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At least 19 recordsLinked to original sources
PubMed1989

Coronaspray nebulization and ionization of liquid samples for ion mobility spectrometry.

Ion mobility spectrometry after electrospray nebulization and ionization was investigated as a method for the detection of components dissolved in liquids. While electrosprary operating conditions proved promising, greater sensitivity was achieved when the electric potential applied to the sample introduction needle was increased above breakdown potential and a corona discharge was established. Passing the liquid through the corona discharge established a "coronaspray" that efficiently nebulized and ionized the solvent and analytes. In this initial investigation of coronaspray ion mobility spectrometry (CIMS), ion current as a function of potential, temperature, and liquid flow rate was studied; several IMS spectra were obtained; and a continuous monitoring mode of operation was demonstrated. The results from this study indicated that CIMS has potential as a versatile and sensitive detection method for a variety of analytical procedures involving liquid flowing streams such as flow injection analysis, liquid chromatography, capillary zone electrophoresis, and field flow fractionation.

Electrochemistry↗
PubMed1990

Screening of solid commercial pharmaceuticals using ion mobility spectrometry.

Ion mobility spectrometry (IMS) was used to analyze vapors generated directly above pharmaceutical solids warmed in air to 100-200 degrees C. Vapors were characterized by IMS/mass spectrometry to evaluate the air-based atmospheric pressure chemical ionization of components in analgesic medicines. A hand-held IMS was used to determine the suitability of membrane-based instrumentation for routine analyses of large polar molecules. Mobility spectra for seven compounds could be individually represented by single or a few intense product ion peaks. Ion source fragmentations were nonexistent with these pharmaceuticals but complex behavior in the IMS involving ion-molecule clustering was pronounced in certain spectra. Mobility spectra were distinct and recognizable for each compound and binary mixtures of individual ingredients and actual over-the-counter medicines produced mobility spectra suggestive of composite spectra. This work represents a first delineation of complex ion mobility spectra for mixtures using spectra from individual components. These findings support further development of IMS for use in quality control during manufacture of such preparations and in routine screening of powders containing analgesic pharmaceuticals.

Acetaminophen↗
PubMed1989

Characterization of benzodiazepine drugs by ion mobility spectrometry.

Chemical ionization ion mobility spectrometry (CI-IMS) was used to characterize a number of benzodiazepines. In almost every example studied, the positive ion mobility spectrum consisted of a single ion peak corresponding to [M]+ or [MH]+. With some compounds, e.g., oxazepam, lorazepam, and chlordiazepoxide, fragment ions were noted that serve as good markers for the identification of these chemicals. Reduced mobility constants (K0) for the most significant peaks were calculated, and all ions produced were mass-analyzed by injection into a quadrupole mass spectrometer. The results of this study point to the potential of IMS as a qualitative tool for the rapid detection (analysis time less than 10 s) and reliable identification of benzodiazepines. Preliminary results on the application of digital signal processing and a second-derivative algorithm to partially overlapping IMS peaks are presented, and potential improvements are discussed.

Anti-Anxiety Agents↗
PubMed1989

Ion mobility spectrometry of halothane, enflurane, and isoflurane anesthetics in air and respired gases.

Three common gaseous anesthetics, halothane, enflurane, and isoflurane, were characterized by using ion mobility spectrometry (IMS)/mass spectrometry, and the dependence of product ion distributions on temperature and concentration was evaluated. At 40 degrees C and 500 ppb, negative ion mobility spectra in air largely consisted of monomer or dimer adducts with Br- or Cl- formed through dissociative electron capture of molecular neutrals. With increased temperature or decreased vapor concentrations, declustering and dissociation of product ions became pronounced. Ion-molecule reactions in the drift region of the IMS were evident as distortions in peak shape in the mass-resolved mobility spectra and in variable reduced mobilities for the same ions. A portable hand-held IMS was used for convenient, real-time detection of enflurane in respired gases following a controlled inhalation episode.

Air↗
PubMed1989

Preliminary investigation of ion mobility spectrometry after capillary electrophoretic introduction.

Using standard capillary electrophoretic and ion mobility methods, several electrospray interface designs were investigated for the capillary electrophoretic introduction of samples into the ion mobility spectrometer. Of the interfaces investigated, the flow assisted interface and the direct coupled interface showed the most promise. These preliminary experiments were encouraging. The ion mobility spectrometer coupled with a capillary electrophoretic introduction system operated with excellent separation efficiency and ion mobility reproducibility. Using tetrabutylammonium iodide, the number of theoretical plates for the spectrometer was calculated to be 3.10(3) and reduced mobilities were found to be reproducible with a relative standard deviation of 1.43%. Because of the desire to hold the spectrometer as hot as possible, the solvent would often vaporize in the interface, creating an unstable spray and inhomogeneities in the electrophoretic field. More work is needed to improve the spray process which contributed to the overall noise of the system and to eliminate the phenomenon of solvent vaporization which limited the reproducibility of electrophoretic migration times.

Electrophoresis↗
PubMed1992

Ion mobility spectrometry of drugs of abuse in customs scenarios: concentration and temperature study.

A custom-built ion mobility spectrometer has been used to obtain the IMS spectra of cocaine, heroin, amphetamine sulfate and LSD at different drug concentrations and desorption temperatures. Practical detection limits for these four drugs were obtained as a function of desorber temperature and for heroin as a function of analysis time. Spectral and ionization interferences for each of the four drugs of interest were determined. Spectral interferences by innocuous materials are few; ionization interferences occur only at very high ratios of the mass of innocuous material to that of the drug of interest.

Amphetamine↗
PubMedDate not supplied

Detection of drug residues on the hands of subjects by surface sampling and ion mobility spectrometry.

This paper deals with the detection of drug residues on the hands of human subjects. The results demonstrate that detectable amounts of particulate matter are transferred to the hands by brief contact with drug tablets. A sampling and analysis method has been developed, and is based on the aspirating and trapping of drug microparticles on a filter plug, to be followed by thermal desorption directly into an ion mobility spectrometer. The technique is suited for initial field screening in clinical and forensic applications. The major drugs detected were diazepam, amitriptyline, codeine, acetaminophen, nitroglycerin, and delta 9-tetrahydrocannabinol (delta 9-THC).

Body Burden↗
PubMed2026

LC-IMS-MS profiling of avocado acetogenins reveals tissue-dependent distribution and cultivar-specific metabolic signatures.

This study presents a comprehensive characterisation of acetogenin-related metabolites in avocado using an LC-IMS-MS workflow. A total of 26 metabolites were semi-quantified across peel, pulp and seed tissues from three cultivars (Hass, Bacon and Fuerte). The integration of ion mobility spectrometry enabled the generation of the first experimental database of collision cross section (CCS) values for avocado acetogenins, improving confidence in metabolite annotation. Results revealed a pronounced tissue-dependent distribution, with seeds and pulp as the primary reservoir of several acetogenins, whereas the peel consistently exhibited lower concentrations. In contrast, acetogenin levels remained largely stable throughout ripening. Clear cultivar-dependent differences were observed, with Hass displaying a distinct metabolic profile compared to Bacon and Fuerte. Multivariate analysis confirmed these findings, showing tissue-dependent cultivar differentiation. This study provides new insights into avocado chemical diversity and highlights the potential of avocado by-products as consistent and promising sources of bioactive acetogenins.

Persea↗
PubMed1990

Ion mobility detection of polydimethylsilicone oligomers following supercritical fluid chromatographic separation.

A mixture of polydimethylsilicones (Dow Corning 200), average molecular weight 2000 a.m.u., was separated by simultaneous density and temperature-programmed supercritical fluid chromatography and detected by ion mobility detection. Ion mobility spectra were captured by Fourier transform ion mobility spectrometry. Using information from these spectra it was possible to selectively detect a single compound in the complex mixture. A detector temperature investigation demonstrated that, for the efficient transfer of high-molecular-weight compounds from the column to the detector, the interface to the detector must be heated. Using a 50 microns I.D. column, a Guthrie-type restrictor and a detection temperature of 250 degrees C, as many as 70 oligomers were separated and detected.

Chromatography, High Pressure Liquid↗
PubMed2025

Mass spectrometry-based top-down proteomics for proteoform profiling of protein coronas.

The protein corona is a layer of biomolecules-primarily proteins-that adsorbs to nanoparticle (NP) surfaces in biological fluids. If the purpose of the NP is therapeutic, this can have a profound effect on its biological activity and function in vivo. Protein corona formation can also be exploited for diagnostic purposes and to differentially enrich proteins for biomarker discovery. For all of these applications, it is useful to determine which proteins, and which specific proteoforms, bind to different types of NP. The traditional mass spectrometry (MS)-based bottom-up proteomics does not accurately identify specific proteoforms within the protein corona. This limitation impedes the nanomedicine field's ability to precisely predict the biological fate and pharmacokinetics of nanomedicines and their effectiveness in early-stage biomarker discovery and disease detection because many different proteoforms of the same gene could exist in the corona, and they have divergent biological functions. Here, we describe how to use capillary zone electrophoresis (CZE)-MS-based top-down proteomics to characterize the proteoform landscape of the protein corona. Our procedures detail the recovery of intact proteoforms from NP surfaces by using detergent-assisted proteoform elution and the measurement of these proteoforms by using CZE-tandem MS (MS/MS) and CZE-high-field asymmetric waveform ion mobility spectrometry (FAIMS)-MS/MS. The entire workflow is completed within 3-4 d. Using this protocol, hundreds of proteoforms from the protein corona of polystyrene NPs can be identified. Distinct protein corona proteoform profiles were observed from NPs with different physicochemical properties. The addition of FAIMS is beneficial for more in-depth proteoform characterization.

Proteomics↗
PubMed2026

A Parallel Accumulation-Mobility Aligned Fragmentation Strategy Utilizing High-Resolution Ion Mobility for High-Performance Proteomics Analysis.

Here we present a novel data-independent acquisition (DIA) mass spectrometry (MS) operating mode termed parallel accumulation-mobility aligned fragmentation (PAMAF) that offers enhanced speed and sensitivity of ion fragmentation analysis for discovery workflows such as bottom-up proteomics. This mode of operation leverages high-resolution ion mobility (HRIM) separation capabilities of the structures for lossless ion manipulation technology to achieve HRIM-based precursor isolation in place of traditional quadrupole filtering approaches. PAMAF mode increases the number of features that can be identified per MS1/MS2 acquisition cycle by employing mobility-based time alignment to associate fragment ions with their corresponding precursor ions. By using a high-speed, lossless separation technique for precursor isolation instead of the comparatively slow and wasteful quadrupole filtering, ion losses are avoided while simultaneously increasing the rate at which precursor ions are sequentially fragmented and detected. In addition, by accumulating ions while the previous packet of ions is being analyzed, the PAMAF mode achieves ∼100% ion utilization efficiency. Benchmarking results of LC-PAMAF-MS analysis of a whole cell protein digest showed ∼6× more protein group identifications compared to a standard data-dependent acquisition analysis without HRIM on the same QTOF instrument, and >100 x improvement for low-load workflows. Quantitative evaluations demonstrated that PAMAF mode could quantify low abundance peptides, including those undetectable by data-dependent acquisition. In addition, since precursor isolation in PAMAF mode is size-based rather than m/z-based, coeluting isobars and isomers can be resolved prior to fragmentation, eliminating chimeric spectra that compromise identification accuracy. We also explored the benefits of combining HRIM and quadrupole isolation to achieve improved specificity termed DIA-PAMAF mode, which enabled the detection of over 8000 protein groups from a HeLa digest analysis. PAMAF mode brings a powerful new technique to the field of proteomics with the potential to improve the sensitivity and selectivity of mass spectrometry-based proteomics.

Proteomics↗
PubMed2026

Spatial Proteomics of the Human Atherosclerotic Microenvironment Reveals Heterogeneity in Intraplaque Proteomes and Extracellular Matrix Remodeling.

Plaque heterogeneity underlies the propensity of atherosclerotic lesions to rupture and trigger cardiovascular events. Most proteomic studies examine bulk changes, obscuring key spatial differences in protein abundance. We report a high-resolution spatial proteomics workflow exploring the molecular landscape of human plaques and a murine myocardium. By combining laser capture microdissection with high-sensitivity ion-mobility mass spectrometry, spatial profiling of cellular and extracellular matrix (ECM) proteomes was achieved. Over 2700 proteins were detected from 50,000 μm2 areas, revealing substantial intraplaque heterogeneity across distinct regions (lipid-rich, media, shoulder, necrotic core, intima) and distance from the artery lumen. Inverse correlations between proteases (cathepsin B) and core structural ECM proteins (perlecan, HSPG2) indicated active ECM remodeling. Analysis of media layers indicated distinct protein signatures associated with smooth muscle contraction and cell-cell communication. Blood coagulation signatures, including platelet degranulation and fibrin formation, were enriched at the intima. Inflammatory (clusters of differentiation 4/68, CD4/CD68; vascular cell adhesion molecule 1, VCAM1) and vascular damage markers (tenascin-C, TNC) were enriched in shoulder regions. The necrotic core was dominated by blood proteins, consistent with intraplaque hemorrhage. This workflow resolves proteomic changes over ∼200 μm distances, providing unprecedented insights into plaque morphology and offers a powerful tool for elucidating plaque biology.

Humans↗
PubMed2026

Single-Cell Proteomics Reveals Proteome Remodeling and Cellular Heterogeneity During NGF-Induced PC12 Neuronal Differentiation.

Single-cell proteomics enables direct measurement of cellular heterogeneity during dynamic biological processes, but its application to fragile and highly adherent neuronal models remains challenging. Here, we developed and applied an optimized single-cell proteomics workflow to characterize proteome remodeling during nerve growth factor (NGF)-induced differentiation of PC12 cells. To enable reliable single-cell analysis, we implemented gentle dissociation, antiaggregation strategies, and thermal inkjet-based cell dispensing, achieving high accuracy in single-cell isolation. Inclusion of n-dodecyl-β-d-maltoside (DDM) improved recovery of membrane-associated and low-solubility proteins. Coupled with LC-ion mobility-mass spectrometry, this workflow enabled quantification of 2,000-3,000 proteins per cell across the differentiation time course. Single-cell proteomic analysis revealed progressive and heterogeneous proteome remodeling during differentiation. While undifferentiated cells formed a relatively homogeneous population, later stages (Days 4-6) exhibited increased variability, including multimodal protein abundance distributions and separation into distinct subpopulations. Dimensionality reduction, clustering, and non-negative matrix factorization identified multiple coexisting proteomic states within the same time points, reflecting asynchronous differentiation trajectories. These subpopulations were characterized by coordinated differences in pathways related to intracellular trafficking, protein translation, cytoskeletal organization, and neuronal maturation. Comparison with bulk proteomics demonstrated that proteins associated with differentiated neuronal states, including those involved in neurite formation and structural remodeling, are underrepresented in population-averaged measurements but are enriched within specific single-cell subpopulations. Temporal and cluster-resolved analyses further revealed distinct protein expression trajectories, including early decreases in cell cycle and metabolic pathways and later increases in neuronal structural and regulatory proteins. Together, this study establishes an optimized workflow for single-cell proteomics of neuronal systems and demonstrates that NGF-induced PC12 differentiation proceeds through heterogeneous and divergent proteomic states that are not resolved by bulk analysis.

Animals↗
PubMed2026

The chemical landscape of plant surface metabolites: Acylsugars as models of ecological function and structural diversity.

Plants produce a multifunctional assortment of specialized metabolites that play important roles in defense, environmental adaptation, and ecological interactions. Among these compounds, acylsugars, nonvolatile metabolites produced primarily in glandular trichomes of Solanaceae species, have emerged as informative model systems for understanding plant surface chemistry. Differences in acyl chain length, branching pattern, saturation, and attachment position generate extensive chemical diversity that influences herbivore deterrence, pathogen resistance, and the physicochemical properties of leaf surfaces. Recent advances in analytical chemistry, particularly liquid chromatography-ion mobility-tandem mass spectrometry (LC-IM-MS/MS), have greatly improved the ability to separate structurally related acylsugar isomers and characterize metabolite complexity at high resolution. When integrated with genomics, transcriptomics, and emerging spatial metabolomics approaches, these analytical tools provide new insights into acylsugar biosynthesis, pathway regulation, evolutionary diversification, and ecological function across plant species. This review positions acylsugars, particularly those of Solanum species, as model systems for understanding how structural diversity, spatial localization, and specialized metabolism shape ecological and physiological function at plant surfaces. We examine acylsugar structural diversity, biosynthetic pathways, ecological and physiological functions, and interactions with environmental and atmospheric processes. Major challenges, including extensive isomeric complexity, incomplete pathway characterization, and difficulties linking chemical structure to biological function, are discussed alongside emerging opportunities in integrative omics, crop improvement, sustainable pest management, and environmental monitoring. Overall, acylsugars provide a powerful model for linking molecular structure, spatial localization, and ecological function, offering broader insight into how specialized metabolism shapes plant adaptation, defense, and environmental interactions.

Acylsugars↗
PubMed1986

Inhibitors of Na+/H+ exchange block epinephrine- and ADP-induced stimulation of human platelet phospholipase C by blockade of arachidonic acid release at a prior step.

The ability of epinephrine or ADP to cause an increase in the production of phospholipase C products (diacylglycerol and inositol phosphates) in human platelets is blocked by perturbants of Na+/H+ exchange, i.e. ethylisopropylamiloride, decreased extraplatelet pH, or removal of extraplatelet Na+. These perturbants do not, however, block inositol phosphate production in response to 0.2 unit/ml thrombin, indicating that inhibition of Na+/H+ exchange does not inhibit the phospholipase C enzyme directly. Since the cyclooxygenase inhibitor indomethacin and the endoperoxide/thromboxane antagonist SQ29548 block epinephrine- and ADP-induced inositol phosphate production, it can be concluded that these agonists activate phospholipase C secondary to mobilization of arachidonic acid and production of cyclooxygenase products. This conclusion is consistent with the observation that the endoperoxide analogue U46619 causes inositol phosphate production. Furthermore, the effect of U46619 is not blocked by inhibitors of Na+/H+ exchange. The initial pool of arachidonic acid mobilized by epinephrine can be measured using negative ion gas chromatography/mass spectrometry and is sensitive to inhibition of Na+/H+ exchange. The present data suggest that epinephrine and ADP cause mobilization of a small pool of arachidonic acid by a pathway involving Na+/H+ exchange. The cyclooxygenase products derived from this pool subsequently activate phospholipase C. Since the same treatments that block epinephrine- and ADP-induced diacylglycerol and inositol phosphate production also block epinephrine- and ADP-induced dense granule secretion, it appears that activation of phospholipase C, albeit indirectly via cyclooxygenase products, may be required for epinephrine and ADP to evoke platelet secretion.

Adenosine Diphosphate↗
PubMed1989

Capillary supercritical fluid chromatography/negative ion chemical ionization mass spectrometry of trichothecenes.

A capillary supercritical fluid chromatography/mass spectrometry interface incorporating a heated frit restrictor is described. The trichothecene mycotoxins T-2 toxin, deoxynivalenol and roridin A were used to evaluate the effect of restrictor temperature and carbon dioxide mobile phase on the negative ion chemical ionization (CI) spectra of these compounds under electron capture, proton abstraction and chloride attachment conditions. Restrictor temperatures less than 100 degrees C above the melting point of the samples retarded sample transfer into the mass spectrometer, but neither restrictor temperature nor carbon dioxide mobile phase significantly affected negative ion CI conditions.

Anti-Bacterial Agents↗