CpG preconditioning reduces accumulation of lysophosphatidylcholine in ischemic brain tissue after middle cerebral artery occlusion

Analytical and Bioanalytical Chemistry

Published On 2021/4

Ischemic stroke is one of the major causes of death and permanent disability in the world. However, the molecular mechanisms surrounding tissue damage are complex and further studies are needed to gain insights necessary for development of treatment. Prophylactic treatment by administration of cytosine-guanine (CpG) oligodeoxynucleotides has been shown to provide neuroprotection against anticipated ischemic injury. CpG binds to Toll-like receptor 9 (TLR9) causing initialization of an inflammatory response that limits visible ischemic damages upon subsequent stroke. Here, we use nanospray desorption electrospray ionization (nano-DESI) mass spectrometry imaging (MSI) to characterize molecular effects of CpG preconditioning prior to middle cerebral artery occlusion (MCAO) and reperfusion. By doping the nano-DESI solvent with appropriate internal standards, we can study and compare …

Journal

Analytical and Bioanalytical Chemistry

Published On

2021/4

Volume

413

Page

2735-2745

Authors

Julia Laskin

Julia Laskin

Purdue University

Position

Professor of Chemistry

H-Index(all)

77

H-Index(since 2020)

50

I-10 Index(all)

0

I-10 Index(since 2020)

0

Citation(all)

0

Citation(since 2020)

0

Cited By

0

Research Interests

mass spectrometry

gas-phase ion chemistry

ion soft-landing

biomolecular imaging

University Profile Page

Kyle Duncan

Kyle Duncan

Vancouver Island University

Position

Department of Chemistry Nanaimo BC Canada

H-Index(all)

13

H-Index(since 2020)

12

I-10 Index(all)

0

I-10 Index(since 2020)

0

Citation(all)

0

Citation(since 2020)

0

Cited By

0

Research Interests

mass spectrometry

bioanalytical chemistry

electrospray ionization

mass spectrometry imaging

University Profile Page

Leonidas Mavroudakis

Leonidas Mavroudakis

Uppsala Universitet

Position

Department of Chemistry - BMC

H-Index(all)

6

H-Index(since 2020)

6

I-10 Index(all)

0

I-10 Index(since 2020)

0

Citation(all)

0

Citation(since 2020)

0

Cited By

0

Research Interests

University Profile Page

Other Articles from authors

Julia Laskin

Julia Laskin

Purdue University

Angewandte Chemie International Edition

Reductive Doping Inhibits the Formation of Isomerization‐Derived Structural Defects in N‐doped Poly (benzodifurandione)(n‐PBDF)

Recently, solution‐processable n‐doped poly(benzodifurandione) (n‐PBDF) has been made through in‐situ oxidative polymerization and reductive doping, which exhibited exceptionally high electrical conductivities and optical transparency. The discovery of n‐PBDF is considered a breakthrough in the field of organic semiconductors. In the initial report, the possibility of structural defect formation in n‐PBDF was proposed, based on the observation of structural isomerization from (E)‐2H,2′H‐[3,3′‐bibenzofuranylidene]‐2,2′‐dione (isoxindigo) to chromeno[4,3‐c]chromene‐5,11‐dione (dibenzonaphthyrone) in the dimer model reactions. In this study, we present clear evidence that structural isomerization is inhibited during polymerization. We reveal that the dimer (BFD1) and the trimer (BFD2) can be reductively doped by several mechanisms, including hydride transfer, forming charge transfer complexes (CTC …

Julia Laskin

Julia Laskin

Purdue University

Editorial–Special Issue Honoring the Recipients of the 2022 Thomson Medal: Lidia Gall and Vicki Wysocki

I am delighted to introduce the Special Issue of the International Journal of Mass Spectrometry (IJMS) honoring Lidia Gall and Vicki Wysocki, the recipients of the 2022 Thomson Medal of the International Mass Spectrometry Foundation. Lidia Gall was recognized for her “outstanding contributions to the development of methods and instruments to study atoms and molecules and for inventing electrospray ionization (ESI).” Vicki Wysocki was recognized for the “development of instrumentation for surface induced dissociation and application of this capability to the structural characterization of proteins and protein complexes.”The breadth of research and influence exerted by these two exceptional scientists on the field of mass spectrometry becomes apparent through the diverse array of topics featured in this issue. These include gas phase ion chemistry, fundamentals of ionization, instrumentation and method …

Julia Laskin

Julia Laskin

Purdue University

Analytical Chemistry

Lipid Isobar and Isomer Imaging Using Nanospray Desorption Electrospray Ionization Combined with Triple Quadrupole Mass Spectrometry

Mass spectrometry imaging (MSI) is widely used for examining the spatial distributions of molecules in biological samples. Conventional MSI approaches, in which molecules extracted from the sample are distinguished based on their mass-to-charge ratio, cannot distinguish between isomeric species and some closely spaced isobars. To facilitate isobar separation, MSI is typically performed using high-resolution mass spectrometers. Nevertheless, the complexity of the mixture of biomolecules observed in each pixel of the image presents a challenge, even for modern mass spectrometers with the highest resolving power. Herein, we implement nanospray desorption electrospray ionization (nano-DESI) MSI on a triple quadrupole (QqQ) mass spectrometer for the spatial mapping of isobaric and isomeric species in biological tissues. We use multiple reaction monitoring acquisition mode (MRM) with unit mass …

Julia Laskin

Julia Laskin

Purdue University

Small

Enhancing Energy Storage Capacity of 3D Carbon Electrodes Using Soft Landing of Molecular Redox Mediators

The incorporation of redox‐active species into the electric double layer is a powerful strategy for enhancing the energy density of supercapacitors. Polyoxometalates (POM) are a class of stable, redox‐active species with multielectron activity, which is often used to tailor the properties of electrochemical interfaces. Traditional synthetic methods often result in interfaces containing a mixture of POM anions, unreactive counter ions, and neutral species. This leads to degradation in electrochemical performance due to aggregation and increased interfacial resistance. Another significant challenge is achieving the uniform and stable anchoring of POM anions on substrates to ensure the long‐term stability of the electrochemical interface. These challenges are addressed by developing a mass spectrometry‐based subambient deposition strategy for the selective deposition of POM anions onto engineered 3D porous carbon …

Julia Laskin

Julia Laskin

Purdue University

International Journal of Mass Spectrometry

A multichannel phase-locked waveform generator for a rotating electric field mass analyzer

We have developed a multichannel phase-locked sine waveform generator for a mass dispersive rotating electric field device, known as a rotating wall mass analyzer (RWMA). The waveform generator outputs eight sine waves phase shifted by 45°. The frequency of the waveforms is adjustable in the range of 0.1–100 kHz and the maximum amplitude is 100 Vp-p, which is greater than 20 Vp-p provided by commercial arbitrary waveform generators. Adjustment of either amplitude or frequency maintains phase alignment for all eight output channels to continually generate a uniform rotating electric field inside the RWMA. The RWMA is a high-throughput mass analyzer for preparative mass spectrometry that separates a multicomponent continuous ion beam in space and enables the deposition of ions of different m/z onto concentric ring shapes on surfaces. Here, we demonstrate that increasing the generator's …

Kyle Duncan

Kyle Duncan

Vancouver Island University

Mass spectrometry imaging methods for visualizing tumor heterogeneity

HighlightsCurrent strategies to map lipids, metabolites, and proteins in tumor tissues.Recent biological insights obtained from MSI of tumor samples.Challenges in applying MSI to study tumor biology.Profiling spatial distributions of lipids, metabolites, and proteins in tumors can reveal unique cellular microenvironments and provide molecular evidence for cancer cell dysfunction and proliferation. Mass spectrometry imaging (MSI) is a label-free technique that can be used to map biomolecules in tumors in situ. Here, we discuss current progress in applying MSI to uncover molecular heterogeneity in tumors. First, the analytical strategies to profile small molecules and proteins are outlined, and current methods for multimodal imaging to maximize biological information are highlighted. Second, we present and summarize biological insights obtained by MSI of tumor tissue. Finally, we discuss important considerations for …

Kyle Duncan

Kyle Duncan

Vancouver Island University

Advances in Prostaglandin

Advances in Prostaglandin

Prostaglandins (PG) are a group of physiologically active lipid compounds called eicosanoids having diverse hormone-like effects in animals. Prostaglandins have been found in almost every tissue in humans and other animals. They are derived enzymatically from the fatty acid arachidonic acid.Every prostaglandin contains 20 carbon atoms, including a 5-carbon ring. They are a subclass of eicosanoids and of the prostanoid class of fatty acid derivatives. In the present book, twelve typical literatures about prostaglandin published on international authoritative journals were selected to introduce the worldwide newest progress, which contains reviews or original researches on prostaglandin. We hope this book can demonstrate advances in prostaglandin as well as give references to the researchers, students and other related people.

Julia Laskin

Julia Laskin

Purdue University

International Journal of Mass Spectrometry

The IJMS Young Scientist Feature: a special article collection featuring perspectives and critical insights from early career mass spectrometrists around the globe

The IJMS Young Scientist Feature: A special article collection featuring perspectives and critical insights from early career mass spectrometrists around the globe - NASA/ADS Now on home page ads icon ads Enable full ADS view NASA/ADS The IJMS Young Scientist Feature: A special article collection featuring perspectives and critical insights from early career mass spectrometrists around the globe Laskin, Julia ; Ouyang, Zheng ; Fournier, Isabelle ; Blanksby, Stephen Abstract Publication: International Journal of Mass Spectrometry Pub Date: March 2024 DOI: 10.1016/j.ijms.2024.117198 Bibcode: 2024IJMSp.497k7198L full text sources Publisher | Graphics figure from paper Click to view more © The SAO/NASA Astrophysics Data System adshelp[at]cfa.harvard.edu The ADS is operated by the Smithsonian Astrophysical Observatory under NASA Cooperative Agreement NNX16AC86A NASA logo Smithsonian logo …

Julia Laskin

Julia Laskin

Purdue University

Cell Communication and Signaling

Regulation of β-cell death by ADP-ribosylhydrolase ARH3 via lipid signaling in insulitis

BackgroundLipids are regulators of insulitis and β-cell death in type 1 diabetes development, but the underlying mechanisms are poorly understood. Here, we investigated how the islet lipid composition and downstream signaling regulate β-cell death.MethodsWe performed lipidomics using three models of insulitis: human islets and EndoC-βH1 β cells treated with the pro-inflammatory cytokines interlukine-1β and interferon-γ, and islets from pre-diabetic non-obese mice. We also performed mass spectrometry and fluorescence imaging to determine the localization of lipids and enzyme in islets. RNAi, apoptotic assay, and qPCR were performed to determine the role of a specific factor in lipid-mediated cytokine signaling.ResultsAcross all three models, lipidomic analyses showed a consistent increase of lysophosphatidylcholine species and phosphatidylcholines with polyunsaturated fatty acids and a reduction of …

Leonidas Mavroudakis

Leonidas Mavroudakis

Uppsala Universitet

Gastroenterology

Tu1212 PROTECTIVE ROLES OF PGE2 SIGNALING PATHWAY IN POSTOPERATIVE INTESTINAL HEALING

marked induction in Gas7 mRNA~ 128%, p< 0.00001). To investigate the functional conse-quences of Gas7 loss, we expressed impact of reconstitution of Gas7 in cells which displayed a successful 386% induction of protein. From a proliferation perspective, we noted that proliferating cell nuclear antigen (PCNA) which was decreased 53% with Gas7OE. The activation of the upstream protein MAPK was suppressed by 78%, supporting the role of Gas7 in proliferation. As far as transducers of the proliferative signal, cyclin D1 protein and c-Myc mRNA were decreased 74 and 57% respectively. Since both transducers can be regulated by beta-catenin (a key early event in colon carcinogenesis), we assessed beta catenin levels and found Gas7 OE reduced it by a marked 52%. Upstream regulators of beta-catenin such as activated AKT (serine 473 phosphorylated) was suppressed by 57%. Looking at proximal events …

Julia Laskin

Julia Laskin

Purdue University

International Journal of Mass Spectrometry

Multiple selected ion monitoring mode for sensitive imaging of eicosanoids in tissues using nanospray desorption electrospray ionization (nano-DESI) mass spectrometry

Nanospray desorption electrospray ionization mass spectrometry imaging (nano-DESI MSI) enables sensitive label-free mapping of multiple classes of molecules in biological samples. Previously, we demonstrated that combining nano-DESI MSI with selected ion monitoring (SIM) increases the sensitivity of the technique in a narrow m/z range. In this study, we use a series of adjacent multiple SIM (mSIM) windows to acquire nano-DESI MSI data with high sensitivity over a broader m/z range. We demonstrate that this approach substantially improves the quality of imaging data obtained for low-abundance eicosanoids, important lipid mediators derived from eicosapolyenoic acid products of arachidonic acid oxidation. Despite their importance as mediators of inflammation, asthma, fever, pain, hypertension, and stroke, eicosanoids have not been extensively investigated using MSI. This is mainly attributed to their low …

Julia Laskin

Julia Laskin

Purdue University

Chemical Science

Multimodal high-resolution nano-DESI MSI and immunofluorescence imaging reveal molecular signatures of skeletal muscle fiber types

The skeletal muscle is a highly heterogeneous tissue comprised of different fiber types with varying contractile and metabolic properties. The complexity in the analysis of skeletal muscle fibers associated with their small size (30–50 μm) and mosaic-like distribution across the tissue tnecessitates the use of high-resolution imaging to differentiate between fiber types. Herein, we use a multimodal approach to characterize the chemical composition of skeletal fibers in a limb muscle, the gastrocnemius. Specifically, we combine high-resolution nanospray desorption electrospray ionization (nano-DESI) mass spectrometry imaging (MSI) with immunofluorescence (IF)-based fiber type identification. Computational image registration and segmentation approaches are used to integrate the information obtained with both techniques. Our results indicate that the transition between oxidative and glycolytic fibers is associated …

Julia Laskin

Julia Laskin

Purdue University

The Journal of Physical Chemistry A

Molecular and Structural Characterization of Isomeric Compounds in Atmospheric Organic Aerosol Using Ion Mobility-Mass Spectrometry

Secondary organic aerosol (SOA) formed through multiphase atmospheric chemistry makes up a large fraction of airborne particles. The chemical composition and molecular structures of SOA constituents vary between different emission sources and aging processes in the atmosphere, which complicates their identification. In this work, we employ drift tube ion mobility spectrometry with quadrupole time-of-flight mass spectrometry (IM-MS) detection for rapid gas-phase separation and multidimensional characterization of isomers in two biogenic SOAs produced from ozonolysis of isomeric monoterpenes, d-limonene (LSOA) and α-pinene (PSOA). SOA samples were ionized using electrospray ionization (ESI) and characterized using IM-MS in both positive and negative ionization modes. The IM-derived collision cross sections in nitrogen gas (DTCCSN2 ) for individual SOA components were obtained using multifield …

Julia Laskin

Julia Laskin

Purdue University

Ion soft landing: A unique tool for understanding electrochemical processes

Ion soft landing (SL) is a preparative mass spectrometry approach that enables deposition of mass- and charge-selected gaseous ions onto surfaces with controlled kinetic energy. The unique capabilities of SL provide an opportunity to populate electrode-electrolyte interfaces (EEIs) with well-defined intact electroactive ions of known composition, thereby facilitating the characterization of their intrinsic electrochemical properties. In this perspective, we describe the SL technique and discuss how it may be used to study the effect of the charge state, stoichiometry, and composition of large redox active molecules and clusters on their electron transfer kinetics. SL has enabled the characterization of redox-active species that cannot be purified and examined using conventional bulk-phase separation and deposition approaches. Furthermore, precise control over the deposition process provides an opportunity to prepare …

Julia Laskin

Julia Laskin

Purdue University

ACS nano

Controlled Formation of Fused Metal Chalcogenide Nanoclusters Using Soft Landing of Gaseous Fragment Ions

The complete ligation of nanoclusters significantly reduces their chemical reactivity, catalytic activity, and charge transfer properties. Therefore, in applications, nanoclusters are activated through partial ligand removal to take advantage of their full potential. However, the precise control of ligand removal in the condensed phase is challenging. In this study, we examine the reactivity of well-defined activated nanoclusters on surfaces prepared through controlled ligand removal in the gas phase. To accomplish this, we utilized a specially designed ion soft-landing instrument equipped with a collision cell to prepare mass-selected fragment ions, which were then deposited onto self-assembled monolayer (SAM) surfaces. Specifically, we generated fragment ions by selectively removing one or two ligands from a series of atomically precise ligated metal sulfide clusters, Co5MS8(L1)6+ (M = Co, Mn, Fe, or Ni, L1 = PEt3 …

Leonidas Mavroudakis

Leonidas Mavroudakis

Uppsala Universitet

Metabolites

Ischemic stroke causes disruptions in the carnitine shuttle system

Gaining a deep understanding of the molecular mechanisms underlying ischemic stroke is necessary to develop treatment alternatives. Ischemic stroke is known to cause a cellular energy imbalance when glucose supply is deprived, enhancing the role for energy production via β-oxidation where acylcarnitines are essential for the transportation of fatty acids into the mitochondria. Although traditional bulk analysis methods enable sensitive detection of acylcarnitines, they do not provide information on their abundances in various tissue regions. However, with quantitative mass spectrometry imaging the detected concentrations and spatial distributions of endogenous molecules can be readily obtained in an unbiased way. Here, we use pneumatically assisted nanospray desorption electrospray ionization mass spectrometry imaging (PA nano-DESI MSI) doped with internal standards to study the distributions of acylcarnitines in mouse brain affected by stroke. The internal standards enable quantitative imaging and annotation of endogenous acylcarnitines is achieved by studying fragmentation patterns. We report a significant accumulation of long-chain acylcarnitines due to ischemia in brain tissue of the middle cerebral artery occlusion (MCAO) stroke model. Further, we estimate activities of carnitine transporting enzymes and demonstrate disruptions in the carnitine shuttle system that affects the β-oxidation in the mitochondria. Our results show the importance for quantitative monitoring of metabolite distributions in distinct tissue regions to understand cell compensation mechanisms involved in handling damage caused by stroke.

Julia Laskin

Julia Laskin

Purdue University

Nanoscale Advances

Soft landing of polyatomic anions onto three-dimensional semiconductive and conductive substrates

Soft landing of well-characterized polyoxometalate anions, PW12O403− (WPOM) and PMo12O403− (MoPOM), was carried out to explore the distribution of anions in the semiconducting 10 and 6 μm-long vertically aligned TiO2 nanotubes as well as 300 μm-long conductive vertically aligned carbon nanotubes (VACNTs). The distribution of soft-landed anions on the surfaces and their penetration into the nanotubes were studied using energy dispersive X-ray spectroscopy (EDX) and scanning electron microscopy (SEM). We observe that soft landed anions generate microaggregates on the TiO2 nanotubes and only reside in the top 1.5 μm of the nanotube height. Meanwhile, soft landed anions are uniformly distributed on top of VACNTs and penetrate into the top 40 μm of the sample. We propose that both the aggregation and limited penetration of POM anions into TiO2 nanotubes is attributed to the lower …

Julia Laskin

Julia Laskin

Purdue University

Advanced Functional Materials

Thermally Activated Aromatic Ionic Dopants (TA‐AIDs) Enabling Stable Doping, Orthogonal Processing and Direct Patterning

Doping plays a critical role in organic electronics, and dopant design has been central in the development of functional and stable doping. In this study, there is departure from conventional molecular dopants and a new class of dopants are reported – aromatic ionic dopants (AIDs). AIDs consist of a pair of aromatic cation and anion that are responsible for molecular doping reaction and charge balancing separately. It is shown that the first AID made from cycloheptatrienyl (tropylium) cation and pentacyanocyclopentadienide anion (PCCp), abbreviated as T‐PCCp, can function as an effective p‐type dopant to dope polydioxythiophenes. Here, tropylium cation induces the doping reaction while the PCCp anion stabilizes the generated polarons and bipolarons. With T‐PCCp, a highly doped (≈120 S/cm) and stable system is achieved up to 150 °C, an orthogonal (sequential)solution processing resulting from the …

Julia Laskin

Julia Laskin

Purdue University

High-throughput mass spectrometry imaging of biological systems: Current approaches and future directions

In the past two decades, the power of mass spectrometry imaging (MSI) for the label free spatial mapping of molecules in biological systems has been substantially enhanced by the development of approaches for imaging with high spatial resolution. With the increase in the spatial resolution, the experimental throughput has become a limiting factor for imaging of large samples with high spatial resolution and 3D imaging of tissues. Several experimental and computational approaches have been recently developed to enhance the throughput of MSI. In this critical review, we provide a succinct summary of the current approaches used to improve the throughput of MSI experiments. These approaches are focused on speeding up sampling, reducing the mass spectrometer acquisition time, and reducing the number of sampling locations. We discuss the rate-determining steps for different MSI methods and future …

Julia Laskin

Julia Laskin

Purdue University

Molecular & Cellular Proteomics

Proteome Mapping of the Human Pancreatic Islet Microenvironment Reveals Endocrine–Exocrine Signaling Sphere of Influence

The need for a clinically accessible method with the ability to match protein activity within heterogeneous tissues is currently unmet by existing technologies. Our proteomics sample preparation platform, named microPOTS (Microdroplet Processing in One pot for Trace Samples), can be used to measure relative protein abundance in micron-scale samples alongside the spatial location of each measurement, thereby tying biologically interesting proteins and pathways to distinct regions. However, given the smaller pixel/voxel number and amount of tissue measured, standard mass spectrometric analysis pipelines have proven inadequate. Here we describe how existing computational approaches can be adapted to focus on the specific biological questions asked in spatial proteomics experiments. We apply this approach to present an unbiased characterization of the human islet microenvironment comprising the …

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Leveraging the third dimension in microfluidic devices using 3D printing: no longer just scratching the surface

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Multiplexed lateral flow assays (LFAs) offer efficient on-site testing by simultaneously detecting multiple biomarkers from a single sample, reducing costs. In cancer diagnostics, where biomarkers can lack specificity, multiparameter detection provides more information at the point-of-care. Our research focuses on epithelial ovarian cancer (EOC), where STn-glycosylated forms of CA125 and CA15-3 antigens can better discriminate cancer from benign conditions. We have developed a dual-label LFA that detects both CA125-STn and CA15-3-STn within a single anti-STn antibody test line. This utilizes spectral separation of green (540 nm) and blue (450 nm) emitting erbium (NaYF4:Yb3+, Er3+)- and thulium (NaYF4: Yb3+, Tm3+)-doped upconverting nanoparticle (UCNP) reporters conjugated with antibodies against the protein epitopes in CA125 or CA15-3. This technology allows the simultaneous detection of …

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Analytical and Bioanalytical Chemistry

Comparison of LC-MS-based methods for the determination of carboxylic acids in animal matrices

Carboxylic acids (CAs) are key players in human and animal metabolism. As they are hardly retained under reversed-phase liquid chromatography (RP-LC) conditions in their native form, derivatization is an option to make them accessible to RP-LC and simultaneously increase their response for mass spectrometric detection. In this work, two RP-LC tandem mass spectrometry-based methods using aniline or 3-nitrophenylhydrazine (3-NPH) as derivatization agents were compared with respect to several factors including completeness of derivatization, apparent recoveries (R A s) in both cow feces and ruminal fluid, and concentrations obtained in feces and ruminal fluid of cows. Anion exchange chromatography coupled to high-resolution mass spectrometry (AIC-HR-MS) served as reference method. Derivatization efficiencies were close to 100% for 3-NPH derivatization but variable (20–100%) and different in …

Rebeca da Rocha Rodrigues

Rebeca da Rocha Rodrigues

Universidade Federal de São Paulo

Analytical and Bioanalytical Chemistry

Artificial neural networks in the modeling of the catalytic activity of a biosensor composed of conjugated polymers and urease

Thin films of conjugated polymer and enzyme can be used to unravel the interaction between components in a biosensor. Using artificial neural networks (ANNs) improves data interpretability and helps construct models with great capacity for classifying and processing information. The present work used kinetic data from the catalytic activity of urease immobilized in different conjugated polymers to create ANN models using time, substrate concentration, and absorbance as input variables since the models had absorbance in a posterior instant as output value to explore the predictivity of the ANNs. The performance of the models was evaluated by Pearson’s correlation coefficient (ρ) and mean squared error (MSE) values. After the learning process, a series of new experiments were performed to verify the generality of the models. As the main results, the best ANN model presented 0.9980 and 3.0736 × 10–5 for ρ …

Matteo D. Gallidabino

Matteo D. Gallidabino

Northumbria University

Analytical and Bioanalytical Chemistry

Correction to: Forensic profiling of smokeless powders (SLPs) by gas chromatography–mass spectrometry (GC‑MS): a systematic investigation into injector conditions and their …

Correction to: Forensic profiling of smokeless powders (SLPs) by gas chromatography–mass spectrometry (GC‑MS): a systematic investigation into injector conditions and their effect on the characterisation of samples - PMC Back to Top Skip to main content NIH NLM Logo Access keys NCBI Homepage MyNCBI Homepage Main Content Main Navigation Preview improvements coming to the PMC website in October 2024. Learn More or Try it out now. Search PMC Full-Text Archive Search in PMC Advanced Search User Guide Journal List Springer PMC10973009 Other Formats PDF (441K) Actions Cite Collections Share Permalink Copy RESOURCES Similar articles Cited by other articles Links to NCBI Databases Journal List Springer PMC10973009 As a library, NLM provides access to scientific literature. Inclusion in an NLM database does not imply endorsement of, or agreement with, the contents by NLM or the …

Arjen Lommen

Arjen Lommen

Wageningen Universiteit

Analytical and Bioanalytical Chemistry

Assessment of exposure to pesticides: residues in 24 h duplicate diets versus their metabolites in 24 h urine using suspect screening and target analysis

Human biomonitoring can add value to chemical risk assessment by reducing the assumptions regarding consumption rates, residue occurrence, and processing effects and by integrating exposures from different sources (diet, household use, environmental). However, the relationship between exposure and concentration in human matrices is unknown for most pesticides. Therefore, we conducted a pilot study to gain more insight into the qualitative and quantitative relationship between dietary intake of pesticides (external exposure) and urinary excretion (reflecting internal exposure). In this cross-sectional observational study, 35 healthy consumers aged 18–65 years from the region of Wageningen, Netherlands, collected an exact duplicate portion of their diets during 24 h. On the same day, they also collected all their urine. The duplicate diets were analyzed using target screening by GC- and LC-HRMS; each …

Ana Rivas

Ana Rivas

Universidad de Granada

Analytical and Bioanalytical Chemistry

New analytical method for the determination of endocrine disruptors in human faeces using gas chromatography coupled to tandem mass spectrometry

Endocrine-disrupting chemicals are environmental pollutants that can enter our bodies and cause diverse pathologies. Some bisphenols and parabens have been shown to be capable of modifying proper functioning of the endocrine system. Among other dysfunctions, endocrine-disrupting chemicals can cause changes in intestinal microbiota. Faeces are a convenient matrix that can be useful for identifying the quantity of endocrine disruptors that reach the intestine and the extent to which the organism is exposed to these pollutants. The present work developed a new analytical method to determine 17 compounds belonging to the paraben and bisphenol families found in human faeces. The extraction method was optimized using an ultrasound-assisted extraction technique followed by a clean-up step based on the QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) technique. Optimization was …

Natalia Ivleva

Natalia Ivleva

Technische Universität München

Analytical and Bioanalytical Chemistry

Towards a reference material for microplastics’ number concentration—case study of PET in water using Raman microspectroscopy

Increasing demand for size-resolved identification and quantification of microplastic particles in drinking water and environmental samples requires the adequate validation of methods and techniques that can be used for this purpose. In turn, the feasibility of such validation depends on the existence of suitable certified reference materials (CRM). A new candidate reference material (RM), consisting of polyethylene terephthalate (PET) particles and a water matrix, has been developed. Here, we examine its suitability with respect to a homogeneous and stable microplastic particle number concentration across its individual units. A measurement series employing tailor-made software for automated counting and analysis of particles (TUM-ParticleTyper 2) coupled with Raman microspectroscopy showed evidence of the candidate RM homogeneity with a relative standard deviation of 12% of PET particle counts …

Muhammad Awais

Muhammad Awais

National University of Computer and Emerging Sciences

Analytical and Bioanalytical Chemistry

Analysis and experimental assessment of an optimized SERS substrate used to detect thiabendazole in apples with high sensitivity

Pesticides that linger in the environment and ecosystems for an extended period can cause severe and dangerous health problems in humans. To detect pesticides in foods, the development of high-sensitivity and quick screening technologies was required. This research investigated the performance of Au@Ag NPs with varying thicknesses of the silver shell for detecting trace quantities of thiabendazole (TBZ) in apples using surface-enhanced Raman spectroscopy (SERS). The Au@Ag NPs were synthesized by coating 32 nm gold seeds with different thicknesses of silver shell ranging from 2.4 to 8.7 nm, achieved by adjusting the incorporation of AgNO3 and ascorbic acid. The optimized Au@Ag NPs with a 7.3 nm silver shell demonstrated outstanding SERS activity, high sensitivity, and a detection limit of 0.05 μg/mL for TBZ. The R2 values, representing the goodness of fit, were found to be 0.990 and 0.986 for …

Jorg Thöming

Jorg Thöming

Universität Bremen

Analytical and Bioanalytical Chemistry

Rapid online analysis of n-alkanes in gaseous streams via APCI mass spectrometry

Online monitoring of dynamic chemical processes involving a wide volatility range of hydrocarbon species is challenging due to long chromatographic measurement times. Mass spectrometry (MS) overcomes chromatographic delays. However, the analysis of n-alkane mixtures by MS is difficult because many fragment ions are formed, which leads to overlapping signals of the homologous series. Atmospheric pressure chemical ionization (APCI) is suitable for the analysis of saturated hydrocarbons and is the subject of current research. Still, although APCI is a “soft ionization” technique, fragmentation is typically inevitable. Moreover, it is usually applied for liquid samples, while an application for online gas-phase monitoring is widely unexplored. Here, we present an automated APCI-MS method for an online gas-phase analysis of volatile and semi-volatile n-alkanes. Mass spectra for n-heptane and n-decane reveal …

Hans J.C.T. Wessels

Hans J.C.T. Wessels

Radboud Universiteit

Analytical and bioanalytical chemistry

Mixed-phase weak anion-exchange/reversed-phase LC–MS/MS for analysis of nucleotide sugars in human fibroblasts

Nucleotide sugars (NS) fulfil important roles in all living organisms and in humans, related defects result in severe clinical syndromes. NS can be seen as the “activated” sugars used for biosynthesis of a wide range of glycoconjugates and serve as substrates themselves for the synthesis of other nucleotide sugars. NS analysis is complicated by the presence of multiple stereoisomers without diagnostic transition ions, therefore requiring separation by liquid chromatography. In this paper, we explored weak anion-exchange/reversed-phase chromatography on a hybrid column for the separation of 17 nucleotide sugars that can occur in humans. A robust and reproducible method was established with intra- and inter-day coefficients of variation below 10% and a linear range spanning three orders of magnitude. Application to patient fibroblasts with genetic defects in mannose-1-phosphate guanylyltransferase beta, CDP …