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  • Analytical Chemistry and Spectroscopy  (347)
  • 1975-1979  (347)
  • 1
    Electronic Resource
    Electronic Resource
    A simplified technique for collecting breath CO2 for isotope ratio mass spectrometry (1978)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 5 (1978), S. 29-31 
    Details
    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A simplified technique of collecting breath CO2 for isotopic analysis has been developed. The subject breathes into a 3 I bag from which a 50 ml aliquot is transferred to an evacuated, septum-capped tube (Vacutainer®). The sample is later withdrawn and the CO2 is cryogenically purified. No isotope fractionation is observed in samples collected in this manner. Samples have been stored up to three months without any change in the isotope ratio.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200050106
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  • 2
    Electronic Resource
    Electronic Resource
    Gas chromatography mass spectrometry studies on biologically important 8-aminoquinoline derivatives (1978)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 5 (1978), S. 76-79 
    Details
    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Several substituted 8-aminoquinolines related to known antimalarial drugs have been studied by gas chromatography mass spectrometry. 5,6-Dihydroxy-8-aminoquinoline, a possible metabolite of Primaquine, can be detected by single ion monitoring after conversion to a trimethylsilyl ether derivative. The mass spectra obtained in this study indicate that there are certain ions which are characteristic of the trimethylsilyl ethers of hydroxylated 8-aminoquinolines and 5,6-dimethoxy-8-aminoquinolines. These compounds should thus be amenable to analysis if they were produced during in vivo metabolism studies. Using selected ion monitoring the derivatized compounds can be detected at submicrogram levels.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200050114
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  • 3
    Electronic Resource
    Electronic Resource
    Mass spectrometric analyses and characterization of Kepone in environmental and human samples (1978)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 5 (1978), S. 232-237 
    Details
    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A specific portion of our environment has been contaminated with Kepone, or chlordecone. Additionally, some specific human exposures to high concentrations of Kepone have been confirmed. Gas chromatography mass spectrometry involving chemical ionization and high resolution mass spectrometry were used to detect, identify and confirm the presence of Kepone, Kepone photoproducts and a reduction product of Kepone in environmental and human samples. Field desorption, field ionization and electron impact mass spectrometric methods, as well as infrared and nuclear magnetic resonance techniques were used to characterize and identify Kepone hydrate and hemiketal in benzene and methanol solutions, respectively.
    Additional Material: 8 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200050312
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  • 4
    Electronic Resource
    Electronic Resource
    A selected ion monitoring assay for primaquine in plasma and urine (1979)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 6 (1979), S. 109-112 
    Details
    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The antimalarial drug primaquine was analysed in plasma and urine by gas chromatography mass spectrometry, using a deuterated internal standard. After freeze-drying and extraction with trichloroethylene the sample plus internal standard was reacted with Tri Sil TBT (a) 3:3:2 by volume mixture of trimethylsilylimidazole, N,O,-bis-(trimethylsilylacetamide and trimethylchlorosilane) and an aliquot injected into the gas chromatograph mass spectrometer. The gas chromatographic effluent was monitored at m/z 403 and m/z 406, the molecular ions of the bis-TMS ethers of primaquine and 6-trideuteromethoxy primaquine. Calibration curves were prepared from standards made up in plasma and urine. Data from the analysis of plasma and urine samples from a volunteer who ingested the equivalent of 45 mg primaquine are presented.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200060306
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  • 5
    Electronic Resource
    Electronic Resource
    Plasma quantitation of warfarin and warfarin alcohol by gas chromatography chemical ionization mass spectrometry in patients on warfarin maintenance therapy (1979)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 6 (1979), S. 208-211 
    Details
    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A quantitative method has been developed to measure plasma concentrations of warfarin and warfarin alcohol. The analytical procedure uses deuterated analogues as internal standards, and the technique of selected ion monitoring following gas chromatography methane chemical ionization mass spectrometry of the 4′-methyl ethers of warfarin and warfarin alcohol. Concentrations of warfarin and warfarin alcohol have been measured in plasma samples from 43 patients maintained on chronic warfarin therapy and compared with the ‘apparent warfarin’ concentration as measured by a fluorometric procedure. The study demonstrated a high degree of correlation between the gas chromatographic mass spectrometric derived sum of the individual concentrations of warfarin and warfarin alcohol, and the ‘apparent warfarin’ concentration determined from a spectrofluorometric assay.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200060508
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  • 6
    Electronic Resource
    Electronic Resource
    A microprocessor controlled mass spectrometer for the fully automated purification and isotopic analysis of breath carbon dioxideThis work was supported by the National Institutes of Health through grant AM 18741 and the US Department of Energy. The work was performed at both the University of Chicago and Argonne National Laboratory. This paper was presented in part at the Third International Conference on Stable Isotopes, Oak Brook, Illinois, USA (1978) and has appeared in abstract form in the conference proceedings. (1979)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 6 (1979), S. 350-355 
    Details
    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Breath tests that measure the oxidative utilization of 13C labeled substrates have been shown to be clinically useful, but have failed to gain wide acceptance because of the slow and costly isotopic analysis of the breath samples. Therefore we have developed a fully automated, microprocessor controlled CO2 purification and isotopic analysis system. The breath CO2 is cryogenically purified by passage through cold traps of -94°C and -196°C to condense water and CO2, respectively. The CO2 is introduced into a dual inlet, peak-stepping mass spectrometer and analyzed for isotopic content by comparison with a known standard. Thirty samples can be analyzed without operator intervention. Analysis time averages 14 minutes per sample, and the analysis has a precision of 0.3‰ which corresponds to 3 parts excess 13C per 106 parts CO2. The speed of analysis is comparable with scintillation counting and permits next day reporting of clinical breath test results. The precision is sufficient for clinical applications as it is less than the 0.7‰ isotopic variation in basal breath CO2.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200060809
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  • 7
    Electronic Resource
    Electronic Resource
    Quantitation of plasma warfarin levels by gas chromatography chemical ionization mass spectrometry (1979)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 6 (1979), S. 101-104 
    Details
    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A quantitative assay for plasma concentrations of warfarin has been developed using a deuterated warfarin analogue as internal standard. The method employs methylation (diazomethane) of warfarin to its 4′-methoxy derivative and gas chromatography chemical ionization mass spectrometry. Selected ion monitoring was used to relate the response of warfarin methyl ether and the internal standard. This technique can measure warfarin plasma concentrations five days after a single oral (25 mg) dose. Warfarin half-lives were determined in 12 healthy male volunteers. Each plasma analysis required six minutes of instrument time.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200060304
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  • 8
    Electronic Resource
    Electronic Resource
    NMR studies of sulphur heterocycles: III - 13C spectra of benzo[b]thiophene and the methylbenzo[b]thiophenes (1976)
    Chichester : Wiley-Blackwell
    Organic Magnetic Resonance 8 (1976), S. 252-257 
    Details
    ISSN: 0030-4921
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: All carbon resonances in the title compounds have been unequivocably assigned. Steric effects in the peri substituted compounds have been compared with analogous effects in naphthalene and benzo[b]furan. The observed effects are not explained by current theory. Unusual deshielding steric shifts are observed at some carbons. Methyl substituent effects are not additive at any position in the sterically crowded 2,3-disubstituted compounds.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/mrc.1270080507
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  • 9
    Electronic Resource
    Electronic Resource
    Spectres RMN des Polysaccharides et de leurs Dérivés: Influence des Substituants sur le Déplacement Chimique 13C (1978)
    Chichester : Wiley-Blackwell
    Organic Magnetic Resonance 11 (1978), S. 344-349 
    Details
    ISSN: 0030-4921
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Methyl and acetyl substituent effects on 13C chemical shift have been determined on (α 1→3), (α 1→4), (β 1→3) and (β 1→4) linked polysaccharides such as pseudo-nigerane, β-cyclodextrine, amylose, laminarane and cellulose. Methyl α- and β-D-glucopyranoside have been used as monomer model compounds. Shift determination of hydroxylated and substituted polysaccharides requires unambiguous assignment of their 13C spectra. Selective heteronuclear spin decoupling and the isotope effect of deuterated hydroxyl have been used as assignment techniques.
    Notes: L'influence des substituants méthyle et acétate sur le déplacement chimique 13C a été déterminée sur les polysaccharides liés par liaison glycosidique (α1→3), (α1→4), (β1→3) et (β1→4) suivants: pseudonigérane, β-cyclodextrine, amylose, laminarane et cellulose. Nous avons utilisé les méthyl α et β glucopyranosides comme composés modès. La détermination de l'effet des substituants sur le déplacement chimique 13C nécessite l'attribution non ambiguë des spectres 13C des polysaccharides hydroxylés et substitués. On a utilisé pour cela la technique d'irradiation sélective hétéronucléaire et l'effet isotopique d'hydroxyle deutérié.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/mrc.1270110706
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  • 10
    Electronic Resource
    Electronic Resource
    Carbon-13 NMR investigation of 2,5-diaryl-1,4-dithiins (1979)
    Chichester : Wiley-Blackwell
    Organic Magnetic Resonance 12 (1979), S. 691-695 
    Details
    ISSN: 0030-4921
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The 13C NMR spectra of eight 2,5-diaryl-1,4-dithiins were recorded and signals were assigned. A linear correlation was observed between the electronegativity of the substituent groups on C-10,10′ and the chemical shifts of C-10,10′ after applying corrections for the magnetic anisotropic effect of the substituents. A Hammett correlation was found between the 13C chemical shifts of C-3,6 and C-7,7′ and the σp+ parameter associated with the substituents on C-10,10′. Extended electronic interaction between the π system of the aryl group and the π system of the dithiin ring was suggested by the observance of an alternating behavior in the magnitude of the substituent effects on the 13C shifts of C-2,5 and C-3,6. An alternating effect was also noted in the magnitude of the long-range 13C—F coupling constants for these same carbon signals in 2,5-(10,10′-difluoro)diphenyl-1,4-dithiin.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/mrc.1270121209
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