvieae or S. agalactiae clustered with reference piscine isolates from intercontinental locations. Our isolates showed resistance against quinolones while being susceptible to other antimicrobials. Histopathological changes demonstrated severe septicemic conditions, with more invasive lesions—especially in the heart and liver—being apparent in L. garvieae‐infected fish compared to S. agalactiae‐infected fish. Conclusion: This study represents the first reported outbreak of L. garvieae with a concurrent S. agalactiae infection in farmed red tilapia in Thailand. Impact statementAn emerging pathogen, Lactococcus garvieae, was isolated from red tilapia in Thailand during May 2023. Concurrent infection by Streptococcus agalactiae was also diagnosed. Although the clinical findings and antimicrobial resistance patterns of these bacterial isolates were comparable, the observed histopathological lesions caused by L. garvieae were more severe. [ABSTRACT FROM AUTHOR]

Rationale: Lomefloxacin hydrochloride ear drops are highly unstable to light and prone to produce photodegradation impurities. These impurities might be related to the phototoxicity of lomefloxacin, which could seriously threaten the health of patients. In this article, the photodegradation impurity profile in lomefloxacin hydrochloride ear drops was studied for further improvement of quality control of the drug. Methods: By studying the chromatographic behavior of photodegradation impurities, the photodegradation impurities in lomefloxacin hydrochloride ear drops were separated and detected effectively. Liquid chromatography combined with ion trap/time‐of‐flight mass spectrometry was applied to characterize the structures of the photodegradation impurities in lomefloxacin hydrochloride ear drops. Results: The structures of 17 impurities in lomefloxacin hydrochloride ear drops were elucidated based on high‐resolution MSn data in positive ion mode, 12 of them being unknown impurities. Conclusions: The structural characteristics and fragmentation patterns of the photodegradation impurities were also studied. The study of the photodegradation impurity profile in lomefloxacin hydrochloride ear drops provides a scientific basis for quality control of these ear drops and ensures the safety of drug use by the public. [ABSTRACT FROM AUTHOR]

Rational: Pogejiuxin decoction (PGJXD) is one of the most important formulas for the treatment of heart failure. However, there is a great lack of research on the material basis of this formula, especially research on its compatibility laws, which restricts its clinical use. Studying the complete ingredients and compatibility rules of PGJXD has great significance for guiding clinical medication. Methods: The entire formula, the major single herbs, the drug pairs and the disassembled formula were analyzed by ultrahigh‐performance liquid chromatography with quadrupole time‐of‐flight mass spectrometry (UHPLC/QTOFMS/MS), matching the chemical composition database and global natural product social molecular networking to explain the chemical composition as well as the combination pattern of PGJXD. Results: A total of 1048 chemical constituents were fully analyzed from the major single herbs, the drug pairs and the disassembled formula and 188 chemical constituents, including 13 potential novel compounds, were firstly identified from the whole formula. We found that the chemical compositions were reduced after the single herbs were matched to the other herbs, especially the significant reduction of highly toxic diester alkaloids after compatibility, indicating that the medicines of PGJXD were interdependent and controlled by each other. Conclusion: This study innovatively researches and compares the compositional differences between the entire formula of PGJXD, the single, paired and separated formulas, greatly extending our understanding of the chemical substance basis of these compounds, and preliminarily explores the compatibility laws of PGJXD, providing some theoretical guidance for clinical medication. [ABSTRACT FROM AUTHOR]

BACKGROUND: Enzymatic crosslinking is a method that can be used to modify Inca peanut albumin (IPA) using polyphenols, and provides desirable functionalities; however, the effect of polyphenol structures on conjugate properties is unclear. In this study, we selected four polyphenols with different numbers of phenolic hydroxyl groups [para‐hydroxybenzoic acid (HBA), protocatechuic acid (PCA), gallic acid (GA), and epigallocatechin gallate (EGCG)] for covalent modification of IPA by enzymatic crosslinking, and explored the structure–function changes of the IPA–polyphenol conjugates. RESULTS: Sodium dodecyl sulfate‐polyacrylamide gel electrophoresis (SDS‐PAGE) and matrix‐assisted laser desorption/ionization time‐of‐flight mass spectrometry (MALDI‐TOF‐MS) analysis showed that laccase successfully promoted covalent crosslinking of IPA with polyphenols, with the order of degree of conjugation as EGCG > GA > PCA > HBA, the IPA–EGCG conjugate showed the highest polyphenol binding equivalents (98.35 g kg−1 protein), and a significant reduction in the content of free amino, sulfhydryl, and tyrosine group. The oxidation of polyphenols by laccase forms quinone or semiquinone radicals that are covalently crosslinked to the reactive groups of IPA, leading to significant changes in the secondary and tertiary structures of IPA, with spherical structures transforming into dense lamellar structures. The 2,2‐diphenyl‐1‐picrylhydrazyl (DPPH) radical scavenging ability and emulsification stability of IPA–EGCG conjugates improved by almost 6‐fold and 2.7‐fold, respectively, compared with those of unmodified IPA. CONCLUSION: These data suggest that the higher the number of polyphenol hydroxyl groups, the higher the degree of IPA–polyphenol conjugation; additionally, enzymatic crosslinking can significantly improve the functional properties of IPA. © 2024 Society of Chemical Industry. [ABSTRACT FROM AUTHOR]

Shengxian decoction, a traditional Chinese medicinal prescription, has been shown to alleviate doxorubicin‐induced chronic heart failure. This study established an ultra‐performance liquid chromatography‐quadrupole time‐of‐flight mass spectrometry method to separate and characterize the complex chemical compositions of Shengxian decoction, and the absorbed compounds in the bio‐samples of the cardiotoxicity rats with chronic heart failure after its oral delivery. Note that 116 chemical compounds were identified from Shengxian decoction in vitro, 81 more than previously detected. Based on the three‐dimensional data of these compounds, 28 absorbed compounds were confirmed in vivo. Network pharmacology and molecular docking experiments indicated that timosaponin B‐II, timosaponin A‐III, gitogenin, and 7,8‐didehydrocimigenol were recognized as the key effective compounds to exert effects against doxorubicin cardiotoxicity by acting on targets such as caspase 3, cyclin‐dependent kinase 1, cyclin‐dependent kinase 4, receptor tyrosine‐protein kinase erbB‐2, and mitogen‐activated protein kinase 1 in p53 and phosphatidylinositol 3‐kinase‐Akt signaling pathways. This study developed the understanding of the composition of Shengxian decoction for the treatment of doxorubicin cardiotoxicity, as well as a feasible strategy to elucidate the effective constituents in traditional Chinese medicines. [ABSTRACT FROM AUTHOR]

The present research aimed to comprehensively investigate the forced degradation of tepotinib through a combined in‐silico and experimental analysis. Tepotinib is a recently approved drug for metastatic non‐small cell lung cancer. A short and precise ultra‐high‐performance liquid chromatography (UHPLC) method utilizing a CSH C18 column (100 × 2.1 mm, 1.7 μm) was developed, using a mobile phase A as 0.1% formic acid and mobile phase B as HPLC‐grade acetonitrile. The flow rate was set at 0.2 mL/min, and detection was carried out at 260 nm. Forced degradation was carried out under acidic, basic, oxidative, and photolytic environments and also virtually with Zeneth software. Structural characterization of degradation products (DPs) was carried out using hyphenated techniques such as LC‐quadrupole time‐of‐flight‐tandem mass spectrometry in positive electrospray ionization mode. Further, toxicity was assessed with Derek and Sarah software. Analysis revealed the formation of five distinct forced DPs: DP‐1 (m/z 511), DP‐2 (m/z 527), DP‐3 (m/z 525), DP‐4 (m/z 512), and DP‐5 (m/z 509) under experimental conditions and eight in Zeneth prediction. Furthermore, nephrotoxicity alerts were observed for DP‐3 and DP‐5, whereas DP‐3 also showed mutagenicity alerts. This integrated blend of in‐silico and real experimental analyses was found to be effective in quality control for routing monitoring of degradation products of tepotinib. [ABSTRACT FROM AUTHOR]

Summary: The nutritional value of Hainan camellia oil is incomparable to other places, and Hainan camellia oil is expensive, so unscrupulous businessmen often mix other edible oils into them for illegal profit. This study detected the changes of volatile components in Hainan camellia oil adulterated with five edible oils (peanut, soybean, corn, rapeseed, and sunflower oils) using comprehensive two‐dimensional gas chromatography and quadrupole time‐of‐flight mass spectrometry (HS‐SPME‐GC × GC‐Q‐TOFMS). The principal component analysis (PCA) score plot showed that pure Hainan camellia oil (PHCO) and Hainan camellia oil samples were adulterated with other edible oils clearly to identify the adulteration separated from each other. The adulteration of PHCO could be accurately predicted using the developed PCA and OPLS‐DA models for concentrations as low as 5%. More importantly, several potential markers were found to identify the impersonate PHCO. Therefore, the volatile compound determination based on HS‐SPME‐GC × GC‐Q‐TOFMS proved to be an effective method for detecting adulteration of other edible oils in PHCO. [ABSTRACT FROM AUTHOR]

Host immunity can influence the composition of the gut microbiota and consequently affect disease progression. Previously, we reported that a Mycobacterium vaccae vaccine could ameliorate allergic inflammation in asthmatic mice by regulating inflammatory immune processes. Here, we investigated the anti‐inflammatory effects of M. vaccae on allergic asthma via gut microbiota modulation. An ovalbumin (OVA)‐induced asthmatic murine model was established and treated with M. vaccae. Gut microbiota profiles were determined in 18 BALB/c mice using 16S rDNA gene sequencing and metabolomic profiling was performed using liquid chromatography quadrupole time‐of‐flight mass spectrometry. Mycobacterium vaccae alleviated airway hyper‐reactivity and inflammatory infiltration in mice with OVA‐induced allergic asthma. The microbiota of asthmatic mice is disrupted and that this can be reversed with M. vaccae. Additionally, a total of 24 differential metabolites were screened, and the abundance of PI(14:1(9Z)/18:0), a glycerophospholipid, was found to be correlated with macrophage numbers (r = 0.52, p = 0.039). These metabolites may affect chemokine (such as macrophage chemoattractant protein‐1) concentrations in the serum, and ultimately affect pulmonary macrophage recruitment. Our data demonstrated that M. vaccae might alleviate airway inflammation and hyper‐responsiveness in asthmatic mice by reversing imbalances in gut microbiota. These novel mechanistic insights are expected to pave the way for novel asthma therapeutic strategies. [ABSTRACT FROM AUTHOR]

The preparation process from waste fibers to regenerated fibers is an environmental significance work. In this work, liquid chromatography/time‐of‐flight mass spectrometry, advanced polymer chromatography/multi‐angle laser‐light‐scattering/refractive index detector, and two‐dimensional wide‐angle X‐ray diffractometry were employed to characterize the polycaprolactam(PA6) fibers above oligomers composition and content, molecular weight and distribution, crystallization and orientation, and analyzing the changes in mechanical properties. The total content of oligomers in physical and chemical regenerated PA6 fiber is 2.084 wt% and 1.812 wt%, individually, which is higher than that in waste PA6 fiber. And the oligomer content of C1–C4 (cyclic monomer, cyclic dimer, cyclic trimer, and cyclic tetramer) in the regenerated PA6 fiber is higher than that of waste PA6 fiber. The regenerated PA6 fiber sample contains more low‐molecular‐weight substances, making it easier to form crystal nuclei and crystallize. During the dyeing process of the regenerated PA6 fiber, the γ crystal transformed into α crystal. The tensile strength of physical and chemical regenerated PA6 fiber is lower than that of waste PA6 fiber. And after dyeing, the oligomers content of regenerated PA6 fiber is significantly decreased, especially in C1–C4 oligomer. However, the crystalliniy and orientation of regenerated PA6 fibers were improved, which also leads to the fracture strength increased by about 20% compared to undyed fibers. [ABSTRACT FROM AUTHOR]

BACKGROUND: Parkia biglobosa stem bark extracts were prepared using methanol, methanol 80%, water and ethyl acetate to investigate their phytochemical contents, as well as antioxidant and enzyme inhibitory properties. RESULTS: Liquid chromatography (LC) quadrupole time-of-flight mass spectrometry (MS) and LC-MSn revealed the presence of flavonoids, hydroxycinnamic acid derivatives and gallotannins. Particularly, the water extract contained rutin (480 ~g per 100 mg) and 3-caffeoylquinic acid (1109 ~g per 100 mg) in higher amounts, whereas the 80% methanol extract contains methoxyluteolin-7-O-rutinoside and catechin derivatives as major compounds. Total phenolic and flavonoid contents of the extracts were yielded in the range of 32.26-119.88 mg gallic acid equivalents g-1 and 0.60-2.39 mg rutin equivalents g-1, respectively. Total antioxidant capacity was also displayed in the range of 0.53-6.34 mmol Trolox equivalents (TE) g-1. Both the methanolic extracts showed higher total antioxidant capacity that could be related to the total phenolic contents. Radical scavenging capacity in DPPH (2,2-diphenyl-2-picryl-hydrazyl) (37.21-508.30 mg TE g-1) and ABTS [2,2-azinobis(3-ethylbenzothiazoline-6-sulfonic acid)] (60.95-1068.06 mg TE g-1) assays, reducing power in cupric ion reducing antioxidant capacity (54.23-1002.78 mg TE g-1) and ferric ion reducing antioxidant power (33.18-558.68 mg TE g-1) assays, as well as metal chelating activity (2.45-11.28 mg EDTA equivalents g-1), were exhibited by all extracts. All extracts were found to inhibit acetylcholinesterase [0.23-2.47 mg galanthamine equivalents (GALAE) g-1], tyrosinase [27.20-83.33 mg kojic acid equivalents g-1], amylase [mmol acarbose equivalents (ACAE) g-1]. On the other hand, all extracts, except the water extract, inhibited butyrylcholinesterase (5.38-6.56 mg GALAE g-1), whereas only the water and ethyl acetate extract showed glucosidase inhibitory potential (1.96 and 1.82 mmol ACAE g-1). In general, the water extract was found to be a weaker enzyme inhibitor suggesting that water is not the preferrable extraction solvent to obtain active products. CONCLUSION: The present study demonstrated that the stem bark extracts of P. biglobosa contains good amount of phytochemical and extracts present significant antioxidant, as well as reasonable enzyme inhibitory effects. Hence, these findings suggest that further studies can be performed on more specific biological targets and models of bioactivity to determine their safe usage as a nutraceutical or for the preparation functional foods. [ABSTRACT FROM AUTHOR]

Jupiter's plasma sheet has been understood to be primarily composed of Io‐genic sulfur and oxygen, along with protons at lower mass density. These ions move radially away from Jupiter, filling its magnetosphere. The material in the plasma sheet interacts with Europa, which is also a source of magnetospheric pickup ions, primarily hydrogen and oxygen. Juno's thermal plasma instrument JADE, the Jovian Auroral Distributions Experiment, has provided comprehensive in situ observations of the composition of Jupiter's plasma sheet ions with its Time‐of‐Flight mass‐spectrometry capabilities. Here, we present observations of the magnetospheric composition in the Europa‐Ganymede region of Jupiter's magnetosphere. We find material from Europa is intermittently present at comparable densities to Io‐genic plasma. The intermittency of Europa‐genic signatures suggests Europa's neutral oxygen toroidal cloud is more localized to Europa's vicinity than its hydrogen cloud. These observations reveal a more complex and compositionally diverse magnetosphere than previously thought. Plain Language Summary: Jupiter's charged particle environment is overwhelmingly driven by material lost from Io. This material interacts with the icy moon Europa, which can also inject charged particles into the environment. We find that Europa appreciably contributes to and modifies its local charged particle environment, revealing a more complex and compositionally diverse magnetosphere than previously thought. Key Points: Three distinct heavy ion populations observed in Jupiter's plasma sheet: Io‐genic plasma, Europa‐genic plasma, and Io‐genic energetic particlesThe mixture of Io‐genic and Europa‐genic plasma varies greatly throughout the Europa‐Ganymede regionWe find evidence Europa's oxygen neutral toroidal clouds are more localized than its hydrogen cloud [ABSTRACT FROM AUTHOR]

Detecting exosomal markers using laser desorption/ionization time‐of‐flight mass spectrometry (LDI‐TOF MS) is a novel approach for examining liquid biopsies of non‐small cell lung cancer (NSCLC) samples. However, LDI‐TOF MS is limited by low sensitivity and poor reproducibility when analyzing intact proteins directly. In this report, gold nanoparticles/cellulose nanocrystals (AuNPs/CNC) is introduced as the matrix for direct analysis of intact proteins in NSCLC serum exosomes. AuNPs/CNC with "dual dispersion" effects dispersed and stabilized AuNPs and improved ion inhibition effects caused by protein aggregation. These features increased the signal‐to‐noise ratio of [M+H]+ peaks by two orders of magnitude and lowered the detection limit of intact proteins to 0.01 mg mL–1. The coefficient of variation with or without AuNPs/CNC is measured as 10.2% and 32.5%, respectively. The excellent reproducibility yielded a linear relationship (y = 15.41x – 7.983, R2 = 0.989) over the protein concentration range of 0.01 to 20 mg mL–1. Finally, AuNPs/CNC‐assisted LDI‐TOF MS provides clinically relevant fingerprint information of exosomal proteins in NSCLC serum, and characteristic proteins S100 calcium‐binding protein A10, Urokinase plasminogen activator surface receptor, Plasma protease C1 inhibitor, Tyrosine‐protein kinase Fgr and Mannose‐binding lectin associated serine protease 2 represented excellent predictive biomarkers of NSCLC risk. [ABSTRACT FROM AUTHOR]

BACKGROUND: Three different organic sunflower seed cakes, produced from seeds differing in the content of their hulls, were extracted by two different extraction methods – conventional extraction (CE) and ultrasound‐assisted extraction (UAE). The total phenolic compound (TPC) content of the extracts was evaluated using Folin–Ciocâlteu reagent (FCR) and high‐performance liquid chromatography (HPLC). The antioxidant capacity of extracts was evaluated with the Trolox equivalent antioxidant capacity (TEAC) and 2,2‐diphenyl‐1‐picrylhydrazyl (DPPH) assays. RESULTS: The results showed that both extracts displayed high TPC content and antioxidant capacity. The UAE method showed significantly higher TPC content and antioxidant capacity values than CE. Individual phenolic compounds such as chlorogenic acid (CGA) isomers (3‐, 4‐ and 5‐O‐caffeoylquinic acids), di‐CGA isomers, and feruloylquinic and coumaroylquinic acids were identified according to their exact masses by HPLC coupled to time‐of‐flight mass spectrometry. CONCLUSION: The results revealed that the UAE method could be used effectively to facilitate the extraction of phenolic compounds from sunflower seed cake. © 2023 The Authors. Journal of The Science of Food and Agriculture published by John Wiley & Sons Ltd on behalf of Society of Chemical Industry. [ABSTRACT FROM AUTHOR]

BACKGROUND: Aroma is one of the most important quality criterion of different honeys and even defines their merchant value. The composition of volatile compounds, especially the characteristic odor‐active compounds, contributes significantly to the aroma of honey. Evodia rutaecarpa (Juss) Benth honey (ERBH) is a special honey in China with unique flavor characteristics. However, no work in the literature has investigated the volatile compounds and characteristic odor‐active compounds of ERBHs. Therefore, it is imperative to conduct systematic investigation into the volatile profile, odor‐active compounds and odor properties of ERBHs. RESULTS: The characteristic fingerprint of ERBHs was successfully constructed with 12 characteristic peaks and a similarity range of 0.785–0.975. In total, 297 volatile compounds were identified and relatively quantified by headspace solid‐phase microextraction coupled with gas chromatography quadrupole time‐of‐flight mass spectrometry, of which 61 and 31 were identified as odor‐active compounds by relative odor activity values and GC‐olfactometry analysis, respectively, especially the common 22 odor‐active compounds (E)‐β‐damascenone, phenethyl acetate, linalool, cis‐linalool oxide (furanoid), octanal, hotrienol, trans‐linalool oxide (furanoid), 4‐oxoisophorone and eugenol, etc., contributed significantly to the aroma of ERBHs. The primary odor properties of ERBHs were floral, followed by fruity, herbaceous and woody aromas. The partial least‐squares regression results showed that the odor‐active compounds had good correlations with the odor properties. CONCLUSION: Identifying the aroma differences of different honeys is of great importance. The present study provides a reliable theoretical basis for the quality and authenticity of ERBHs. © 2023 Society of Chemical Industry. [ABSTRACT FROM AUTHOR]

Summary: Cereal‐based diets supplemented with legumes have proven to be an effective approach to enhancing nutritional value. This study evaluated the consumer acceptability and metabolite profile of fermented sorghum mahewu improved with different proportions (20% and 30%) of Bambara groundnut (BGN). Consumer acceptability, metabolite profile analysis using gas chromatography high‐resolution time‐of‐flight mass spectrometry (GC‐HRTOF‐MS), storage stability and microbial quality of mahewu were determined. Sorghum (100SORG) mahewu without BGN was the most preferred by the consumer panellists followed by 80SORG:20BGN. Metabolites identified in all three mahewu products included esters (21%), alcohols (17%), alkanes (12%), acids and derivatives (9%). Overall, 70SORG:30BGN had an improved metabolite profile but least preferred by consumer. The sorghum‐BGN mahewu maintained their pH, while increases in consistency and TTA were observed with storage time and BGN supplementation. Inclusion of BGN in sorghum mahewu did not alter microbial quality; however, more awareness is required to increase its acceptance among consumers. [ABSTRACT FROM AUTHOR]

Qi‐Wei‐Tong‐Bi oral liquid (QWTB), a famous Chinese medicine preparation composed of seven crude drugs has a good therapeutic effect on rheumatoid arthritis and is widely used in China. However, its chemical composition and quality control have not been comprehensively and systematically investigated. In this study, high‐performance liquid chromatography coupled with quadrupole time‐of‐flight mass spectrometry was employed for its chemical profiling. As a result, 100 components were chemically characterized. Additionally, high‐performance liquid chromatography coupled with a quadrupole linear ion trap mass spectrometry method was developed to simultaneously quantify nine bioactive components (hyperoside, ononin, quercetin, sinomenine, magnoflorine, gallic acid, protocatechuic acid, monotropein, and cyclo‐(Pro‐Tyr)) in multiple‐reaction monitoring mode. After successful validation in terms of linearity, precision, repeatability, and recovery, the assay method was applied for the determination of 10 batches of QWTB. The results showed that QWTB was enriched in sinomenine and magnoflorine with the highest amount up to hundreds or even thousands of µg/mL, while quercetin, ononin, cyclo‐(Pro‐Tyr), and hyperoside were much lower with the lowest content below 10 µg/mL. This study work would help to reveal the chemical profiling and provide a valuable and reliable approach for quality evaluation and even pharmacodynamic material basis studies of QWTB. [ABSTRACT FROM AUTHOR]

With the development in the early 2000s of new cluster ion sputtering sources, a reliable analysis of organic multilayers and interfaces has become possible. Nowadays, time‐of‐flight secondary ion mass spectrometry (ToF‐SIMS) and X‐ray photoelectron spectroscopy (XPS) depth profiling are routinely used to investigate organic stacks. However, analysis beams can cause bond scission or beam‐induced degradations that accumulate in buried layers. We developed a correlative protocol that minimises damages related to analysis beams. It uses a shallow angle bevel crater fabricated inside the ToF‐SIMS analysis chamber. With this preparation method, the in‐depth information is displayed over the surface of the bevel crater. XPS profiles and high‐resolution spectra paired with ToF‐SIMS images enable an easy identification of the organic layers and complete understanding of their chemistry. The reduction of beam‐induced degradation is achieved by minimising the acquisition times, therefore beam exposure on materials. Finally, an important advantage of this preparation method is that the analysis can be performed on exactly the same spot by multiple techniques. Several ToF‐SIMS and XPS acquisitions can be carried out with various parameters (investigation of backscattered Arn+ cluster ion fragments, tandem MS imaging...) as well as analysis with other techniques that possess limitations in spatial resolution and/or inaptitude to probe buried layers such as Raman or AFM. [ABSTRACT FROM AUTHOR]

Eleutherococcus senticosus (Rupr. & Maxim.) Maxim. fruits (ESF), as a natural edible fruit, has long been popularized. However, few studies have conducted comprehensive chemical analyses of it. This study aimed to assess nonvolatile, volatile, and fatty oil components of ESF and to preliminarily explore the antioxidant activities. The qualitative and quantitative analyses of volatile and fatty oil components of ESF from 15 different regions were performed by the gas chromatography–mass spectrometry (GC–MS). Totally, 37 and 28 compounds were identified from volatile oil and fatty oil, respectively. The ultra‐high‐performance liquid chromatography–quadrupole time‐of‐flight mass spectrometry (UPLC–QTOF–MS/MS) was used to accurately detect 43 compounds of nonvolatile components. The volatile and fatty oil components and nonvolatile components of ESF were used as samples to determine the antioxidant activity of 2,2‐diphenyl‐1‐picrylhydrazyl (DPPH) in vitro. The components of ESF had antioxidant activity, and the nonvolatile components had stronger antioxidant activity. The results revealed that the proposed method, which is of great significance for the screening of new active ingredients, is valuable for the identification of pharmaceutical component and further development of food industry. [ABSTRACT FROM AUTHOR]

Rationale: Ozenoxacin (OXC) is an antibiotic used topically to treat impetigo. This study aimed to evaluate the degradation products (DP) of OXC drug substance under different stress conditions, including hydrolysis, oxidation, thermal and photolysis, in accordance with the International Council for Harmonisation of Technical Requirements for Pharmaceuticals for Human Use (ICH) guidelines Q1A(R2) and Q1B. The analytical technique was validated in compliance with ICH Q2(R1) requirements. Methods: The drug substance underwent degradation under various forced degradation conditions, including thermal, oxidative, photolytic and hydrolytic (neutral, acidic and basic) degradation. Overall, four DPs were formed under oxidative stress conditions with AIBN. The formed DPs were identified and separated using a Shimadzu LC system with a reversed-phase Phenomenex Kinetex C18 column (4.6 = 250 mm, 5 µm), using 10 mM NH4CH3COOH buffer (pH 5.0) as mobile phase A and acetonitrile as mobile phase B at a detection wavelength of 254 nm. Results and Conclusion: The drug was found to be stable in neutral, acidic, basic and oxidative degradation conditions with hydrogen peroxide. Liquid chromatographyelectrospray ionisation-quadrupole time-of-flight-tandem mass spectrometry-was employed in positive ionisation mode to analyse both the drug and the mass of the identified DP. The mechanism and the pathway of mass fragmentation have been proposed. The developed method was accurate, repeatable, linear and selective for further research. The ADMET Predictor software was applied to predict the in silico toxicity of the drugs and its DPs as well as their physicochemical characteristics. [ABSTRACT FROM AUTHOR]

Phellodendri Amurensis Cortex (PAC) is a medicinal herb that has been generally used to treat diarrhea and jaundice. In order to comprehensively evaluate the PAC in the main production areas quality, a qualitative and quantitative method with highly effective, sensitive, and reliable was developed. The chemical compositions of PAC were analyzed, and fingerprints were established by ultra‐high‐performance liquid chromatography‐quadrupole time‐of‐flight tandem mass spectrometry (UPLC‐Q‐TOF‐MS). Then, the determination of berberine, canthin‐6‐one, dictamnine, γ‐fagarine, and magnoflorine from PAC samples was simultaneously performed using UPLC‐QQQ‐MS. Furthermore, the chemical components of PAC from different regions were compared and analyzed by combining hierarchical cluster analysis, principal component analysis, and orthogonal partial least squares discriminant analysis. A total of 58 compounds were identified, including 36 alkaloids, four phenylpropanoids, seven terpenoids, four flavonoids and their glycosides, an organic acid compound, and six other components. The fingerprint results show that samples have good similarity. Meanwhile, the content of the five ingredients in different habitats is quite different. By multivariate statistical analysis, 18 batches of PAC could be divided into three categories, and 20 components were identified as differential markers of various origins. A comprehensive method of PAC quality evaluation and chemical composition difference analysis was established, which provided the scientific basis for quality evaluation and further pharmacological mechanism research. [ABSTRACT FROM AUTHOR]