Rapid diagnosis of drug agglomeration and crystallinity in pharmaceutical preparations by electrospray laser desorption ionization mass spectrometry imaging.

In this study we evaluate the applicability of electrospray laser desorption ionization mass spectrometry imaging (ELDI-MSI) to interrogate tablet formulations for the spatial distributions of ingredients. Tablet formulations with varying amounts of crystalline acetaminophen (the active pharmaceutical ingredient, API) were analyzed to determine if crystallinity could be evaluated via ELDI-MSI. ELDI-MSI concurrently imaged the (API, binders, and surfactants.

Light-Dependent Changes in the Spatial Localization of Metabolites in (Coleus Henna) Visualized by Matrix-Free Atmospheric Pressure Electrospray Laser Desorption Ionization Mass Spectrometry Imaging.

The visualization of foliage color in plants provides immediate insight into some of the compounds that exist in the leaf. However, many non-colored compounds are also present; their cellular distributions are not readily identifiable optically. In this study we evaluate the applicability of mass spectrometry imaging (MSI) via electrospray laser desorption ionization (ELDI) to reveal the spatial distribution of metabolites.

Abundance and Impact of Doubly Charged Polyatomic Argon Interferences in ICPMS Spectra.

Doubly charged molecular ions of alkaline earth metals and argon could be identified as spectral interferences in an inductively coupled plasma mass spectrometer. These molecular ions were found to occur at abundances reaching about 10(-4) relative to the alkaline earth atomic ion abundances. They can thus substantially affect ultratrace analyses and, when present at similar concentration as the analyte elements, also isotope ratio measurements.

Mass Spectrometric Observation of Doubly Charged Alkaline-Earth Argon Ions.

Doubly charged diatomic ions MAr(2+) where M=Mg, Ca, Sr or Ba have been observed by mass spectrometry with an inductively coupled plasma ion source. Abundance ratios are quite high, 0.1 % for MgAr(2+) , 0.

Giant magnetic anisotropy and tunnelling of the magnetization in Li₂(Li(1-x)Fe(x))N.

Large magnetic anisotropy and coercivity are key properties of functional magnetic materials and are generally associated with rare earth elements. Here we show an extreme, uniaxial magnetic anisotropy and the emergence of magnetic hysteresis in Li₂(Li(1-x)Fe(x))N. An extrapolated, magnetic anisotropy field of 220 T and a coercivity field of over 11 T at 2 K outperform all known hard ferromagnets and single-molecular magnets.

High-resolution time-of-flight mass spectrometry fingerprinting of metabolites from cecum and distal colon contents of rats fed resistant starch.

Time-of-flight mass spectrometry along with statistical analysis was utilized to study metabolic profiles among rats fed resistant starch (RS) diets. Fischer 344 rats were fed four starch diets consisting of 55 % (w/w, dbs) starch. A control starch diet consisting of corn starch was compared against three RS diets.

Analysis of resistant starches in rat cecal contents using Fourier transform infrared photoacoustic spectroscopy.

Fourier transform infrared photoacoustic spectroscopy (FTIR-PAS) qualitatively and quantitatively measured resistant starch (RS) in rat cecal contents. Fisher 344 rats were fed diets of 55% (w/w, dry basis) starch for 8 weeks. Cecal contents were collected from sacrificed rats.

Selenium-modified TiO2 and its impact on photocatalysis.

This work describes the preparation of a selenium-modified TiO(2) photocatalyst and a preliminary evaluation of its photocatalytic activity. Se-TiO(2) displayed greater visible absorption than undoped TiO(2) and was still capable of degrading quinoline at a slightly faster rate than undoped TiO(2) under UV light. Se-TiO(2) was also able to degrade organic molecules under purely visible light by a single electron transfer pathway.

Effects of ion/ion proton transfer reactions on conformation of gas-phase cytochrome c ions.

Positive ions from cytochrome c are studied in a 3-D ion trap/ion mobility (IM)/quadrupole-time-of-flight (TOF) instrument with three independent ion sources. The IM separation allows measurement of the cross section of the ions. Ion/ion reactions in the 3-D ion trap that remove protons cause the cytochrome c ions to refold gently without other degradation of protein structure, i.

Atmospheric pressure laser desorption/ionization of plant metabolites and plant tissue using colloidal graphite.

Colloidal graphite is a promising matrix for atmospheric pressure laser desorption/ionization mass spectrometry. Intact [M+H](+) and [M-H](-) ions are readily produced from a wide range of small molecule plant metabolites, particularly anthocyanins, fatty acids, lipids, glycerides, and ceramides. Compared with a more traditional organic acid matrix, colloidal graphite provides more efficient ionization for small hydrophobic molecules and has a much cleaner background spectrum, especially in negative ion mode.

Reduction of matrix effects in inductively coupled plasma mass spectrometry by flow injection with an unshielded torch.

Solution samples with matrix concentrations above approximately 0.1% generally present difficulties for analysis by inductively coupled plasma mass spectrometry (ICP-MS) because of cone clogging and matrix effects. Flow injection (FI) is coupled to ICP-MS to reduce deposition from samples such as 1% sodium salts (as NaCl) and seawater (approximately 3% dissolved salts).

An ion trap-ion mobility-time of flight mass spectrometer with three ion sources for ion/ion reactions.

This instrument combines the capabilities of ion/ion reactions with ion mobility (IM) and time-of-flight (TOF) measurements for conformation studies and top-down analysis of large biomolecules. Ubiquitin ions from either of two electrospray ionization (ESI) sources are stored in a three dimensional (3D) ion trap (IT) and reacted with negative ions from atmospheric sampling glow discharge ionization (ASGDI). The proton transfer reaction products are then separated by IM and analyzed via a TOF mass analyzer.

A linear ion trap mass spectrometer with versatile control and data acquisition for ion/ion reactions.

A linear ion trap (LIT) with electrospray ionization (ESI) for top-down protein analysis has been constructed. An independent atmospheric sampling glow discharge ionization (ASGDI) source produces reagent ions for ion/ion reactions. The device is also meant to enable a wide variety of ion/ion reaction studies.

Theoretical investigation of small polyatomic ions observed in inductively coupled plasma mass spectrometry: H(x)CO+ and H(x)N2(+) (x = 1, 2, 3).

Two series of small polyatomic ions, HxCO+ and HxN2(+) (x = 1, 2, 3), were systematically characterized using three correlated theoretical techniques: density functional theory using the B3LYP functional, spin-restricted second-order perturbation theory, and singles + doubles coupled cluster theory with perturbative triples. On the basis of thermodynamic data, the existence of these ions in inductively coupled plasma mass spectrometry (ICP-MS) experiments is not surprising since the ions are predicted to be considerably more stable than their corresponding dissociation products (by 30-170 kcal/mol). While each pair of isoelectronic ions exhibit very similar thermodynamic and kinetic characteristics, there are significant differences within each series.

Normal cellular prion protein protects against manganese-induced oxidative stress and apoptotic cell death.

The normal prion protein is abundantly expressed in the central nervous system, but its biological function remains unclear. The prion protein has octapeptide repeat regions that bind to several divalent metals, suggesting that the prion proteins may alter the toxic effect of environmental neurotoxic metals. In the present study, we systematically examined whether prion protein modifies the neurotoxicity of manganese (Mn) by comparing the effect of Mn on mouse neural cells expressing prion protein (PrP(C)-cells) and prion-knockout (PrP(KO)-cells).

Analysis of glass fragments by laser ablation-inductively coupled plasma-mass spectrometry and principal component analysis.

Laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) is used to differentiate glass samples with similar optical and physical properties based on trace elemental composition. Laser ablation increases the number of elements that can be used for differentiation by eliminating problems commonly associated with dissolution and contamination. In this study, standard residential window and tempered glass samples that could not be differentiated by refractive index or density were successfully differentiated by LA-ICP-MS.

Urinary metal and polycyclic aromatic hydrocarbon biomarkers in boilermakers exposed to metal fume and residual oil fly ash.

Background: Boilermakers are occupationally exposed to known carcinogens.

Methods: The association of urinary 1-hydroxy-pyrene (1-OHP), a biomarker of polycyclic aromatic hydrocarbon (PAH) exposure, with biomarkers of metal exposure (vanadium, chromium, manganese, nickel, copper, and lead) in boilermakers exposed to metal fume from welding and dust particulates from residual oil fly ash (ROFA) was examined. A repeated measures cohort study was conducted during the overhaul of an oil-fired boiler.

Behavior of bacteria in the inductively coupled plasma: atomization and production of atomic ions for mass spectrometry.

The combination of perfusion chromatography (PC) and inductively coupled plasma mass spectrometry (ICPMS) is a fast, general way to monitor metal incorporation into bacteria. U+ signals from U incorporated intrinsically in Bacillus subtilis (B. subtilis) are measured with 4 ms time resolution to investigate the behavior of individual cells in the ICP.

Controlled dissolution for elemental analysis of sample layers by inductively coupled plasma-mass spectrometry: a feasibility study.

Aqueous acid mixtures at room temperature are used to partially dissolve steel samples. The dissolved elements are washed off the surface, diluted, and then determined by inductively coupled plasma-mass spectrometry (ICP-MS) using a magnetic sector mass analyzer. The amount of material removed is measured from the amount of Fe dissolved and increases linearly with HNO(3) concentration in the etch acid.

Multivariate pattern matching of trace elements in solids by laser ablation inductively coupled plasma-mass spectrometry: source attribution and preliminary diagnosis of fractionation.

Laser ablation inductively coupled plasma mass spectrometry (LA-ICPMS) is used with two variations of principal components analysis (PCA) for objective, routine comparisons of forensic materials without time-consuming and destructive sample dissolution. The relative concentrations of trace elements in a solid sample are examined to provide a "fingerprint" composition that can be used for identification and source matching of the material. Residue samples are matched to bulk materials using PCA.

Smoking status and occupational exposure affects oxidative DNA injury in boilermakers exposed to metal fume and residual oil fly ash.

Epidemiologic studies demonstrate increased cancer incidence among workers exposed to polycyclic aromatic hydrocarbons (PAH) and metals, probably through cumulative oxidative DNA damage in response to carcinogens. Boilermakers are exposed to particulates of residual oil fly ash (ROFA) and metal fume that contain carcinogenic PAH and metals. We conducted a repeated-measures cohort study in boilermakers during the overhaul of an oil-fired boiler to determine a possible association between the level of 8-hydroxy-2'-deoxyguanosine (8-OH-dG; an oxidative injury biomarker) and biomarkers of PAH (1-hydroxypyrene; 1-OHP) and metal exposure.

Pore exclusion chromatography-inductively coupled plasma-mass spectrometry for monitoring elements in bacteria: a study on microbial removal of uranium from aqueous solution.

The interstitial spaces between spherical particles in a packed column can act as a sieve that passes microorganisms below a certain size. If the bed is a perfusion-type material (containing a binary distribution of large and small pores), colloidal-size microorganisms are subject only to pore exclusion, while all molecules are subject to size exclusion among the various pores. Thus, microorganisms elute first, followed by macromolecules, and then small molecules.

Association of expired nitric oxide with urinary metal concentrations in boilermakers exposed to residual oil fly ash.

Background: Exposure to metal-containing particulate matter has been associated with adverse pulmonary responses. Metals in particulate matter are soluble, hence are readily recovered in urine of exposed individuals. This study investigated the association between urinary metal concentrations and the fractional concentration of expired nitric oxide (F(E)NO) in boilermakers (N = 32) exposed to residual oil fly ash (ROFA).

Tandem mass spectrometry of metal nitrate negative ions produced by electrospray ionization.

M(NO(3))(x)(-) ions are generated by electrospray ionization (ESI) of metal solutions in nitric acid in negative ion mode. Collision-induced reactions of these ions are monitored in a tandem mass spectrometer (MS) of quadrupole-octopole-quadrupole (QoQ) geometry. For Group 1 and 2 elements, the M(NO(3))(x)(-) ions dissociate into NO(3)(-) and neutral metal nitrate molecules.

Determination of carbon isotope ratios in amino acids, proteins, and oligosaccharides by inductively coupled plasma-mass spectrometry.

Carbon isotope ratios ((12)C/(13)C) are measured for aqueous solutions of tryptophan, myoglobin, and beta-cyclodextrin using C(+) ions from an inductively coupled plasma (ICP) and a prototype twin quadrupole mass spectrometer (MS). (13)C/(12)C ratios can be determined with a relative standard deviation (RSD) of approximately 1%. This precision is close to the limiting value predicted by counting statistics (1.