Gas Chromatography-Atmospheric Pressure Chemical Ionization (GC-APCI) Expands the Analytical Window for Detection of Large PAHs (≥24 Ringed-Carbons) in Pyroplastics and Other Environmental Matrices Open waste burning, large-scale fires, and maritime disasters produce partially burnt plastic called “pyroplastic”. Chemical markers would provide a complementary method to appearance and physical properties for identifying pyroplastics in environmental samples, particularly with respect to microplastics. Pyroplastic can contain significant quantities and unique distributions of parent polycyclic aromatic hydrocarbons (PAHs) with molecular weights up to 278 Da. Because of this enrichment, we considered whether large PAHs (≥24 ringed-carbons) could serve as chemical markers for pyroplastics. To address this, we developed a high-temperature method for gas chromatography atmospheric pressure chemical ionization (GC-APCI) coupled with tandem mass spectrometry (MS/MS) to target large PAHs with molecular weights ranging from 314–424 Da. Method development was performed using National Institute of Standards and Technology standard reference materials (SRMs) previously characterized for PAHs greater than 302 Da. A PAH class-specific MS/MS acquisition scheme combined with a simple, generic microextraction provided sensitive and specific detection without the need for sample fractionation or cleanup. Pyroplastics collected during the 2021 M/V X-Press Pearl ship fire and plastic spill were analyzed. A semiquantitative comparison showed that the pyroplastic samples contained over 2 orders of magnitude more of the 16 large PAHs (314–424 Da) than unburnt plastic pellets, reflecting previously observed trends for parent PAHs up to 278 Da. Qualitative comparison of samples and SRMs revealed multiple potential candidates (including 1,3,5-triphenylbenzene) suitable for further study as markers of pyroplastics in complex environmental samples. A suite of chemical markers for pyroplastics should prove helpful in monitoring efforts for air quality, waste management, microplastic pollution, and fires at the forest–urban interface.

Gas Chromatography-Atmospheric Pressure Chemical Ionization (GC-APCI) Expands the Analytical Window for Detection of Large PAHs (≥24 Ringed-Carbons) in Pyroplastics and Other Environmental Matrices #ACSOmega pubs.acs.org/doi/10.1021/...

Immunocapture-LC-MS/MS Method for Quantification of the Anti-Alzheimer’s Monoclonal Antibody Donanemab in Human and Mice Serum Monoclonal antibodies hold significant promise for the treatment of Alzheimer’s disease (AD), and donanemab is the latest therapeutic human IgG1 antibody approved for clinical use. The development and...

Immunocapture-LC-MS/MS Method for Quantification of the Anti-Alzheimer’s Monoclonal Antibody Donanemab in Human and Mice Serum #ACSOmega pubs.acs.org/doi/10.1021/...

Exploring Approaches for Accelerated Mass Spectrometric Detection of Fluorochemicals from Aqueous Solutions Using Indirect, Adsorbent-Facilitated Desorption Ionization There is a growing need for rapid, low-cost analytical tools to screen water supplies for persistent contaminants. Due to their ubiquitous presence in the environment and their detrimental effects on ...

Exploring Approaches for Accelerated Mass Spectrometric Detection of Fluorochemicals from Aqueous Solutions Using Indirect, Adsorbent-Facilitated Desorption Ionization #ACSOmega pubs.acs.org/doi/10.1021/...

Comprehensive Characterization of Oligolactide Architecture by Multidimensional Chromatography and Liquid Chromatography–Mass Spectrometry Oligolactides (OLA) are increasingly finding applications in drug delivery systems, implant coating, and tissue engineering. The most common synthetic route to OLA, ring-opening polymerization, produces polymer chains with complex architecture, including cyclic structures, chains with acid end groups, and initiator-bound oligomeric species. This inherent molecular heterogeneity presents significant challenges in analytical characterization. To address this complexity, it is essential to develop a robust separation method for comprehensive analysis. In this study, we developed a novel and robust high-performance liquid chromatography (HPLC) method using ethanol-modified chloroform as an eluent on a normal-phase column, which effectively separates the OLA chains. Additionally, the impact of different initiators on the molecular heterogeneity of OLA chains was investigated. To elucidate the separation mechanism, the HPLC method is hyphenated with size exclusion chromatography in a two-dimensional liquid chromatography setup. The results indicate that OLA chains are separated based on increasing degree of polymerization or increasing lactide incorporation. Furthermore, online coupling of HPLC with mass spectrometry provided deeper insight into the heterogeneity of the bulk. This study highlights the importance of correlative characterization techniques as a preferred approach for determining microstructural heterogeneity in low molar mass OLA samples.

Comprehensive Characterization of Oligolactide Architecture by Multidimensional Chromatography and Liquid Chromatography–Mass Spectrometry #ACSOmega pubs.acs.org/doi/10.1021/...

Changes in Components During Quality Formation and Evaluation of Honey-Processed Glycyrrhiza uralensis Fisch. from Different Geographical Origins by Sequential Electrospray Ionization Mass Spectrometry To explore the changes in quality formation during the honey-processing of Glycyrrhiza uralensis from six geographical origins, including Inner Mongolia, Xinjiang, Anhui, Gansu, Guangdong, and Jiangxi. In this study, raw G. uralensis was mixed with honey and smoldered, then heated and stir-fried, and finally cooled. The water-soluble components (WSCs) and methanol-soluble components (MSCs) in G. uralensis were simultaneously analyzed by sequential electrospray ionization mass spectrometry (SESI-MS) without the need for complex sample pretreatment. Fifteen WSCs (e.g., proline, arginine, serine, glabrol, monosaccharides, disaccharides, and trisaccharides) and twenty-eight MSCs (e.g., liquiritigenin, naringenin, glycyrrhizic acid, glycyrrhetinic acid, and formononetin) were identified within 2 min. Both principal component analysis and partial least-squares discrimination analysis showed that samples of honey-processed G. uralensis (HPGU) from six different geographical origins were effectively distinguished; liquiritin, daidzein, sinapic acid, and ferulic acid were identified as potential differential metabolites by variable importance for the projection; and the contents of saccharides, glabridin, formononetin, glabrol, and glycyrrhetinic acid were high in HPGU. Meanwhile, Inner Mongolia showed the highest contents of glycyrrhetinic acid and daidzein, suggesting these samples may possess superior quality based on these specific markers. SESI-MS could enhance our understanding of the changes in quality formation during the honey-processing of G. uralensis.

Changes in Components During Quality Formation and Evaluation of Honey-Processed Glycyrrhiza uralensis Fisch. from Different Geographical Origins by Sequential Electrospray Ionization Mass Spectrometry #ACSOmega pubs.acs.org/doi/10.1021/...

Predictive N-Glycan Signatures of Severe Traumatic Brain Injury in Biofluids Using LC–MS/MS Traumatic brain injury (TBI) poses a significant global health issue, frequently resulting in persistent and even lifelong cognitive and neurological impairments. Despite remarkable advances in biomarker discovery, significant challenges remain in the accurate diagnosis and prognosis of TBI. Glycosylation, an important post-translational modification of proteins and other biomolecules, plays an essential role in neuronal function and neuroinflammation. However, its contribution to the pathogenesis of TBI has been insufficiently investigated. This study examines changes in N-glycosylation patterns in serum and cerebrospinal fluid (CSF) from individuals with severe traumatic brain injury (sTBI) at various time points postinjury. Employing advanced glycomics methodologies and liquid chromatography–tandem mass spectrometry (LC–MS/MS), we identified 102 N-glycans in serum and 86 N-glycans in CSF, revealing substantial alterations in N-glycan expression, including differential expression of fucosylated and sialylated structures. Elevated fucosylation was observed in serum, whereas decreased fucosylation was found in CSF. Altered sialylation patterns were noted, suggesting glycosylation alterations in neuroinflammatory processes and possible neurodegeneration. Furthermore, our study examined N-glycans with isomeric properties. We identified several isomers that demonstrated potential as a biomarker panel reflective of TBI progression. Overall, these studies offer new insights into systemic and central nervous system-specific glycomic responses following sTBI and emphasize the potential of glycan-based biomarkers for monitoring specific changes as TBI progresses, which could be a possible target for enhanced TBI therapy and enhanced prognosis.

Predictive N-Glycan Signatures of Severe Traumatic Brain Injury in Biofluids Using LC–MS/MS #ACSOmega pubs.acs.org/doi/10.1021/...

Rapid Profiling, Fingerprinting, and Speciation of Poloxamer 188 in Biotherapeutic Drug Production Using Comprehensive Liquid Chromatography-Charge Reduction Mass Spectrometry Analysis #ACSOmega pubs.acs.org/doi/10.1021/...

Simultaneous, Online Membrane Inlet Mass Spectrometry (MIMS) and UV–Vis Absorbance for Kinetic Studies of the Formation of Disinfection Byproducts (DBPs) during Chlorination In this article, we demonstrate the major advantages of performing online kinetic studies of the formation of disinfection byproducts (DBPs) during chlorination using membrane inlet mass spectrometry (MIMS) supplemented with simultaneous UV–vis absorbance. MIMS is a well-known technique for online monitoring of small volatile organic compounds, but it cannot measure polar and/or nonvolatile organic compounds. This is problematic, since chemical DBP precursors, such as pesticides and pharmaceuticals, are generally not detectable by MIMS and must be analyzed offline using typical GC/MS or LC/MS. Supplementation of MIMS with simultaneous UV–vis absorbance makes it possible to monitor many of these non-MIMS detectable precursors. In addition, in many cases, UV–vis absorbance can be used to monitor the active chlorination agent, hypochlorite, during reactions. This is important for understanding mass balances in the chlorination process, since significant amounts of oxidant are lost to oxidation of reactive constituents in natural waters other than DBP precursors. Additionally, the UV absorbance spectra recorded simultaneously with MIMS monitoring can verify the identification of short-lived transient intermediates. This article will demonstrate the benefits of supplementing MIMS monitoring of DBP formation with simultaneous UV/vis absorbance for kinetic chlorination studies of the common water contaminants acetaminophen (a pain reliever), caffeine (a lifestyle compound), and difenoconazole (an herbicide). Concretely, UV/vis demonstrated that acetaminophen and its aromatic degradation product 1,4-benzoquinone were completely transformed into nonaromatic DBPs within 30 min, caffeine was only reduced by 30% after 24 h, and difenoconazole was unaffected after 24 h. In all three cases, the oxidant hypochlorite could be monitored during the reactions, and it was possible to separate the used hypochlorite into that used to oxidize the precursor itself and that used to oxidize oxidizable natural constituents present in the tap water. Finally, UV/vis supplemented the MIMS identification of the intermediate degradation product, 1,4-benzoquinone, from acetaminophen, and halophenols from phenol.

Simultaneous, Online Membrane Inlet Mass Spectrometry (MIMS) and UV–Vis Absorbance for Kinetic Studies of the Formation of Disinfection Byproducts (DBPs) during Chlorination #ACSOmega pubs.acs.org/doi/10.1021/...

QuEChERS Combined with Low-Temperature Partitioning and GC–MS as an Analytical Strategy for the Determination of Multiclass Pesticide Residues in Cocoa Beans The QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) technique has gained wide acceptance worldwide due to its efficiency in multiresidue pesticide analysis across diverse matrices. Continuous improvements have further enhanced its applicability and accuracy. In this study, QuEChERS was combined with low-temperature partitioning (LTP) for the simultaneous determination of 15 multiclass pesticide residues in cocoa beans by gas chromatography–mass spectrometry (GC–MS). A fractional factorial design (24–1) was employed to optimize extraction parameters. The optimal conditions comprised 2.0 g of sample, 8.0 mL of acetonitrile and 2.0 mL of water as the extraction solvent, 150 mg of PSA sorbent, vortex extraction for 3 min at 2500 rpm, and partitioning for 24 h in a conventional freezer. The method was validated, with limits of detection and quantification ranging from 4.16 to 6.95 μg kg–1 and 13.9 to 23.1 μg kg–1, respectively. Recoveries were within 70–120%. The procedure was applied to 15 cocoa samples from Bahia and Pará, Brazil, and permethrin was the only pesticide detected, occurring in five samples. These results demonstrate that the proposed approach is effective and reliable, highlighting low-temperature partitioning as a simplified cleanup strategy for complex matrices such as cocoa.

QuEChERS Combined with Low-Temperature Partitioning and GC–MS as an Analytical Strategy for the Determination of Multiclass Pesticide Residues in Cocoa Beans #ACSOmega pubs.acs.org/doi/10.1021/...

Unveiling Differences in Bioavailability, Metabolism, and Excretion of Neohesperidin in Lean and Obese Rats Based on Liquid Chromatography-Tandem Mass Spectrometry Neohesperidin, the most abundant compound found in the flowers of Citrus aurantium L. var. amara Engl., has shown a significant therapeutic effect on obesity caused by a high sugar diet. Nevertheless,...

Unveiling Differences in Bioavailability, Metabolism, and Excretion of Neohesperidin in Lean and Obese Rats Based on Liquid Chromatography-Tandem Mass Spectrometry #ACSOmega pubs.acs.org/doi/10.1021/...

Inline Analysis of the Plastics Melt Emissions in Real Time During Mechanical Recycling Using the SIFT-MS Method The quality of recycled plastics is significantly influenced by the contamination content of volatile organic compounds (VOCs), which enter the plastic through additives, migration or degradation processes. This poses a challenge for applications with high chemical requirements, such as food and cosmetics packaging or components in automotive interiors. In addition, previous analytical methods are based on random samples and only analyze a fraction of the material. Particularly with inhomogeneous input streams, there is a risk that potentially harmful substances will not be detected. For this reason, this study investigated the suitability of Selected Ion Flow Tube Mass Spectrometry (SIFT-MS) for the continuous inline analysis of VOCs during the extrusion process. By measuring the gas flow in real time at a vacuum dome of a twin-screw extruder, various VOCs from the input materials, including limonene and model substances in accordance with FDA requirements, were clearly identified and quantified. The measurement results showed a high correlation between the VOC content in the input material and the concentration in the gas flow. The results demonstrate the potential of SIFT-MS for process monitoring and quality control in mechanical plastics processing, especially for increasing safety and traceability when using recycled materials in sensitive applications.

Inline Analysis of the Plastics Melt Emissions in Real Time During Mechanical Recycling Using the SIFT-MS Method #ACSOmega pubs.acs.org/doi/10.1021/...

Development and Validation of a Cannabinoid Quantification Method in Oil and Marijuana by UHPLC-MS Cannabis sativa L. is an ancient species that has been cultivated over the years for various applications, including recreational and medicinal use. Nowadays, the demand for its products has grown significantly, leading to an increase in the search for medicinal oils and a rise in smuggling, making it the main trafficked drug. In this context, our work optimized the extraction process of six cannabinoids in Cannabis oil and marijuana samples, as well as an analytical validation of a quantitative and qualitative method for seven cannabinoids using ultra-performance liquid chromatography coupled with low-resolution mass spectrometry (UHPLC-LTQ-MS). The optimization showed that ethyl acetate is the most suitable solvent for oil extraction. For the marijuana sample, the extraction was performed using the same solvent and sonication and vortex agitation for 10 and 7.5 min, respectively. In the presented method, no matrix effect was observed, where LOQ ranged between 1 and 5 ng mL–1 and LOD between 0.3 and 1.5 ng mL–1. Recovery ranged from 84.6 to 107.6% in oil and from 80.6 to 105.9% in marijuana. Precision was evaluated in three ways: within a single day (RSD: 3.14–10.87% in oil, 3.25–10.14% in marijuana), across different days with a second analyst (RSD: 1.98–10.71% in oil, 4.65–12.81% in marijuana), and laboratories with a third analyst (RSD: 5.59–13.94% in oil, 4.65–13.56% in marijuana). The proposed method offers high sensitivity, selectivity, and precision, being adequate and satisfactory for the quantification of CBD, CBN, CBC, CBDA, Δ9-THC, and Δ9-THCA.

Development and Validation of a Cannabinoid Quantification Method in Oil and Marijuana by UHPLC-MS #ACSOmega pubs.acs.org/doi/10.1021/...

A Validated LC–MS/MS Method for the Determination of Sulindac and Its Metabolite Su-EP-C in Human Plasma and Their Pharmacokinetic Application in Healthy Volunteers A rapid, specific, and sensitive LC–MS/MS method for the determination of sulindac and its metabolite Su-EP-C in human EDTA-K2 plasma was developed. The method was fully validated using sulindac-d3 and Su-EP-C-d3 as internal standards. Separation was performed on a Kinetex C18 analytical column (100 Å, 50 × 2.1 mm, 5 μm). MPA consisted of 0.05% formic acid (FA) in water, while MPB comprised 0.05% FA in ACN. The flow rate was maintained at 0.300 mL/min, and the injection volume was 3 μL. Mass spectrometry conditions: ESI, positive mode, MRM. The linear range of detection was from 60.00 to 24,000.00 ng/mL for sulindac and from 30.00 to 12,000.00 ng/mL for Su-EP-C. The intra- and interbatch accuracy deviations of sulindac ranged from −5.1 to 5.0%, and the intra- and interbatch precision ranged from 3.3 to 4.2%. The intra- and interbatch accuracy of Su-EP-C ranged from −3.9 to 6.9%, and the intra- and interbatch precision ranged from 4.8 to 7.2% at all concentration levels. At a dilution of 10, the deviation for sulindac was 3.5% and the precision was 1.5%; the deviation for Su-EP-C was 2.7%, and the precision was 4.4%. The plasma matrix, at both −20 °C and −70 °C, remained stable for 52 days with 5 freeze–thaw cycles. The method was successfully applied to fasting and postprandial pharmacokinetic clinical trials of orally administered sulindac tablets.

A Validated LC–MS/MS Method for the Determination of Sulindac and Its Metabolite Su-EP-C in Human Plasma and Their Pharmacokinetic Application in Healthy Volunteers #ACSOmega pubs.acs.org/doi/10.1021/...

Spotlight on Endocannabinoids in Healthy Individuals Using Volumetric Absorptive Microsampling Combined with LC-MS/MS Analysis Endocannabinoids (eCBs) are crucial to regulating physiological function in the human body. This study investigates the applicability of volumetric absorptive microsampling (VAMS) for eCB analysis in blood samples. First, a liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed and validated to quantify a series of primary eCBs and eCB-like lipid mediators (i.e., AEA, OEA, SEA, PEA, LEA, 2-AG, and 2-OG). We then evaluated VAMS, considering several key parameters such as temperature, humidity, and hematocrit levels. This research systematically compared, for the first time, eCB levels in whole blood and plasma samples. We demonstrated an accuracy between 72.5% and 98.9%, with an interday and intraday precision below 8%, for all eCBs and eCB-like lipid mediators. The method exhibited minimal matrix effects, ranging from −15.0% to +9.0%. Most eCBs were stable under varying temperatures and storage conditions. However, drying time significantly affected the detected levels of 2-AG and 2-OG, suggesting that ex vivo biosynthesis may occur during drying. Interestingly, substantial differences in eCB levels were found between whole blood and plasma samples, emphasizing the importance of cellular components in eCB distribution. For example, 2-AG levels in whole blood ranged from 219–1,143 ng mL–1; plasma samples exhibited lower levels, ranging from 1.73–8.44 ng mL–1. These results highlight the need for standardized sampling methods to ensure accurate and consistent measurements of eCBs in both blood and plasma samples. While this work has significant implications for clinical eCB research, further investigation is necessary to understand the underlying mechanisms and clinical impact of eCB and eCB-like lipid mediators research.

Spotlight on Endocannabinoids in Healthy Individuals Using Volumetric Absorptive Microsampling Combined with LC-MS/MS Analysis #ACSOmega pubs.acs.org/doi/10.1021/...

Sample Preparation for MALDI-TOF Mass Spectrometry of Model Prebiotic Reactions in Simulated Ocean World Environments The prebiotic potential of ocean worlds such as Europa and Enceladus, while not well constrained, is vital in the search for potential life elsewhere. To better understand this potential, laboratory studies provide experimental insight into the chemical environment(s) of ocean worlds and any constraints to hold prebiotically relevant systems. However, simulated ocean world solutions present a technical challenge for analytical techniques such as mass spectrometry (MS), as the high saline content required for simulating ocean world environments results in ion suppression and reduced sensitivity. Here, we compare three sample preparation techniques, C4 ZipTips, C18 ZipTips, and on-plate washing, for matrix-assisted laser desorption/ionization – time-of-flight (MALDI-TOF) MS of saline solutions similar to environments expected in ocean worlds. We determined that using C18 ZipTips was optimal when paired with 2,5-dihydroxybenzoic acid (DHB) matrix, whereas on-plate desalting was optimal when paired with α-cyano-4-hydroxycinnamic acid (CHCA) matrix. The methodology described here presents simple, low-volume sample preparation strategies for MALDI-TOF MS of model prebiotic reactions in saline solutions.

Sample Preparation for MALDI-TOF Mass Spectrometry of Model Prebiotic Reactions in Simulated Ocean World Environments #ACSOmega pubs.acs.org/doi/10.1021/...

ForMileS: A Python Open-Source Program to Generate Molecular Structures for Tandem Mass Spectrometry Fragment Ions Tandem mass spectrometry is a central analytical tool in chemistry, yet the fragmentation mechanisms underlying collision-induced dissociation remain incompletely understood. A key challenge is predic...

ForMileS: A Python Open-Source Program to Generate Molecular Structures for Tandem Mass Spectrometry Fragment Ions #ACSOmega pubs.acs.org/doi/10.1021/...

A GC–MS-Based Urinary Metabolomic Profiling to Identify Potential Biomarkers of Metabolic Syndrome Metabolic syndrome (MetS) is a multifactorial condition characterized by central obesity, dyslipidemia, hypertension, and insulin resistance, increasing the risk of cardiovascular disease and type 2 diabetes. Despite its clinical significance, current diagnostic methods rely on invasive blood-based assessments. This study investigates the potential of urinary metabolomics as a noninvasive alternative for MetS diagnosis. Using gas chromatography–mass spectrometry (GC–MS), we analyzed urinary metabolites from 127 individuals classified into Normal, Borderline (BL), and MetS groups based on clinical diagnostic criteria. A total of 80 metabolites were identified, and partial least-squares discriminant analysis (PLS–DA) revealed distinct metabolic profiles between groups. Key metabolites, including glucuronate, galacturonic acid, and cystine, showed significant associations with MetS and its diagnostic components. Pathway analysis indicated metabolic perturbations primarily in carbohydrate, amino acids, and fatty acid metabolism. Furthermore, receiver operating characteristic (ROC) curve analysis demonstrated that a selected panel of urinary metabolites improved MetS classification accuracy. These findings suggest that urinary metabolomics profiling can provide novel biomarkers for MetS, offering a promising approach for noninvasive screening and early detection.

A GC–MS-Based Urinary Metabolomic Profiling to Identify Potential Biomarkers of Metabolic Syndrome #ACSOmega pubs.acs.org/doi/10.1021/...

Neurotoxicity-Based Toxicometabolomics of N-Ethyl Pentedrone Using Zebrafish as an In Vivo Model New psychoactive substances (NPS), particularly synthetic cathinones, have gained increasing attention due to their widespread recreational use and associated public health risks. Within this class, N...

Neurotoxicity-Based Toxicometabolomics of N-Ethyl Pentedrone Using Zebrafish as an In Vivo Model #ACSOmega #MassSpec pubs.acs.org/doi/10.1021/...

Affinity Selection-Mass Spectrometry for the Identification of Ligands of Acetylcholinesterase from Topsentia ophiraphidites and Docking Studies for the Dereplicated Ligands Acetylcholinesterase (AChE) inhibition has been successful for the treatment of Alzheimer’s disease and still stands as an important target in the search for novel ligands. In this context, affinity selection-mass spectrometry (AS-MS) has been acknowledged as a high-throughput screening (HTS) technique for large molecular libraries in drug discovery programs and natural product investigations. In this work, an AS-MS assay with AChE immobilized onto magnetic beads (AChE-MB) has been used to search for ligands in samples of the sponge Topsentia ophiraphidites collected in the archipelago of Fernando de Noronha, Brazil. Ligand dereplication disclosed 6-desmethyl-6-ethyl-9,10-dihydrospongosoritin A, 3,5-dibromo-O-methyltyrosine, 3-bromo-5-iodo-O-methyltyrosine, and 3,5-di-iodo-O-methyltyrosine as AChE ligands, which showed affinity ratios of 1.84, 1.34, 1.26, and 1.20, respectively, in the AS-MS assay. As a complementary approach, molecular docking analysis with human AChE has been carried out for the disclosed dereplicated ligands, in which the (R, R) stereoisomer of 6-desmethyl-6-ethyl-9,10-dihydrospongosoritin A stood out, performing important intermolecular interactions with the active sites of AChE, especially with the peripheral anionic site, at the entrance of the gorge. The results stimulate further investigations of these ligands in other pharmacological assays in order to better understand their mechanisms of action.

Affinity Selection-Mass Spectrometry for the Identification of Ligands of Acetylcholinesterase from Topsentia ophiraphidites and Docking Studies for the Dereplicated Ligands #ACSOmega pubs.acs.org/doi/10.1021/...

Thorough Chemical Characterization of Boerhavia elegans: GC-MS and LC-MS Analysis of Leaf and Root Extracts The phytochemical composition of Boerhavia elegans remains poorly understood, particularly in its leaves and roots, despite the plant’s traditional medicinal use. This study addresses this gap by conducting a comprehensive chemical characterization using gas chromatography–mass spectrometry (GC-MS) and liquid chromatography–mass spectrometry (LC-MS). Sequential Soxhlet extraction with hexane, ethyl acetate, and methanol yielded extracts ranging from 0.86 to 12.07%, with methanol providing the highest recoveries (12.07% in leaves, 10.01% in roots). GC-MS analysis of leaf hexane extracts identified 12 compounds (86% of total content), dominated by fatty acids (palmitic and oleic acids, 28.9%) and steroids (38.5%), particularly stigmast-5-en-3-ol (27.0%). Ethyl acetate fractions were enriched in sterols (42.5%), including stigmasterol and campesterin. LC-MS profiling of methanol extracts revealed bioactive molecules, including lutein, echinulin, pheophorbide a, and pectolinarigenin. The prevalence of sterols, fatty acids, flavonoids, and chlorophyll derivatives with antioxidant, antimicrobial, and anticancer activities underscores the pharmaceutical potential of Boerhavia elegans. These findings provide the first quantitative insight into the chemical diversity of Boerhavia elegans leaves and roots, establishing a foundation for its future use in medicinal and pharmaceutical applications.

Thorough Chemical Characterization of Boerhavia elegans: GC-MS and LC-MS Analysis of Leaf and Root Extracts #ACSOmega pubs.acs.org/doi/10.1021/...

Using Resonance-Enhanced Multiphoton Ionization Time-of-Flight Mass Spectrometry to Quantitatively Evaluate the Transfer Behavior of A Compound in An Oil-in-Water-in-Oil Emulsion during Preparation In the present study, an oil-in-water-in-oil (O1/W/O2) emulsion during preparation was measured in real time by resonance-enhanced multiphoton ionization time-of-flight mass spectrometry (REMPI-TOFMS)...

Using Resonance-Enhanced Multiphoton Ionization Time-of-Flight Mass Spectrometry to Quantitatively Evaluate the Transfer Behavior of A Compound in An Oil-in-Water-in-Oil Emulsion during Preparation #ACSOmega pubs.acs.org/doi/10.1021/...

Untargeted Headspace Fingerprinting and Targeted Characterization to Reveal High-Intensity Ultrasonication Effects on the Volatilome Evolution of Milk Suspensions This study aimed at elucidating the impact of high-intensity ultrasonication (HIU) on milk’s aromatic profile and the molecular interaction behaviors between aroma compounds and β-lactoglobulin (BLG) through nontargeted headspace-gas chromatography–ion mobility spectrometry (HS-GC-IMS) and headspace solid-phase microextraction gas chromatography/mass spectrometry (HS-SPME-GC/MS), as well as targeted multispectral characterization. GC-IMS effectively distinguished different milk dispersions with and without HIU pretreatments based on the volatile patterns, complemented by HS-SPME-GC/MS for precise classification based on its high sensitivity to detect aroma compounds, simultaneously revealing the significant effects on the evolution of volatile flavor compounds in milk suspensions after nonthermal HIU treatments. Principal component analysis (PCA) of GC-IMS data showed clear separation between all milk samples and controls with 20 min HIU. Additionally, the unbound fraction of hexanal in the headspace decreased by 12% following BLG addition. Conformational changes in BLG induced by HIU, showing more subtle structural transformation compared to thermal pretreatments, significantly altered the interaction processes between proteins and volatile flavors, thus explaining the fluctuation in the contents of headspace aldehyde-ketones following HIU pretreatments of milk suspensions. Molecular docking confirmed the binding between BLG and volatile ligands, highlighting the protein’s role in flavor retention and release. The combined volatilomic and protein-structure approaches emphasized specific effects of HIU on the aroma profiling of dairy products and molecular structure of their proteins under cold sterilization conditions, providing new insights into flavor optimization and preservation.

Untargeted Headspace Fingerprinting and Targeted Characterization to Reveal High-Intensity Ultrasonication Effects on the Volatilome Evolution of Milk Suspensions #ACSOmega #MassSpec pubs.acs.org/doi/10.1021/...

New #ICMABResearch published in #ACSOmega!

📌Anionic Boron-Cluster BODIPY Conjugates As Promising Photosensitizers for Targeted Antimicrobial Photodynamic Therapy

icmab.es/anionic-boro...

📜Read the paper here: pubs.acs.org/doi/10.1021/...

Multilayered Forensic Protocol Based on In-Depth Mass Spectrometry Techniques for the Investigation of Suspicious Drums of Oils with the 2019–2022 Brazilian Oil Spill Disaster In 2019, the northeast coast of Brazil experienced the country’s largest environmental disaster involving a mysterious oil spill. At the same time, two drums containing an oily substance were found as...

Multilayered Forensic Protocol Based on In-Depth Mass Spectrometry Techniques for the Investigation of Suspicious Drums of Oils with the 2019–2022 Brazilian Oil Spill Disaster #ACSOmega pubs.acs.org/doi/10.1021/...

Mapping Metabolomic Relationships of Hop Cultivars in an Ancestral Lineage Context Hops (Humulus lupulus) are one of the most valuable raw materials in the global brewing industry as they provide resins and essential oils highly relevant to beer production. Hop cultivars commonly us...

Mapping Metabolomic Relationships of Hop Cultivars in an Ancestral Lineage Context #ACSOmega #MassSpec pubs.acs.org/doi/10.1021/...

Check out this great article in the latest ACS Omega--'Fundamental Discoveries in Enzymology through Undergraduate Research'.
#ACS #ACSOmega #UWEC #BlueGold

https://pubs.acs.org/doi/10.1021/acsomega.5c07487

Pharmacokinetic Profiling and Tissue Distribution of Seven Key Saponins in Rats Following Oral Administration of Panacis Japonici Rhizoma Extracts The pharmacokinetics and distribution of natural compounds in living organisms are crucial to understanding their therapeutic potential and safety. In the study, ultraperformance liquid chromatography–mass spectrometry (UPLC-MS/MS) was employed to develop a method for the separation and analysis of seven saponins, namely, G-Rg1, G-Re, G-Rb1, G-Ro, PG-RT1, CS-IV, and CS-IVa, in plasma and tissue samples derived from Panacis Japonici Rhizoma (PJR). Additionally, the pharmacokinetic profiles and tissue distribution characteristics of these saponins in rats were systematically investigated. Following the oral administration of 2 g/kg of PJR extracts, UPLC-MS/MS was utilized to analyze the compounds’ presence in plasma and various tissues. Key findings indicate that G-Rb1 exhibited the highest Tmax, T1/2, Cmax, and AUC0–t values, reflecting its slow and extended presence in the bloodstream. Dual and triple peak phenomena were observed in the plasma concentration–time curves for certain saponins, suggesting complex absorption dynamics. All seven saponins were detected across multiple tissues within 1 h postadministration and remained detectable for up to 10 h, with the lung and brain showing the highest and lowest concentrations, respectively. These results highlight the compounds’ broad distribution and prolonged elimination, providing a foundational understanding that is beneficial for future clinical applications of PJR.

Pharmacokinetic Profiling and Tissue Distribution of Seven Key Saponins in Rats Following Oral Administration of Panacis Japonici Rhizoma Extracts #ACSOmega #MassSpec pubs.acs.org/doi/10.1021/...

Enrichment of Low-Abundance and Low-Molecular-Weight Proteins in Human Milk Using Mass Spectrometry-Based Proteomics Human milk is a uniquely complex biological fluid, rich in bioactive components such as proteins, antibodies, enzymes, and hormones that are critical for immunity, development, and disease prevention....

Enrichment of Low-Abundance and Low-Molecular-Weight Proteins in Human Milk Using Mass Spectrometry-Based Proteomics #ACSOmega pubs.acs.org/doi/10.1021/...

Analytical Development for Detecting Femtomole-Level Organophosphorus Compounds in Biogeochemical Samples by Ion Chromatography/High-Resolution Mass Spectrometry Phosphorus (P) is a crucial element for life, and its organic forms play a central role in modern biology. Therefore, the analysis of their presence in environmental samples is important for evaluatin...

Analytical Development for Detecting Femtomole-Level Organophosphorus Compounds in Biogeochemical Samples by Ion Chromatography/High-Resolution Mass Spectrometry #ACSOmega pubs.acs.org/doi/10.1021/...

Reactivity of Petrobactin and Its Sulfonated Derivatives with Iron and Their Determination by Isotopic Saturation Fast Size-Exclusion Chromatography–Inductively Coupled Plasma Mass Spectrometry (ICP-MS) Petrobactin is a bis-catechol siderophore, synthesized by Marinobacter nauticus (formerly Marinobacter hydrocarbonoclasticus), an important oil-degrading bacterium that proliferates in oil-polluted marine ecosystems. The complexes formed by petrobactin and its sulfonated derivatives with iron were, for the first time, chromatographically separated and identified by mass spectrometry. Conditions for the separation of the iron complexes using reversed-phase HPLC and size-exclusion LC were optimized. A method for quantifying petrobactin and its sulfonated derivatives has been developed. The analytical procedure is based on the saturation of the apo form of the siderophore with isotopically enriched iron, followed by its separation by ultraperformance size-exclusion chromatography with ICP-MS detection. The method is characterized by a detection limit of 0.03 ± 0.01 and 0.02 ± 0.01 μmol L–1, for petrobactin and sulfonated derivatives, respectively. Conditions of the formation of iron complexes were discussed in terms of iron source and pH. The complexation reaction was the fastest when iron was supplied as citrate or malate and when it occurred at pH 8. The monosulfonated derivative bound iron significantly faster than petrobactin itself, unlike the disulfonated derivative.

Reactivity of Petrobactin and Its Sulfonated Derivatives with Iron and Their Determination by Isotopic Saturation Fast Size-Exclusion Chromatography–Inductively Coupled Plasma Mass Spectrometry (ICP-MS) #ACSOmega pubs.acs.org/doi/10.1021/...