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1.
Brenton R. Clarke 《Journal of multivariate analysis》2007,98(5):916-931
In this paper, we consider the estimation of a parameter of interest where the estimator is one of the possibly several solutions of a set of nonlinear empirical equations. Since Newton's method is often used in such a setting to obtain a solution, it is important to know whether the so obtained iteration converges to the locally unique consistent root to the aforementioned parameter of interest. Under some conditions, we show that this is eventually the case when starting the iteration from within a ball about the true parameter whose size does not depend on n. Any preliminary almost surely consistent estimate will eventually lie in such a ball and therefore provides a suitable starting point for large enough n. As examples, we will apply our results in the context of M-estimates, kernel density estimates, as well as minimum distance estimates. 相似文献
2.
Z. V. I. Zaretskii J. M. Curtis A. G. Brenton J. H. Beynon Carl Djerassi 《Journal of mass spectrometry : JMS》1988,23(6):453-459
The mechanism of water elimination from metastable molecular, [M ? CH3˙]+ and [M ? ring D]+˙ ions of epimeric 3-hydroxy steroids of the 5α-series has been elucidated. Deuterium labelling, the measurement of the translational energy released during the loss of water, and collision-induced decomposition mass-analysed kinetic energy spectrometry were the techniques used. It was found that the mechanisms of water loss from metastable M+˙ and [M ? ring D]+˙ ions is different from that from [M ? CH3˙]+ ions. 相似文献
3.
Russell P. Newton Jalal A. Khan Dipankar Ghosh James I. Langridge A. Gareth Brenton Frank M. Harris Terence J. Walton 《Journal of mass spectrometry : JMS》1991,26(5):447-453
The determination of cytidine 3′,5′-cyclic monophosphate-specific phosphodiesterase activity by means of fast-atom bombardment (FAB) mass Spectrometry with mass-analysed ion kinetic energy (MIKE) spectrum scanning is described. Initial efforts to determine the activity of the enzyme by this method were unsuccessful owing to the obfuscation of sample-related peaks by peaks emanating from the incubation buffer and cation adducts; dilution of buffer and a desalting procedure overcame these difficulties. In the resulting positive-ion FAB mass spectra, characteristic peaks of the enzyme substrate and product could be readily identified and the protonated molecular ions selected for MIKE scanning. By spiking enzyme incubates with known amounts of substrate and product, and measuring peak heights in the MIKE spectra of both spiked and unspiked samples, the substrate/product ratio at the end of a series of phosphodiesterase incubations was determined. From the data obtained, the Km and Vmax of the phosphodiesterase were calculated as 6.08 mM and 11 μmol min?1 mg?1, respectively, showing good agreement with the analogous values of 8.06 mM and 5.8 μmol?1 min?1 mg?1 obtained by radioactive assay. 相似文献
4.
Joachim G. Liehr Gareth A. Brenton John H. Beynon James A. McCloskey Wolfgang Blum Wilhelm J. Richter 《Helvetica chimica acta》1981,64(3):835-843
In isobutane chemical ionization mass spectrometry benzyl alcohol exhibits ions at m/z 147 (‘M + 39’) that arise by a loss of H2O from [M + C4H9]+, i.e. ‘M + 57’ complex ions. Electrophilic aromatic substitution of a proton at an ortho-position of neutral C6H5CH2OH with [t-C4H9]+ and, alternatively, nucleophilic substitution of H2O at the benzylic carbon in \documentclass{article}\pagestyle{empty}\begin{document}$ {\rm C_6 H_5 CH_2}\mathop {\rm O}\limits^+ {\rm H}_2 $\end{document} with CH2?C (CH3)2 are discussed as possible pathways. Evidence in favor of the latter is derived from the analysis of C6D5CH2OH and C6H5CD2OH for the origin of the H-atoms lost in H2O. The inferred ion structure of m/z 147 is verified by mass-analyzed ion kinetic energy (MIKE.) measurements of its collision-activated (CA.) decomposition. MIKE./CA. spectra of mass-selected m/z 147 ions, once generated by (CI(i-C4H10) from benzyl alcohol and, once, from 2-methyl-4-phenyl-2-butanol match closely and, thus, reflect identical ion structures. With reference to the simple genesis of this ion from the latter precursor, the structure in question can be concluded to be \documentclass{article}\pagestyle{empty}\begin{document}$ {\rm C_6 H_5 CH_2 CH_2}\mathop {\rm C}\limits^+ ({\rm CH}_3)_2 $\end{document} . 相似文献
5.
A. R. Godfrey C. M. Williams E. Dudley R. P. Newton P. Willshaw A. Mikhail L. Bastin A. G. Brenton 《Rapid communications in mass spectrometry : RCM》2009,23(19):3194-3204
Historically, structural elucidation of unknown analytes by mass spectrometry alone has involved tandem mass spectrometry experiments using electron ionization. Most target molecules for bioanalysis in the metabolome are unsuitable for detection by this previous methodology. Recent publications have used high‐resolution accurate mass analysis using an LTQ‐Orbitrap with the more modern approach of electrospray ionization to identify new metabolites of known metabolic pathways. We have investigated the use of this methodology to build accurate mass fragmentation maps for the structural elucidation of unknown compounds. This has included the development and validation of a novel multi‐dimensional LC/MS/MS methodology to identify known uremic analytes in a clinical hemodialysate sample. Good inter‐ and intra‐day reproducibility of both chromatographic stages with a high degree of mass accuracy and precision was achieved with the multi‐dimensional liquid chromatography/tandem mass spectrometry (LC/MS/MS) system. Fragmentation maps were generated most successfully using collision‐induced dissociation (CID) as, unlike high‐energy CID (HCD), ions formed by this technique could be fragmented further. Structural elucidation is more challenging for large analytes >270 Da and distinguishing between isomers where their initial fragmentation pattern is insufficiently different. For small molecules (<200 Da), where fragmentation data may be obtained without loss of signal intensity, complete structures can be proposed from just the accurate mass fragmentation data. This methodology has led to the discovery of a selection of known uremic analytes and two completely novel moieties with chemical structural assignments made. Copyright © 2009 John Wiley & Sons, Ltd. 相似文献
6.
A. Gareth Brenton A. Ruth Godfrey 《Journal of the American Society for Mass Spectrometry》2010,21(11):1821-1835
High-resolution mass spectrometry has become ever more accessible with improvements in instrumentation, such as modern FT-ICR
and Orbitrap mass spectrometers. This has resulted in an increase in the number of articles submitted for publication quoting
accurate mass data. There is a plethora of terms related to accurate mass analysis that are in current usage, many employed
incorrectly or inconsistently. This article is based on a set of notes prepared by the authors for research students and staff
in our laboratories as a guide to the correct terminology and basic statistical procedures to apply in relation to mass measurement,
particularly for accurate mass measurement. It elaborates on the editorial by Gross in 1994 regarding the use of accurate
masses for structure confirmation [1]. We have presented and defined the main terms in use with reference to the International
Union of Pure and Applied Chemistry (IUPAC) recommendations for nomenclature and symbolism for mass spectrometry. The correct
use of statistics and treatment of data is illustrated as a guide to new and existing mass spectrometry users with a series
of examples as well as statistical methods to compare different experimental methods and datasets. 相似文献
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10.
Bob Boyd Gareth Brenton Eddie Clayton Jonathan Curtis R. M. Elliott G. A. Errock B. N. Green R. H. Bateman Simon J. Gaskell Iwan Griffiths Zdenek Herman Philip Jonathan Rich Kondrat Mila Laušević Chris Lock Deepak Mathur John F. J. Todd Károly Vékey 《Rapid communications in mass spectrometry : RCM》2016,30(11):1253-1264