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Quality Spectra (quality + spectrum)
Selected AbstractsThe use of in vitro technologies coupled with high resolution accurate mass LC-MS for studying drug metabolism in equine drug surveillanceDRUG TESTING AND ANALYSIS, Issue 1 2010James P. Scarth Abstract The detection of drug abuse in horseracing often requires knowledge of drug metabolism, especially if urine is the matrix of choice. In this study, equine liver/lung microsomes/S9 tissue fractions were used to study the phase I metabolism of eight drugs of relevance to equine drug surveillance (acepromazine, azaperone, celecoxib, fentanyl, fluphenazine, mepivacaine, methylphenidate and tripelennamine). In vitro samples were analyzed qualitatively alongside samples originating from in vivo administrations using LC-MS on a high resolution accurate mass Thermo Orbitrap Discovery instrument and by LC-MS/MS on an Applied Biosystems Sciex 5500 Q Trap. Using high resolution accurate mass full-scan analysis on the Orbitrap, the in vitro systems were found to generate at least the two most abundant phase I metabolites observed in vitro for all eight drugs studied. In the majority of cases, in vitro experiments were also able to generate the minor in vivo metabolites and sometimes metabolites that were only observed in vitro. More detailed analyses of fentanyl incubates using LC-MS/MS showed that it was possible to generate good quality spectra from the metabolites generated in vitro. These data support the suggestion of using in vitro incubates as metabolite reference material in place of in vivo post-administration samples in accordance with new qualitative identification guidelines in the 2009 International Laboratory Accreditation Cooperation-G7 (ILAC-G7) document. In summary, the in vitro and in vivo phase I metabolism results reported herein compare well and demonstrate the potential of in vitro studies to compliment, refine and reduce the existing equine in vivo paradigm. Copyright © 2010 John Wiley & Sons, Ltd. [source] Laser desorption/ionization techniques in the characterization of high molecular weight oil fractions.JOURNAL OF MASS SPECTROMETRY (INCORP BIOLOGICAL MASS SPECTROMETRY), Issue 9 2006Part 1: asphaltenes Abstract The molecular weight distribution of the asphaltene fractions of two types of crude oils from two different Italian fields (samples 1 and 2) was investigated. The analytical tools used to perform these analyses were matrix assisted laser desorption ionization (MALDI) and laser desorption ionization (LDI) mass spectrometry. After observing that the use of the matrix (as well as the addition of Ag+) did not improve the quality of the data compared to that obtained in LDI conditions, all further measurements were performed with the latter technique. Operating under usual conditions of laser power and delay time, a very low resolution was observed, showing only macroscopic differences between the two samples in the molecular weight distribution of the different components. An accurate study on the possible reasons of this undesirable behavior indicates that it can originate from space charge phenomena occurring either in the ion source region or during the flight. A valid parameterization of the delay time and the laser power allowed higher quality spectra to be obtained. Surface-enhanced laser desorption ionization (SELDI) measurements were also performed using normal phase (silica) as the sample holder surface. Under these conditions, better results are obtained, proving that the sample,surface interaction is important to achieve, by means of laser irradiation, a homogeneous set of product ions. Both asphaltene samples were fractionated in five subfractions by gel-permeation chromatography (GPC) to obtain a better separation of the molecular weight distributions; the related spectra confirmed these findings. By using different approaches, relevant and reproducible differences between the asphaltene fractions of the two oil samples were observed. Copyright © 2006 John Wiley & Sons, Ltd. [source] INTERCOLONIAL VARIABILITY IN MACROMOLECULAR COMPOSITION IN P-STARVED AND P-REPLETE SCENEDESMUS POPULATIONS REVEALED BY INFRARED MICROSPECTROSCOPY,JOURNAL OF PHYCOLOGY, Issue 5 2008Philip Heraud Macromolecular variability in microalgal populations subject to different nutrient environments was investigated, using the chlorophyte alga Scenedesmus quadricauda (Turpin) Bréb. as a model organism. The large size of the four-cell coenobia in the strain used in this study (,35 ,m diameter) conveniently allowed high quality spectra to be obtained from individual coenobia using a laboratory-based Fourier transform infrared (FTIR) microscope with a conventional globar source of IR. By drawing sizable subpopulations of coenobia from two Scenedesmus cultures grown under either nutrient-replete or P-starved conditions, the population variability in macromolecular composition, and the effects of nutrient change upon this, could be estimated. On average, P-starved coenobia had higher carbohydrate and lower protein absorbance compared with P-replete coenobia. These parameters varied between coenobia with histograms of the ratio of absorbance of the largest protein and carbohydrate bands being Gaussian distributed. Distributions for the P-replete and P-starved subpopulations were nonoverlapping, with the difference in mean ratios for the two populations being statistically significant. Greater variance was observed in the P-starved subpopulation. In addition, multivariate models were developed using the spectral data, which could accurately predict the nutrient status of an independent individual coenobium, based on its FTIR spectrum. Partial least squares discriminant analysis (PLS-DA) was a better prediction method compared with soft independent modeling by class analogy (SIMCA). [source] Matrix/analyte ratio influencing polymer molecular weight distribution in matrix-assisted laser desorption/ionization time-of-flight mass spectrometryRAPID COMMUNICATIONS IN MASS SPECTROMETRY, Issue 9 2009Gitta Schlosser Matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF-MS) has been used to characterize poly(L-lysine) polymers and unique oligomer peptides, like 10-, 15- and 25-mer [Lys]n oligolysine peptides. Several matrices have been tried in order to find optimal conditions, but only , -cyano-4-hydroxycinnamic acid gave analytically useful spectra. The synthetic oligomers and their mixtures gave good quality spectra, showing protonated and cationized molecules, including doubly charged species. The polymers, analogously, gave a wide distribution of single- and double-cationized peak series. The polymer distributions observed indicate the presence of significant suppression effects. The concentration (matrix/analyte ratio) was found to influence the results significantly; distributions shifting to higher masses when higher polymer concentrations were used. This effect was studied in detail using the synthetic (,monodisperse') oligolysine peptides. It was found that the relative intensities change by over an order of magnitude in the 0.1,10,pmol/µL concentration range (typical for most proteomic analyses). The results indicate that concentration effects need to be considered when MALDI-MS is used for quantitative purposes. Copyright © 2009 John Wiley & Sons, Ltd. [source] Elemental abundance analyses with DAO spectrograms: XXX.ASTRONOMISCHE NACHRICHTEN, Issue 4 20102 Ceti (B9 III), 21 Aquilae (B8 II-III), Aquilae (B5 III), Delphini (A2V), The middle B through early A stars Abstract This series of high quality elemental abundance analyses of mostly main-sequence band normal and peculiar B, A, and F stars defines their properties and provides data for the comparison with the analyses of somewhat similar stars and with theoretical predictions. Most use high dispersion and high S/N (, 200) spectrograms obtained with CCD detectors at the long camera of the Coudé spectrograph of the 1.22-m Dominion Astrophysical Observatory telescope. Here we reanalyze 21 Aql with better quality spectra and increase the number of stars consistently analyzed in the spectral range B5 to A2 by analyzing three new stars for this series. In the early A stars the normal and non-mCP stars have abundances with overlapping ranges. But more stars are needed especially in the B5 to B9 range. ,2 Cet on average has a solar composition with a few abundances outside the solar range while both 21 Aql and , Aql have abundances marginally less than solar. The abundances of , Del are greater than solar with a few elements such as Ca being less than solar. It is an Am star (© 2010 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim) [source] | ||||||||||