Mass Spectrometry Research Articles

Systematic Profiling and Quantitative Comparison of Chemical Components in Fagopyri Dibotryis Rhizoma From Different Habitats and Growing Periods Based on Ultra-High-Performance Liquid Chromatography With Mass Spectrometry.

Fagopyri Dibotryis Rhizoma, a traditional Chinese medicine, is widely used to treat various ailments such as pulmonary abscesses, measles pneumonia, and swelling. Its notable therapeutic effects are closely related to the chemical constituents, making it crucial to conduct in-depth research on the chemical components. In this study, a total of 209 compounds were preliminarily identified using ultra-high-performance liquid chromatography-quadrupole time-of-flight tandem mass spectrometry in Fagopyri Dibotryis Rhizoma. Subsequently, a method was established using ultra-high-performance liquid chromatography-triple quadrupole/linear ion trap tandem mass spectrometry for the simultaneous determination of 24 main ingredients (flavonoids and phenolic acids) in Fagopyri Dibotryis Rhizoma from different habitats and growing periods. Quantitative results showed that different compounds displayed varying contents across different habitats, with catechin, epicatechin, procyanidin B2, and procyanidin C1 being relatively abundant. Principal component analysis and partial least squares discriminant analysis showed there were significant differences among Fagopyri Dibotryis Rhizoma from different habitats, and the quality from Yunnan was superior. Entropy weight TOPSIS analysis showed that Fagopyri Dibotryis Rhizoma grown until late October has better comprehensive quality, which is basically consistent with the traditional harvesting time. In summary, this study can provide reference methods for the comprehensive evaluation of the quality of Fagopyri Dibotryis Rhizoma.

Deciphering the alteration of MAP2 interactome caused by a schizophrenia-associated phosphorylation

Microtubule-associated protein 2 (MAP2) is a crucial regulator of dendritic structure and neuronal function, orchestrating diverse protein interactions within the microtubule network. We have shown MAP2 is hyperphosphorylated at serine 1782 (S1782) in schizophrenia and phosphomimetic mutation of S1782 in mice (MAP2S1782E) is sufficient to impair dendritic architecture. We sought to determine how this hyperphosphorylation affects the MAP2 interactome to provide insights into the disorder's mechanisms. We investigated the MAP2 interactome using co-immunoprecipitation and mass spectrometry in MAP2S1782E and MAP2WT mice. We found that S1782E MAP2 led to a substantial disruption of protein-protein interactions relative to WT MAP2. Reduced interactions with PDZ domain-containing proteins, calmodulin-binding proteins, ribosome proteins, and kinesin proteins may all contribute to dendritic impairments induced by S1782E, and may be linked to schizophrenia pathogenesis. Interestingly, novel gain-of-function interactions with PPM1L and KLHL8 nominated these as regulators of phosphoS1782 MAP2 abundance and potential therapeutic targets in schizophrenia.

The crucial quality marker of Panax ginseng: Glycosylated modified ribonuclease-like storage protein

Panax ginseng C.A.Mey is a famous natural herbal medicine worldwide. Mountain-cultivated ginseng (MCG) and garden-cultivated ginseng (GCG) are two types of Panax ginseng. There is a significant difference in economic benefits between MCG and GCG, which can always lead to problems such as adulteration and substitution of MCG with lower-priced alternatives. We explored the quality marker of ginseng at the intact protein level and established a foundation for the quality control of ginseng. Cellulose nanocrystal assisted sample preparation combined with matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF MS) equipped with a high mass detector was performed to analyze intact proteins in ginseng. The results revealed that the ribonuclease-like storage protein is the most abundant protein in MCG and GCG. Meanwhile, the molecular weight of the ribonuclease-like storage protein showed great difference between different ginseng species, which is 26.2 kDa in MCG and 24.2 kDa in GCG. The ribonuclease-like storage protein glycosylation modification difference provides data support for the differentiation between MCG and GCG. This study showed that glycosylated modified ribonuclease-like storage protein can be a crucial quality marker of ginseng, facilitating the rapid distinction between MCG and GCG.

Identification of Marijuana Using Silver-Phosphine Ion Complexation and a Semi-Quantitative 1% Decision-Point Assay

Due to the strict federal regulations concerning ∆9-tetrahydrocannabinol (∆9-THC) content for the differentiation of hemp and marijuana outlined in the 2018 Farm Bill, the ability to quickly and reliably differentiate cannabis as marijuana or hemp is crucial within both the seized drug community and hemp industry. This study provides a novel direct mass spectrometry approach for the identification of marijuana using Ag-phosphine ion complexation and a semi-quantitative 1% decision-point assay. The main constituents of hemp and marijuana, cannabidiol (CBD) and ∆9-THC, are isomeric and cannot be differentiated using soft ionization mass spectrometry techniques alone. However, the incorporation of [Ag(PPh3)(OTf)]2 enables the formation of unique MS/MS product ions at m/z 421/423, m/z 353/355, and m/z 231 for CBD due to differences in binding affinity, allowing CBD to be differentiated from ∆9-THC. Likewise, the isomeric cannabinoid precursors ∆9-tetrahydrocannabinolic acid (∆9-THCA) and cannabidiolic acid (CBDA) can be differentiated due to the formation of unique MS/MS product ions at m/z 465/467 and m/z 379/381, which are specific to CBDA. Eight additional cannabinoids were also characterized utilizing the proposed Ag-phosphine ion complexation approach. To reduce the potential for false positives, a more conservative 1% decision-point assay was developed by fortifying 1% weight-by-volume ∆9-THC-d9 into methanolic extracts of authentic cannabis plant material, followed by assessing if the total ∆9-THC content (containing ∆9-THC and ∆9-THCA) was greater than or less than the intensity of the spiked internal standard. When the developed approach was applied to 20 methanolic extracts of authentic cannabis samples with known cannabinoid compositions, 90% of the samples were correctly identified as marijuana or not marijuana based on the 1% administrative threshold for the total ∆9-THC content. The two lone misidentifications were due to the presence of elevated ∆8-THC, which highlights the necessity to explore more selective ligands in the future. This study provides the first application of Ag-ligand ion complexation for the identification of marijuana based on a semi-quantitative 1% decision-point assay, which shows great promise as an alternative method for the rapid identification of marijuana.

Transcription factor PRRX1-activated ANXA6 facilitates EGFR-PKCα complex formation and enhances cisplatin sensitivity in bladder cancer

BackgroundTumor resistance to cisplatin represents a major clinical challenge, particularly in bladder cancer (BC). ANXA6 is a member of annexin family, and its role in cisplatin resistance remains unclear. This study explores ANXA6's role in promoting cisplatin sensitivity. MethodsBioinformatics analyses and clinical specimen verifications assessed the correlation between ANXA6 and cisplatin treatment. A series of assays, including CCK-8, clone formation assay, flow cytometry assays for reactive oxygen species (ROS) and apoptosis, and comet assays, were used to confirm ANXA6's role in enhancing cisplatin sensitivity and re-sensitizing resistant BC cells. Mass spectrometry, immunofluorescence, and co-immunoprecipitation experiments elucidated ANXA6's role in enhancing PKCα/EGFR complex formation and inhibiting the EGFR pathway. ChIP-PCR and dual-luciferase assays determined PRRX1's regulatory role on ANXA6 transcription. Finally, the impact of ANXA6 in vivo was evaluated using xenograft models. ResultsBioinformatics analyses showed a significant correlation between ANXA6 expression and cisplatin sensitivity. In vitro and in vivo experiments confirmed that ANXA6 was a new target for cisplatin treatment. ANXA6 overexpression not only enhanced cell viability inhibition, DNA damage and apoptosis caused by cisplatin, but also re-sensitized cisplatin-resistant cells. Mechanistically, ANXA6 promotes PKCα/EGFR complex formation, inhibiting EGFR phosphorylation and downstream AKT and ERK1/2. Moreover, PRRX1 was identified as a transcription factor promoting ANXA6 expression, thereby augmenting the cytotoxic effects of cisplatin. ConclusionOur study reveals the mechanism by which ANXA6 enhances cisplatin sensitivity and re-sensitizes resistant cells. The roles of PRRX1 and ANXA6 in cisplatin resistance offer new therapeutic targets to overcome cisplatin resistance in clinical practice.

Liquidambaric acid inhibits cholangiocarcinoma progression by disrupting the STAMBPL1/NRF2 positive feedback loop

BackgroundAbnormal antioxidant capacity in cancer cells is intimately linked to tumor aggressiveness. Modulating oxidative stress status and inhibiting ferroptosis represents a novel anticancer therapeutic strategy. STAM Binding Protein Like 1 (STAMBPL1), a deubiquitinase, is implicated in various malignancies, yet its function in inhibiting ferroptosis and therapeutic potential for cholangiocarcinoma (CCA) remains unexplored. Purpose: This study elucidates STAMBPL1's function in ferroptosis and evaluates liquidambaric acid (LDA) as its inhibitor for therapeutic applications. MethodsUsing bioinformatics, WB, IHC, the expression and prognostic value of STAMBPL1 in CCA tissue was detected. The carcinogenic capacity of STAMBPL1 and LDA were assessed through CCK-8, EdU, cloning, transwell, scratch, apoptosis, and cell cycle assays. Flow cytometry and fluorescence microscopy, as well as transmission electron microscopy (TEM), examines the effects of STAMBPL1 and LDA on intracellular reactive oxygen species (ROS) and changes in mitochondrial membrane potential. The tumorigenic ability of STAMBPL1 and LDA in vivo was evaluated through subcutaneous tumor model and lung metastasis model. The underlying mechanism of STAMBPL1 was explored using immunoprecipitation coupled with Mass spectrometry (IP/MS), Co-immunoprecipitation (Co-IP), GST pull-down, DNA pull-down, and Dual-luciferase reporter assays. Molecular docking simulations, SPR, DARTS and CETSA predict the putative binding site of LDA on STAMBPL1 protein. Rescue experiments further confirmed the above conclusions. ResultsThis study unveils the upregulation and oncogenic role of STAMBPL1 in CCA. Functionally, STAMBPL1 notably enhances CCA cell proliferation and metastasis while impeding ferroptosis. STAMBPL1 stabilizes NRF2, a pivotal regulator of antioxidant enzymes, through K63 deubiquitination. Elevated NRF2, stabilized by STAMBPL1 overexpression, triggers GPX4 activation and reactive oxygen species (ROS) elimination. Particularly, sites 251-436 of STAMBPL1 interact with sites 228-605 of NRF2, facilitating DUB activity and eliminating ubiquitin molecules attached to NRF2, thus protecting it from proteasome-mediated degradation. Moreover, NRF2, acting as a transcription factor, binds to the promoter region of STAMBPL1 and activates its transcription, thus forming STAMBPL1/NRF2 positive feedback loop and regulating redox homeostasis. Molecular docking and in vitro/in vivo experiments identified that LDA binds to and inhibits STAMBPL1, thereby disrupting the STAMBPL1/NRF2 positive feedback loop, consequently suppressing CCA progression. ConclusionThis study firstly reveals that STAMBPL1 promotes cholangiocarcinoma progression by upregulating NRF2, indicating that targeting the STAMBPL1/NRF2 axis is a novel therapeutic strategy. Additionally, our findings firstly suggest that LDA can bind to STAMBPL1, inhibiting NRF2 deubiquitination and offering significant therapeutic potential.

Snake venom weakens neurovascular integrity and promotes vulnerability to neuroinflammation

Snake envenomation poses significant medical challenges, particularly in subtropical and tropical regions, with long-term impacts on neurovascular integrity and neuroinflammation remaining underexplored. This study investigates the effects of venom from four species of venomous snakes in southern China—Zhoushan Cobra (Naja atra, NA), Many-banded Krait (Bungarus multicinctus, BM), Five-paced Pit Viper (Deinagkistrodon acutus, DA), and Chinese Moccasin (Protobothrops mucrosquamatus, PM) — on the blood–brain barrier (BBB) and chronic neuroinflammation. Using mass spectrometry, we analyzed venom protein compositions, while cytotoxic effects on mouse brain endothelial cells (bEND.3) were evaluated to determine IC50 values. In vitro BBB models and in vivo experiments in C57BL/6J mice revealed that NA venom, in particular, significantly compromised BBB integrity without inducing large-scale apoptosis, leading to persistent BBB disruption characterized by increased permeability and selective degradation of extracellular matrix and tight junction proteins. Moreover, to simulate secondary infections that often occur following snakebites, we combined venom exposure with lipopolysaccharide (LPS) treatment, which exacerbated neuroinflammatory responses by intensifying microglial activation and promoting a pro-inflammatory phenotype. These findings highlight the role of snake venom in compromising neurovascular integrity and promoting vulnerability to chronic neuroinflammation, emphasizing the need for further research into venom-induced neuroinflammatory pathways and their potential as therapeutic targets.

Single-step purification and characterization of Pseudomonas aeruginosa azurin.

Azurin is a small periplasmic blue copper protein found in bacterial strains such as Pseudomonas and Alcaligenes where it facilitates denitrification. Azurin is extensively studied for its ability to mediate electron-transfer processes, but it has also sparked interest of the pharmaceutical community as a potential antimicrobial or anticancer agent. Here we offer a novel approach for expression and single-step purification of azurin in Escherichia coli with high yields and optimal metalation. A fusion tag strategy using an N-terminal GST tag was employed to obtain pure protein without requiring any additional purification steps. After the on-column cleavage by HRV 3C Protease, azurin is collected and additionally incubated with copper sulphate to ensure sufficient metalation. UV-VIS absorption, mass spectroscopy, and circular dichroism analysis all validated the effective production of azurin, appropriate protein folding and the development of an active site with an associated cofactor. MD simulations verified that incorporation of the N-terminal GPLGS segment does not affect azurin structure. In addition, the biological activity of azurin was tested in HeLa cells.

Photoelectrocatalytic degradation of hyaluronic acid and regulation effects of its degradation products on gut microbiota in vitro.

Hyaluronic acid (HA) has multiple biological activities which are closely related to its molecular weight. In the present study, the photoelectrocatalytic method was established for HA degradation and the influences of bias potentials, H2O2 additions and reaction times on the degradation results were investigated to optimize the reaction condition. Moreover, a series of analysis methods, such as FT-IR and NMR were used to analyze chemical compositions of the degradation products, revealing that photoelectrocatalytic degradation did not damage the structural blocks of HA obviously. Then 11 oligosaccharides with polymerization degrees from 2 to 8 in the degradation products were identified by mass spectroscopy and their reducing ends were all GlcA or AraA. In addition, in the photoelectrocatalytic degradation of HA, ·OH were identified as the most influential among the produced free radicals, and it could be proposed that ·OH specifically targeted the anomeric carbon of GlcA, resulting in the disaggregation of polysaccharides chain. Furthermore, the results of in vitro fermentation with fecal microbiota demonstrated that HA and its degradation products regulated microbiota structure discriminately, indicating their possible different outcomes as nutritional supplements and agents.

Imaging and Non-imaging Analytical Techniques Used for Drug Nanosizing and their Patents: An Overview.

Nanosizing is widely recognized as an effective technique for improving the solubility, dissolution rate, onset of action, and bioavailability of poorly water-soluble drugs. To control the execution and behavior of the output product, more advanced and valuable analytical techniques are required. The primary intent of this review manuscript was to furnish the understanding of imaging and non-imaging techniques related to nanosizing analysis by focusing on related patents. In addition, the study also aimed to collect and illustrate the information on various classical (laser diffractometry, photon correlation spectroscopy, zeta potential, laser Doppler electrophoresis, X-ray diffractometry, differential scanning calorimeter, scanning electron microscopy, transmission electron microscopy), new, and advanced analytical techniques (improved dynamic light scattering method, Brunauer-Emmett- Teller method, ultrasonic attenuation, biosensor), as well as commercial techniques, like inductively coupled plasma mass spectroscopy, aerodynamic particle sizer, scanning mobility particle sizer, and matrix- assisted laser desorption/ionization mass spectroscopy, which all relate to nano-sized particles. The present manuscript has taken a fresh look at the various aspects of the analytical techniques utilized in the process of nanosizing, and has achieved this through the analysis of a wide range of peer-reviewed literature. All summarized literature studies provide the information that can meet the basic needs of nanotechnology. A variety of analytical techniques related to the nanosizing process have already been established and have great potential to weed out several issues. However, the current scenarios require more relevant, accurate, and advanced analytical techniques that can minimize the time and deviations associated with different instrumental and process parameters. To meet this requirement, some new and more advanced analytical techniques have recently been discovered, like ultrasonic attenuation technique, BET technique, biosensors, etc. Conclusion: The present overview certifies the significance of different analytical techniques utilized in the nanosizing process. The overview also provides information on various patents related to sophisticated analytical tools that can meet the needs of such an advanced field. The data show that the nanotechnology field will flourish in the coming future.

HPLC with parallel ESI-MS and ICP-AES detection as a tool for the speciation studies of phosphovanadotungstates

The presence of different equilibrated chemical species in aqueous solutions of polyoxometalates represents a challenge for their identification, requiring the use of both separation and detection techniques. The use of reversed-phase ion-pair high-performance liquid chromatography (HPLC) in gradient elution mode resulted in optimal separation conditions. The detection was accomplished by parallel hyphenation of the inductively coupled plasma atomic emission spectrometry (ICP-AES) and electrospray ionization mass spectrometry (ESI-MS), which combined the advantages of element and molecule specific detectors. This hyphenation resulted in an unambiguous identification of the products of the synthesis of mixed-addendum Keggin-type phosphovanadotungstates of [PVxW12-xO40](3+x)- (x = 1 – 3) general formula without the isolation of the individual species.

Impact of an extreme drought event on clonal reproduction and the acclimation capacity of the succulent plant Sempervivum tectorum L.

Functional traits have been defined as those that affect organismal performance, that is growth and development, reproduction and survival, so they have been generally associated with acclimation and adaptation. Here, we aimed to study the impact of an extreme drought event on clonal reproduction and hormonal mechanisms underlying acclimation of houseleek (Sempervivum tectorum L.), a plant adapted to survive harsh environments. We also explored the validity of growth- and stress-related phytohormones as functional traits to evaluate stress acclimation responses in the field. We compared the response of plants, considering both mother rosettes and newly produced clones, to a very extreme summer drought event occurring in small cliffs in Les Guilleries mountains (NE Spain). We measured various stress makers in the field together with hormonal profiling through a metabolomic approach using liquid chromatography coupled to tandem mass spectrometry. Results showed that clonal propagation was arrested during the study period and revealed a 100-fold increase in abscisic acid content from spring to summer both in mothers and new clones, concomitantly with reductions in relative water content, which decreased by 20% only. The stress-related bioactive jasmonate, jasmonoyl-isoleucine increased simultaneously with abscisic acid, while growth-related hormones, including bioactive cytokinins (2-isopentenyl adenine and trans-zeatin) decreased from spring to summer, which was consistent with growth arrest. It is concluded that S. tectorum adjusts recruitment of new clones during periods of low water availability and withstands extreme drought events during the summer (preventing severe cell turgor loss at soil water contents below 2% and temperatures above 43 ºC) by successfully activating a complex hormonal response that underlies the great capacity of this species to survive extreme climatic events.

Dissociation Chemistry of Protonated α-, β- and Other Amino Acids Using Multiple Stage Tandem Mass Spectrometry.

To discriminate amino acid isomers by multiple stage tandem mass spectrometry (MSn), the fragmentation of protonated amino acids were investigated by MSn with collision-induced dissociation (CID) and density functional theory calculations. The CID of protonated α-amino acids results in a loss of 46 Da, corresponding to H2O and CO, and iminium ions appear as resultant fragments. The CID of protonated β-amino acids also produces iminium ions, but the corresponding loss is 60 Da instead of 46 Da. H2O loss initiates the fragmentation of protonated β-amino acids, producing protonated β-lactams as an intermediate. Subsequently, protonated β-lactams are easily converted to iminium ions and CH2CO. By contrast, H2O loss from the protonated forms of γ- and ε-amino acids provides protonated lactams with 5- and 7-membered rings, respectively. Protonated lactams with more than 5-membered rings provide stable fragments and do not undergo further degradation during CID. In addition, protonated forms of γ- and ε-amino acids undergo NH3 loss as a competitive fragmentation pathway of H2O loss, producing protonated lactones. Because the fragmentation of protonated amino acid by CID depends on the position of amino and carboxyl groups, the tandem mass spectrometry with CID can discriminate α-, β-, and other amino acids.

Bioactive Constituents and the Molecular Mechanism of Melastoma dodecandrum Lour. in the Treatment of Inflammation Based on Network Pharmacology and Molecular Docking

Background: Melastoma dodecandrum Lour. (MD) is a component used in traditional Chinese medicine that is widely distributed in southern China. MD has long been used clinically to treat various diseases, such as inflammation. However, the potential anti-inflammatory mechanism of MD remains to be elucidated. Objective: In this study, network pharmacology and experimental validation have been used to explore the underlying mechanism of MD in inflammation. Methods: The chemical composition of MD was determined using ultra-high performance liquid chromatography-electrospray ionization-high resolution mass spectrometry (UHPLC-ESI-HRMS). The effects of MD on pro-inflammatory cytokines, such as NO, i-NOS, IL-1β, and TNF-α, in RAW264.7 cells stimulated by lipopolysaccharide (LPS) were determined by ELISA and QRT-PCR. Through the analysis of multiple databases, targets for the treatment of inflammation with MD were identified. Other extensive analyses included PPI, GO, and KEGG pathway enrichment, which were completed through the use of the STRING database, Cytoscape software, and the DAVID database. Key targets and key components have been selected for molecular docking. Results: A total of 33 active components were identified in MD, and 134 common targets were obtained and used to construct the networks. Of these, 10 core components and 10 core targets of MD in the treatment of inflammation were identified. The GO and KEGG enrichment analyses revealed that the common targets were involved in multiple signaling pathways, including the PI3K-Akt signaling pathway, NOD-like receptor signaling pathway, chemokine signaling pathway, and IL-17 signaling pathway. The molecular docking methods confirmed the high affinity between bioactive molecules of MD and their targets in inflammation. Two core targets (PIK3CA and AKT) and three core components (asiatic acid, apigenin, and kaempferol) were found to be closely related to MD in the treatment of inflammation. In vitro, MD exerted a significant effect on LPS-stimulated NO, IL- 1β, and TNF-α secretion, and iNOS, IL-1β, and TNF-α expressions in macrophages. Conclusion: This study has demonstrated the bioactive constituents and mechanisms of MD in inhibiting the secretion of inflammatory factors and the multicomponent, multitarget, and multipathway treatment characteristics involved in inflammation, but this still needs further in vivo/in vitro experiments.

Siling Decoction Ameliorates Adenine-Induced Renal Fibrosis in Rats by the AKT/IKKβ/NFκB Signaling Pathway

ObjectiveInvestigating how Siling decoction (SLD) mitigates fibrosis in rats with chronic kidney disease CKD (chronic kidney disease) through network pharmacology analysis and experimental verification. MethodsInitially, the primary active components and their target actions of SLD (Fuling, Zhuling, Zexie, and Baizhu) were identified by the TCMSP database and liquid chromatography mass spectrometry (LC-MS). Treatment targets for renal fibrosis were screened through databases such as GeneCard, OMIM, PharmGkb, and GEO. Subsequently, a drug-disease-target network was constructed and subjected to PPI analysis. Intersecting targets underwent GO and KEGG pathway enrichment analyses. Renal fibrosis model was induced by adenine gavage, then treat with SLD. Masson, Sirius red, immunohistochemistry, and Western blot were used to detect renal function and fibrosis-related indicators. The mechanism was further validated in vitro experiments. ResultsNetwork pharmacology analysis identified 100 common targets associated with the active components of SLD, including core genes such as AKT1 and CCND1. GO enrichment analysis revealed that the top three biological processes impacted include response to xenobiotic stimulus, response to nutrient levels and response to oxidative stress. These processes involved cellular components such as membrane raft, membrane microdomain and synaptic membrane, with molecular functions predominantly associated with ubiquitin-like protein ligase binding, ubiquitin protein ligase binding, DNA-binding transcription factor binding, and RNA polymerase II-specific DNA binding transcription factor binding. KEGG pathway enrichment analysis indicated potential involvement of pathways like Lipid and atherosclerosis, PI3K-AKT signaling pathway, and prostate cancer are likely involved in the anti-fibrotic effect of SLD. Notably, the highlighted was the AKT/IKKβ/NFκB signaling pathway as a key mechanism. These findings were further confirmed in vivo and in vitro. ConclusionThe SLD effectively ameliorates adenine-induced chronic kidney disease fibrosis in rats, potentially by inhibiting the AKT/IKKβ/NFκB signaling pathway.

Phytochemical Composition and Antioxidant Properties of Canarium odontophyllum (Sarawak Olive): A Seasonal Fruit from Borneo, East Malaysia.

BackgroundCanarium species are reported rich of polyphenol, alkaloids, flavones, and saponins compounds. Canarium odontophyllum from Borneo's variety, on the other hand is remaining unclear especially on the antioxidant activity towards radicals. PurposeTo investigate phytochemical composition and antioxidant properties of C. odontophyllum. MethodsAntioxidant properties were evaluated using 2,2-diphenyl-1-picrylhydrazyl-hydrate (DPPH) assay, 2,2′-azino-bis(3-ethylbenzthiazoline-6-sulphonic acid) (ABTS) assay, and ferric-reducing antioxidant power (FRAP) assay with different polarity of extraction solvents (methanol, acetone and hexane). The phytochemical composition was determined by Liquid Chromatography Mass Spectrometry Quadrupole Time of Flight (LCMS-QTOF). ResultsAcetone showed the highest scavenging activity in the DPPH (0.0307 mg/ml) and FRAP (3.926 mg/ml) assays, while hexane exhibited the highest activity in the ABTS assay (0.119 mg/ml). The LCMS-QTOF chromatogram identified 22 potential compounds. Among these, the major compounds oleamide (10.49%) and emmotin A (7.23%) have previously been reported to exhibit antioxidant activity. Other health-beneficial compounds were also found, such as palmitic amide (2.46%), deoxymiroestrol (6.23%), and N-Cyclohexanecarbonylpentadecylamine (48.92%), which are important in preventing metal corrosion, regulating hormones, and distinguishing between N-palmitoylethanolamine-hydrolyzing acid amidase (NPAA) and fatty acid amide hydrolase (FAAH), respectively. ConclusionThe results indicate that C. odontophyllum shows a promising potential an alternative drug in pharmaceutical developments.

A new sample preparation approach based on microwave-induced combustion in disposable vessels for Ni and V determination by ICP-MS in crude oil

The presence of Ni and V in crude oil is associated with pollutant emissions, corrosive processes and low-quality products. Nevertheless, the knowledge of the concentration of these elements, helps to predict geochemical characteristics and to bring information about the crude oil source. Moreover, Ni and V can cause problems during the crude oil refining process. Therefore, the development of alternative, low-cost and rapid approaches for Ni and V determination in crude oil is still welcomed and was the aim of this work. The proposed microwave-induced combustion in disposable vessels (MIC-DV) system allows the use cheap and/or reusable materials, combined to the possibility of sample combustion under atmospheric pressure and using a domestic microwave. The parameters evaluated during MIC-DV optimization were, sample mass (5 to 20 mg) and volume (1 to 10 mL) and concentration (0.5 to 7 mol L-1 HNO3) of absorbing solution. MIC-DV was applied for the digestion of ten crude oil and the results were compared with those obtained after microwave-assisted digestion (MAD) and Ni and V determination by inductively couple plasma mass spectrometry (ICP-MS). The agreement values achieved ranged from 92 to 103% for Ni and from 93 to 106% for V. The limits of quantification after MIC-DV/ICP-MS were 0.28 and 0.15 μg g-1 for Ni and V, respectively. The developed MIC-DV method, can be considered environmentally friendly since it uses low-cost materials and instrumentation, requires reduced handling (based on the single vessel principle), avoids the use of additional dilution steps and minimizes the digest contamination.

Fluorotelomer Alcohol (FTOH) Emission Rates from New and Old Rain Jackets to Air Determined by Iodide High-Resolution Chemical Ionization Mass Spectrometry

Per- and polyfluoroalkyl substances (PFAS), which include fluorotelomer alcohols (FTOHs), are synthetic chemicals used in consumer products because of their water-, stain-, and grease-repellent properties; thus, PFAS are commonly found in functional clothing such as rain jackets. To date, emissions of PFAS from products to indoor air have not been well characterized, although many PFAS-containing products are used and stored indoors. We used a test chamber connected to a high-resolution time-of-flight chemical ionization mass spectrometer equipped with iodide as a reagent ion (I-HR-ToF-CIMS) to measure emission rates for four FTOHs from 10 rain jackets and one backpack cover. The materials were categorized as old/used, new, or “PFAS-free”, and they were tested under two different scenarios, i.e., immediately out of package and after airing out. We observed real-time FTOH emissions from all materials. Under the out-of-package scenario, emissions of 6:2, 8:2 and 10:2 FTOH showed characteristics that indicate mass transfer is limited by internal diffusion, with a high initial peak followed by a lower steady-state emission rate. Peak emission rates correlated well with material-phase concentrations determined by an offline extractive gas chromatography-mass spectrometry (GC-MS) method. Our results further suggest that the old, used jackets had, on average, higher peak emission rates and higher material-phase concentrations than the new jackets, largely driven by 8:2 FTOH. “PFAS-free” materials had the overall lowest emission rates and material-phase concentrations. After airing out, emission rates were on average an order of magnitude lower than peak emission rates. Our findings emphasize the importance of considering consumer products like rain jackets as sources of indoor exposure to PFAS.

A facile approach for fabricating g-C3N4-based materials as metal-free photocatalysts

This study presents a novel, straightforward approach for synthesizing graphitic carbon nitrides (g-C3N4, g-CN) from melamine, requiring merely 30 minutes of thermal holding at temperatures ranging from 400 to 550 °C in an atmosphere comprising either nitrogen or air. Elemental analysis, X-ray powder diffraction (XRD), Fourier-transform infrared spectroscopy (FTIR), diffuse reflectance (UV-Vis DRS), photoluminescence (PL) spectroscopy and scanning electron microscopy (SEM) were employed to assess the quality of the as-prepared powders. Furthermore, theoretical calculations utilizing the Density Functional Theory (DFT) method were conducted to reinforce the experimental findings of the research. A further investigation of the thermal stability of the selected sample was conducted using a unique combination of thermogravimetry–coupled with differential scanning calorimetry, quadrupole mass spectrometry (TG-DSC-MS) and advanced temperature-programmed desorption (TPD) analyzes. The current study focuses on the effect of synthesis conditions (temperature and nitrogen/air environment) on the structure, morphology, and photocatalytic performance of g-C3N4 compounds synthesized using this approach. The g-C3N4-based materials were examined as potential photocatalysts using the acid orange 7 (AO7) photodegradation methodology. To enable comparison of the photodegradation experiments, two separate lamps with wavelengths of 360 nm (UV light) and 420 nm (VIS light) were utilized. The primary objective was to present a novel method for the synthesis of g-C3N4-based materials. This was achieved by demonstrating that organic composites generated at lower temperatures have the best photocatalytic capabilities. Furthermore, the approach to achieving high-quality photocatalysts was shown to be cost-effective, environmentally friendly, and scalable.

Parental arsenic exposure and tissue-specific DNA methylation in Bangladeshi infants with spina bifida.

An emerging hypothesis linking arsenic toxicity involves altered epigenetic mechanisms, such as DNA methylation. In this study, we examined the relationship between parents' arsenic exposure and DNA methylation in tissues obtained from 28 infants with spina bifida from Bangladesh. We analyzed arsenic in parents' toenails using inductively coupled plasma mass spectrometry (ICP-MS). DNA methylation was measured in infants' dural tissue, buccal swabs, and whole blood using the Illumina Infinium MethylationEPIC BeadChip. We performed epigenome-wide association analyses (EWAS) and tested differentially methylated regions (DMRs). In EWAS, DNA methylation at cg24039697 in dural tissue was positively associated (β = 0.59, p = 7.6 × 10-9) with father's toenail arsenic concentrations, adjusting for covariates. We did not identify any CpG sites related to father's arsenic exposure in the other tissues, or any CpG sites related to mother's arsenic exposure. Gene ontology analysis identified many biological pathways of interest, including the Wnt signaling pathways. We identified several DMRs across the tissues related to arsenic exposure that included probes mapping to genes that have previously been identified in studies of neural tube defects. This study emphasizes the potential impact of arsenic exposure in fathers, often understudied in epidemiological studies, on DNA methylation in a unique neurological tissue specific to spina bifida.