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  • Analytical Chemistry and Spectroscopy  (3)
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  • Analytical Chemistry and Spectroscopy  (3)
  • Chemistry  (3)
  • 1
    Electronic Resource
    Electronic Resource
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 8 (1981), S. 5-9 
    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Isotope dilution mass spectrometry is one of the best candidates for reference and definitive methods for the quantitative measurement of organic compounds. In this study sources of error were investigated. Where possible they were removed, and commercially available equipment had to be modified. The method was applied to the measurement of serum cholesterol. The precision is optimized and in the order of 0.5%. The mean of the recoveries of three measurements is 99.8%. The accuracy of the mean of three measurements is 0.2% if no interference are present in the gas chromatographic mass spectrometric measurements.
    Additional Material: 6 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 method has been described for the quantification of diethylstilboestrol (DES) in bovine urine. The determining step is based on isotope dilution mass spectrometry (IDMS). The chemical work-up consisted of enzymatic deconjugation, Sep-Pak® clean-up and high-performance liquid chromatography (HPLC). The labelled compound synthesized for IDMS is hexadeutero DES (DES-2H6). The labelled compound is not only used to quantify DES, but also to check the recovery of the chemical work-up procedure, in order to avoid false negative results. At the 1-5 μg I-1 level of urinary DES, the average recovery of 2 μg I-1 DES-2H6 is 70±20% (s.d.).
    Additional Material: 7 Ill.
    Type of Medium: Electronic Resource
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  • 3
    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A confirmation method which can be used in regulatory screening programs for diethylstilbestrol in the urine of cattle is presented. trans- Diethylstilbestrol is purified from urine by Sep-Pak extraction and high-performance liquid chromatography and converted into its trimethylsilyl derivative. Identification is based on both accurate mass measurement of the molecular ion of trans-diethylstilbestrol trimethylsilyl by gas chromatography high resolution mass spectrometry and determination of the [M + 1]+/[M]+ peak height ratio by selected ion monitoring in low resolution. Specificity is such that on the basis of mass spectrometric data alone, all molecular formulae except those of diethylstilbestrol trimethylsilyl and only one other compound can be excluded. Additional specificity is provided by chromatographic data. The quantification is based on the standard addition method. The average recovery of trans-diethylstilbestrol is 76% with a standard deviation of 18% (n = 23).
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
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