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61.
Mauriala T Chauret N Oballa R Nicoll-Griffith DA Bateman KP 《Rapid communications in mass spectrometry : RCM》2005,19(14):1984-1992
Discovery stage studies that address issues of absorption, distribution, metabolism and excretion (ADME) are vital for lead optimization resulting in new drug candidates. Often pharmacokinetics (PK) is assessed in these experiments without regard for the metabolism of the compound or the potential for metabolites to circulate in vivo. This work presents a strategy for drug level determination and detection of metabolites using dried blood spots for sample collection. Initially, metabolites are detected from microsomal incubations and characterized using tandem mass spectrometry. Data dependent enhanced MS and enhanced product ion (EMS-EPI) scanning with dynamic background subtraction was used on a hybrid quadruple linear ion trap mass spectrometer. On-the-fly background subtraction greatly improved the detection of metabolites. These data were used to build a multiple reaction monitoring (MRM) method for the parent and metabolites. MRM-EPI scanning was used to analyze the extracted dried blood spots from the PK study. Circulating metabolites were detected using MRM and their identities confirmed on the basis of fragment ion spectra collected simultaneously. The use of dried blood spots provides a means for re-analysis of PK samples for metabolite identification without the need for complex sample storage and preparation. Both parent compound and metabolite information can be collected in these studies, resulting in a savings of time and resources. 相似文献
62.
Anna Mujal-Colilles Jose M. Mier Kenneth T. Christensen Allen Bateman Marcelo H. Garcia 《Experiments in fluids》2014,55(1):1-19
Exploratory measurements of oscillatory boundary layers were conducted over a smooth and two different rough beds spanning the laminar, transitional and turbulent flow regimes using a multi-camera 2D-PIV system in a small oscillatory-flow tunnel (Admiraal et al. in J Hydraul Res 44(4):437–450, 2006). Results show how the phase lag between bed shear stress and free-stream velocity is better defined when the integral of the momentum equation is used to estimate the bed shear stress. Observed differences in bed shear stress and phase lag between bed shear stress and free-stream velocity are highly sensitive to the definition of the bed position (y = b). The underestimation of turbulent stresses close to the wall is found to explain such differences when using the addition of Reynolds and viscous stresses to define both the bed shear stress and the phase lag. Regardless of the flow regime, in all experiments, boundary-layer thickness reached its maximum value at a phase near the flow reversal at the wall. Friction factors in smooth walls are better estimated using a theoretical equation first proposed by Batchelor (An introduction to fluid dynamics. Cambridge University Press, Cambridge, 1967) while the more recent empirical predictor of Pedocchi and Garcia (J Hydraul Res 47(4):438–444, 2009a) was found to be appropriate for estimating friction coefficients in the laminar-to-turbulent transition regime. 相似文献
63.
Wattenberg A Organ AJ Schneider K Tyldesley R Bordoli R Bateman RH 《Journal of the American Society for Mass Spectrometry》2002,13(7):772-783
A study has been undertaken to evaluate the usefulness of MALDI Q-TOF data for protein identification. The comparison of MS data of protein digests obtained on a conventional MALDI TOF instrument to the MS data from the MALDI Q-TOF reveal peptide patterns with similar intensity ratios. However, comparison of MS/MS Q-TOF data produced by nanoelectrospray versus MALDI reveals striking differences. Peptide fragment ions obtained from doubly charged precursors produced by nanoelectrospray are mainly y-type ions with some b-ions in the lower mass range. In contrast, peptide fragment ions produced from the singly charged ions originating from the MALDI source are a mixture of y-, b- and a-ions accompanied by ions resulting from neutral loss of ammonia or water. The ratio and intensity of these fragment ions is found to be strongly sequence dependent for MALDI generated ions. The singly charged peptides generated by MALDI show a preferential cleavage of the C-terminal bond of acidic residues aspartic and glutamic acid and the N-terminal bond of proline. This preferential cleavage can be explained by the mobile proton model and is present in peptides that contain both arginine and an acidic amino acid. The MALDI Q-TOF MS/MS data of 24 out of 26 proteolytic peptides produced by trypsin or Asp-N digestions were successfully used for protein identification via database searching, thus indicating the general usefulness of the data for protein identification. De novo sequencing using a mixture of 160/18O water during digestion has been explored and de novo sequences for a number of peptides have been obtained. 相似文献
64.
Ranya Simons Stefanie Nina Guntari Tor Kit Goh Greg G. Qiao Stuart A. Bateman 《Journal of polymer science. Part A, Polymer chemistry》2012,50(1):89-97
Exfoliated poly(dicyclopentadiene) (pDCPD)—montmorillonite (MMT) nanocomposites were synthesized via intergallery‐surface‐initiated ring opening metathesis polymerization (ROMP). This is the first example of in situ polymerization of pDCPD from clay intergallery surfaces using ROMP. Grubbs catalyst was immobilized on the surface of MMT clay modified with vinylbenzyl dimethyloctadecyl ammonium chloride (VOAC), and DCPD polymerized from the clay surface while simultaneously crosslinking to form a thermoset nanocomposite in a one‐pot reaction. X‐ray diffraction and transmission electron microscopy analysis indicated that the resultant nanocomposites exhibited exfoliated morphologies with heterogeneous clay platelet distribution. Conventional bulk‐initiated nanocomposites containing VOAC modified MMT were also synthesized as a comparison, and these resulted in nanocomposites with intercalated morphologies. The differences between the morphologies demonstrated that growing polymer chains from the initiator sites on the intergallery surface of the clay platelets pushed the platelets apart during the polymerization of the intergallery‐surface‐initiated nanocomposites, aiding in the exfoliation process. Compression testing indicated that the intergallery‐surface‐initiated nanocomposites led to improvements of up to 50% in the compressive Young's Modulus, while the bulk‐initiated nanocomposites at the same clay loadings did not exhibit improved properties. © 2011 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem, 2012 相似文献
65.
Kevin P. Bateman Markus Kellmann Helmut Muenster Robert Papp Lester Taylor 《Journal of the American Society for Mass Spectrometry》2009,20(8):1441-1450
Current approaches to discovery-stage drug metabolism studies (pharmacokinetics, microsomal stability, etc. ) typically use
triple-quadrupole-based approaches for quantitative analysis. This necessitates the optimization of parameters such as Q1
and Q3 m/z values, collision energy, and interface voltages. These studies detect only the specified compound and information about
other components, such as metabolites, is lost. The ability to perform full-scan acquisition for quantitative analysis would
eliminate the need for compound optimization while enabling the detection of metabolites and other non-drug-related endogenous
components. Such an instrument would have to provide sensitivity, selectivity, dynamic range, and scan speed suitable for
discovery-stage quantitative studies. In this study, a prototype benchtop Orbitrap-based mass analyzer was used to collect
both quantitative and qualitative data from human microsomal incubation samples as well as rat plasma from pharmacokinetic
studies. Instrumental parameters such as scan speed, resolution, and mass accuracy are discussed in relation to the requirements
for a quantitative-qualitative workflow. The ability to perform highly selective quantitative analysis while simultaneously
characterizing metabolites from both in vitro and in vivo studies is discussed. 相似文献
66.
E. Bateman 《Fresenius' Journal of Analytical Chemistry》1916,55(4):211-213
Ohne Zusammenfassung 相似文献
67.
Authority roles among teachers and students have traditionally been hierarchal and centered with the expertise and power of the teacher limiting opportunities for students to act with autonomy to build and justify mathematics. In this paper we discuss authority roles for teachers and students that have been realized in an inquiry-based university, honors calculus classroom. We define and discuss four types of authority we identified from video data: institutional, expertise, mathematical, and performative. We suggest that the institutional authority of the instructor is present whether or not she is acting with the intention to bear authority, thereby interfering with the instructor's ability to share authority with her students. Further, we believe that the traditional focus on the bearer of authority limits our ability to create environments wherein authority can be shared. Instead we suggest that a focus on empowering the receiver to recognize expertise and mathematical authorities may be more fruitful. 相似文献
68.
Kenny DJ Brown JM Palmer ME Snel MF Bateman RH 《Journal of the American Society for Mass Spectrometry》2006,17(1):60-66
We present a novel enhancement to matrix-assisted laser desorption ionization (MALDI) post-source decay (PSD) analysis whereby fragment ions from multiple precursor ions are acquired into the same spectrum without employing a timed ion gate to preselect each parent ion. Fragment ions are matched to their corresponding precursor ions by comparing spectra acquired at slightly different reflectron electric fields. By measuring the difference in time-of-flight (TOF) between the two spectra for each fragment, it is possible to calculate the mass of the fragment ion and its parent. This new "parallel PSD" technique reduces analysis time and consumes less sample than conventional PSD, which requires an ion gate for serial preselection of precursor ions. 相似文献
69.
70.
Lewin M Guilhaus M Wildgoose J Hoyes J Bateman B 《Rapid communications in mass spectrometry : RCM》2002,16(6):609-615
Ions experience small deflections in the vicinity of grids in accelerators and ion mirrors in time-of-flight (TOF) mass spectrometers. Recent experiments with an orthogonal acceleration (oa) TOF instrument have verified that the effect can significantly degrade resolution when ions approach grids at an angle deviating from 90 degrees. The phenomenon becomes significant only when ions have components of velocity at right angles to the wires of the grids. A model is presented in this study to predict this phenomenon for parallel wire grids. The fractional energy spread of ions (calculated in the static TOF-spectrometer frame of reference) scales directly with the approach angle of ions to the grid (as measured from normal approach). The energy spread also scales with the range of angles that is a consequence of the focusing effect in each gap between the wires of the grid. The equations imply that closely spaced parallel wire grids are best for deployment in oa-TOF systems where non-zero approach angles are unavoidable. Such grids are relatively impractical to manufacture and support but rectangular repeat cell grids with relatively few wires at right angles to the source axis are shown experimentally to introduce minimal energy spread. When these grids are rotated by 90 degrees, the resolution measured in a Q-TOF spectrometer is degraded in approximate agreement with the parallel wire model. A practical implication of this work is that grid transmissions in oa-TOF systems may be significantly increased without loss of resolution. Improvements of approximately 200% (V-mode) and approximately 400% (W-mode) in ion transmission were obtained in this study without compromising resolution. This was achieved with approximately 73% transmission grids and greater potential improvements in transmission are being realised since this study with approximately 89% transmission grids having similar geometry. 相似文献