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  • Analytical Chemistry and Spectroscopy  (18)
  • 1
    ISSN: 1040-7685
    Keywords: microcolumn liquid chromatography ; liquid chromatography/mass spectrometry ; temperature programming ; optimization methods ; fatty acids ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A temperature-programmed microcolumn liquid chromatography/mass spectrometry (LC/MS) system has been developed as a practical alternative to conventional solvent-programmed LC/MS. Good reproducibility of solute retention was achieved in a specially modified oven that permitted linear temperature programming between 40 and 100°C at rates of 0.1 to 0.5°C min-1. Through theoretical modelling studies performed under isocratic and isothermal conditions, the optimum separation under temperature-programmed conditions was rapidly and accurately predicted. This method enabled the complete resolution of saturated and unsaturated fatty acids in a fish oil dietary supplement with identification from their characteristic fragmentation patterns under electron-impact MS conditions. The mass spectra from the LC/MS system correlated very well with those from a standard reference library to facilitate spectral searching methods.
    Additional Material: 11 Ill.
    Type of Medium: Electronic Resource
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  • 2
    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A quantitative assay for dexamethasone in human plasma is described as based on methodology employing electron capture negative ionization mass spectrometry (ECNI/MS). The unique feature of this assay is the sample preparation involving chemical oxidation which transforms dexamethasone to a highly electrophilic species while not significantly affecting the electrophilic character of the biochemical matrix, thereby permitting selective and sensitive detection of the analyte. Optimized chemical procedures and instrumental parameters are described for the detection of oxidized dexamethasone. Finally, the newly developed methodology, based on gas chromatography/mass spectrometry (GC/MS) with ECNI, is evaluated by comparison with a conventional GC/MS assay using electron impact of an 11,17,21-tris-trimethylsilyl ether 20-enol-trimethylsilyl ether derivative of dexamethasone and with a radioimmunoassay in the analysis of pooled samples of human plasma containing widely varying concentrations of the drug as obtained from patients at different stages of the dexamethasone suppression test.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
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  • 3
    Electronic Resource
    Electronic Resource
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 1 (1974), S. 156-157 
    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
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  • 4
    Electronic Resource
    Electronic Resource
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 4 (1977), S. ix 
    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
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  • 5
    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Fast atom bombardment collisionally activated dissociation tandem mass spectrometry (FAB CAD MS/MS) of a disulfide-containing peptide, [2-D-penicillamine, 5-D-penicillamine]-enkephalin ([Pen]-enkephalin), is described. Unlike those of most other disulfide-containing peptides investigated, CAD of the native, unreduced protonated molecule of [Pen]-enkephalin yields a relatively large number of fragment ions. Most of the peaks in the CAD spectrum represent fragmentations of the peptide backbone with ‘unsymmetric’ cleavage of the disulfide bond with charge retention on the N-terminus; the fragment ions generally do not contain a sulfur atom or a disulfide group. The CAD spectrum of the N-terminal ethyl-triphenylphosphonium derivative, on the other hand, shows few fragment ions and is dominated by the single peak at m/z 523. This dominant ion also results from ‘unsymmetric’ cleavage and corresponds to the analogous protonated species (m/z 235) in the spectrum of the underivatized peptide. The chemical method of charge localization by triphenylphosphonium derivative formation at one end of the peptide is shown to be useful for investigating fragmentation mechanisms in FAB CAD MS/MS. Comparison of the CAD spectra of derivatized and underivatized [Pen]-enkephalin suggests that charge-remote fragmentation plays a significant role in the high-energy dissociation of this disulfide-bonded peptide.
    Additional Material: 4 Ill.
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  • 6
    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Vapor phase methodology for quantitative analysis of urine for metanephrine and normetanephrine as the pentafluoropropionyl derivative is described. The use of selected ion monitoring provided sufficient sensitivity and selectivity that milliliter aliquots of urine required only a simple scheme of sample processing; preliminary purification consisted of percolation through a column of XAD-2 followed by solvent extraction. The sample extracts were converted to the pentafluoropropionyl derivatives and analyzed by gas chromatography mass spectrometry with selected ion monitoring. Quantitative analysis was based on α[2H2]-β-[2H1]metanephrine and α-[2H2]-β-[2H1]normetane phrine which were added to the urine sample at the outset. The calibration plots for metanephrine and normetanephrine were linear from 10 ng ml-1 to 2000 ng ml-1 of urine permitting the detection of metanephrine and normetanephrine levels throughout the normal range and well into the subnormal range. Examples of application of the methodology to clinical investigation are described. The overall reproducibility of the sample processing methodology and instrumentation was assessed by replicate analyses of the same urine sample over a period of several weeks; the coefficient of variation was ±2.5% (n = 8).
    Additional Material: 5 Ill.
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  • 7
    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Fast atom bombardment (FAB) is useful for the characterization of all major metabolites of the analgesic acetaminophen (APAP). It is particularly useful for providing mass spectra of the polar glucuronide and sulfate conjugates which eluded identification by field desorption and other more conventional methods of ionization. A protocol is described for the use of FAB in the identification of urinary APAP metabolites isolated by reversed phase high-performance liquid chromatography (HPLC) following therapeutic dosages of the drug. A tentative set of recommendations for the off-line use of HPLC and FAB is directed towards solving problems encountered when using these two analytical techniques in concert. In addition, a method for calculating the signal to background ratio (S/B) for analyte peaks in FAB spectra from selected relative ion intensities is proposed. Examples are presented that show the potential of S/B as an empirical parameter for judging the quality of FAB spectra.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
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  • 8
    Electronic Resource
    Electronic Resource
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 7 (1973), S. 1227-1234 
    ISSN: 0030-493X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The mass spectra of N-propyl and N-butyl barbitals show the loss of olefin radical (CnH2n-1) in analogy to structurally similar molecules such as N-alkyl succinimides and 3-alkyl uracils. Trimethylsilylation of the N-substituted barbitals suppresses this fragmentation and loss of olefin via apparent McLafferty rearrangement from the even-electron ion, [M - 15]+, becomes significant. The trimethylsilyl derivatives of N-allyl barbital and N-phenyl barbital show an unusually facile elimination of the appropriate isocyanate from the molecular ion.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
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  • 9
    ISSN: 0030-493X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The isomeric prostaglandins, A and B, can be readily distinguished by differences in the mass spectra of their derivatives. The mass spectra of the PGA1- or PGA2-methyl ester (ME)-trimethyl silyl (TMS) ether derivatives have a prominent ion at [M - 71]+ or [M - C5H11]+ while those of the PGB1- or PGB2-ME-TMS derivatives have a predominant ion at [M - 99]+ or [M - C6H11O]+ in addition to that at [M - 71]+. Ions of similar origin characterize the spectra of the PGA1- or PGA2-TMS ether-TMS ester and PGB1- or PGB1-TMS-TMS derivatives, respectively. The fragmentation of other derivatives of PGA1, PGA2, PGB1 and PGB2 such as the ME-t-Bu-DMS (t-butyl-dimethylsilyl ether); ME-MO (methoxime)-TMS; ME-MO-Ac (acetate), and ME-Ac are also described comparatively. The composition of important ions was confirmed by deuterium labeling and/or high resolution mass spectroscopy, where appropriate. The potential advantages and limitations of the derivatives for quantitative analysis of prostaglandins by the specialized technique of multiple ion detection (MID) are described.
    Additional Material: 5 Ill.
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  • 10
    Electronic Resource
    Electronic Resource
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1983), S. 457-461 
    ISSN: 0030-493X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The dicyanomethylene derivative of a benzophenone analog significantly alters the fragmentation pattern observed during electron impact ionization of the underivatized parent compound. A double bond connecting the dicyanomethylene moiety to the parent compound is cleaved during a major fragmentation pathway for many of these compounds. A mechanism involving rearrangement of two hydrogen atoms is proposed to rationalize cleavage of this double bond. Conventional mass spectra as well as collisionally activated dissociation mass spectra of selected ions of several model compounds are reported and described in support of a proposed fragmentation mechanism.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
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