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  • Analytical Chemistry and Spectroscopy  (46)
  • SPACE SCIENCES
  • 1990-1994
  • 1975-1979  (46)
  • 1970-1974
  • 1976  (46)
  • 1
    Electronic Resource
    Electronic Resource
    Chichester : Wiley-Blackwell
    Organic Magnetic Resonance 8 (1976), S. 354-356 
    ISSN: 0030-4921
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: 77Se n.m.r. spectra of twenty-six organoselenium compounds, including some with an endocyclic selenium atom, have been recorded. Our measurements complete the scale of chemical shifts previously established by McFarlane. It seems difficult to define a range of chemical shifts which is characteristic of the valency state of selenium or of its endo- or exocyclic position. Some results are discussed qualitatively. In the case of selenolo[2,3-b]thiophene, evidence has been obtained for a 4J[Se, H] coupling across the sulphur atom.
    Notes: La résonance magnétique du 77Se a été observée dans vingt-six composés organiques dont certains contiennent un atome de sélénium endocyclique. Nous avons pu ainsi compléter l'échelle de déplacements chimiques établie par McFarlane. II apparaît difficile de définir une gamme de déplacement chimique du 77Se caractéristique de son état de valence ou de sa position endo- ou exocyclique. Certains résultats sont discutés qualitativement. Dans le cas du sélénolo [2,3-b]thiophène, des arguments en faveur d'un couplage 4J(Se, H) à travers l'atome de soufre ont été découverts.
    Additional Material: 4 Tab.
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  • 2
    Electronic Resource
    Electronic Resource
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 3 (1976), S. 28-31 
    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A general derivatization method has been developed for both primary and secondary aminoalkylphosphonic acids. Derivatization is effected by reaction with trifluoroacetic acid and trifluoroacetic acid anhydride followed by esterification using ethereal diazo-n-butane. This method can be used for microgram quantities and permits ready characterization by both gas chromatography and gas chromatography mass spectrometry. The structure of this derivative has been verified by mass spectrometry and proton magnetic resonance. Fragmentation patterns were confirmed by high resolution mass spectrometry, isotope labeling and the formation of derivative analogs.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
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  • 3
    Electronic Resource
    Electronic Resource
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 3 (1976), S. 272-277 
    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Using electron impact and field desorption mass spectrometry, structures are proposed for narasin and a related ionophore, A28086B, derived from fermentation. The ionic fragmentation of these compounds and their derivatives is discussed and compared with that of salinomycin, whose structure has been determined by X-ray diffraction.
    Additional Material: 6 Ill.
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  • 4
    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Two methods are described for the determination of salbutamol in human plasma. The drug is extracted from the plasma as a salbutamol tetraphenylboron ion pair and determined by gas chromatography mass spectrometry. Trideuterio-salbutamol is used as an internal standard. In the first method an extensive purification procedure is used to separate salbutamol from plasma cholesterol which interferes in the assay. Salbutamol is then determined as its TMS-ether using a multiple ion recording technique to measure the intensity of the fragment ion m/e 369 and the ion m/e 372 from the TMS ether of trideuterio-salbutamol. The second method is based on the ion pair extraction of salbutamol into heptan-3-one and its determination by gas chromatography mass spectrometry as the t-butyldimethylsilyl ether. The base peak in the mass spectrum of the t-butyldimethylsilyl-salbutamol is ion of m/e 495, which is of sufficiently high mass to distinguish it from any of the ions which arise from t butyldimethylsilyl-cholesterol. Six replicate analyses of plasma samples containing 1 ng salbutamol ml-1 were carried out using both methods. When the first method was used the mean value obtained was 1.3 ng ml-1 and the coefficient of variation was 17.7%. When the second method was used the mean value obtained was 0.95 ng ml-1 and the coefficient of variation was 10%. The second method is more rapid and therefore preferable for use in clinical pharmacological studies. This method has been used to determine the plasma salbutamol concentrations at varying times after either a 4mg oral or a 200 μg intravenous dose of salbutamol to man.
    Additional Material: 5 Ill.
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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: A low resolution, high sensitivity study has been made of the field desorption mass spectrum of glucagon, a 29 amino acid residue underivatized peptide. The highest molecular weight fragments observed, when spectra were taken under conditions which minimized surface reactions of the peptide on the emitter, were found to contain no more than 18 amino acid residues. The most probable fragmentation processes for ions larger than m/e 600 were the production of fragments containing 10, 11 or 12 amino acid residues.
    Additional Material: 1 Ill.
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  • 6
    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Excellent resolution and subsequent identification of free organic acids extracted from mixed, unstimulated human saliva was obtained by gas chromatography using high resolution open tubular glass capillary columns coupled with mass spectrometry computer instrumentation. In addition to the organic acids, identified as their trimethylsilyl derivatives, the presence of 2,6-di-t-butylcresol - a food preservative - and cholesterol was established by mass spectrometry. The effects of aspirin ingestion as well as diurnal variation were studied to demonstrate the possible clinical significance of this noninvasive approach to metabolic profiling.
    Additional Material: 2 Ill.
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  • 7
    Electronic Resource
    Electronic Resource
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 3 (1976), S. 191-195 
    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The terminal amino group of amino acids and peptides is blocked as the N-succinyl derivative by reaction with succinic anhydride. The product is then converted to the N,O-permethyl derivative in order to increase its volatility for use in mass spectrometry. The permethylated N-succinyl derivative retains the advantages of the permethylated N-acetyl derivative in regard to ease of preparation on a small scale, volatility and the presence of characteristic fragmentation patterns in their mass spectra. However, peaks in the high mass region are more abundant due to loss of CH3O· from the N-succinyl carbomethoxyl group as well as from the C-terminal carbomethoxyl group. Ions characteristic of the sequence and of individual amino acids are observed, and molecular weight can be determined from the relatively abundant ion at [M — CH3O]+ and from the weak molecular ion.
    Additional Material: 4 Ill.
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  • 8
    Electronic Resource
    Electronic Resource
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 3 (1976), S. 217-225 
    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Through the combined use of stable isotope labeling and gas chromatographic mass spectrometric analysis, the metabolic patterns for propoxyphene have been determined in laboratory animals and man. The rat and dog eliminated propoxyphene and its metabolites principally via the bile, while the rabbit more closely resembled man in excreting the metabolic products into urine. Metabolites in rat and rabbit existed as conjugates, whereas in dog and man the metabolites were excreted as a mixture of the free and unconjugated forms. The primary route of metabolism in all species studied was N-demethylation. However, the rat and rabbit extensively hydroxylated propoxyphene and its metabolltes prior to elimination. Metabolites arising from ester hydrolysis were found in rat and man. N-acetylated products were identified in all four species. A metabolite formed from cyclization and dehydration of dinorpropoxyphene was isolated in urine and was further identified as a circulating metabolite in dog plasma.
    Additional Material: 5 Ill.
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  • 9
    Electronic Resource
    Electronic Resource
    New York, NY [u.a.] : Wiley-Blackwell
    X-Ray Spectrometry 5 (1976), S. 29-30 
    ISSN: 0049-8246
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: Eleven international standards [U.S.G.S. Standards. G-2, GSP-1, AGV-1 and BCR-1; C.R.P.G. standards: GA, GH, BR and Mica-Fe; A.N.R.T. standard: DR-N; G.S.J. standards: JG-1 and JB-1] have been analysed by X-ray fluorescence for niobium and yttrium. Coefficients for full matrix effect correction are reported.
    Additional Material: 3 Tab.
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  • 10
    Electronic Resource
    Electronic Resource
    New York, NY [u.a.] : Wiley-Blackwell
    X-Ray Spectrometry 5 (1976), S. 36-40 
    ISSN: 0049-8246
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: Depth distributions of X-ray production by electrons in the energy range of six to fifteen key have been measured for Si and Cu characteristic X-rays in matrices of Al, Ni, Ag and Au. Corrections from these curves show that the modified Philibert absorption correction predicts the wrong dependence on matrix atomic number at these low electron energies, while the Duncomb and Reed atomic number correction shows too strong a dependence on atomic number. The curves should be valuable for comparison with both theoretical and empirical models for quantitative analysis at low energies.
    Additional Material: 4 Ill.
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