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  • 1
    ISSN: 1040-7685
    Keywords: supercrirical fluid chromatography ; mass spectrometry ; capillary column ; inositol ; phosphate ; phytic acid ; silyl derivatives ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Capillary supercritical fluid chromatography with flame ionization detection appears promising for the separation and detection of silylated inositol phosphates. Inositol triphosphate and phytic acid, following ion exchange to their fully protonated forms, were silylated in one step with the addition of 9 and 12 trimethylsilyl groups, respectively. The resulting derivatives are well behaved in open-tubular chromatography columns with methyl-silicone stationary phase when CO2 is used as the mobile phase. Both flow-splitting and directinjection methods were evaluated. The identities of the derivatives were confirmed by supercritical fluid chromatography-mass spectrometry using chemical ionization with both ammonia and isobutane, and using electron ionization - CO2 charge exchange.
    Additional Material: 9 Ill.
    Type of Medium: Electronic Resource
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  • 2
    Electronic Resource
    Electronic Resource
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 10 (1983), S. 155-161 
    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A computer system (MSSMET), using methylene unit retention indices for an off-line reverse library search analysis of selected ion chromatograms from gas-liquid chromatographic mass spectrometric data, has been applied for the qualitative and quantitative determination of daily variations in the excreted levels of urinary steroids of two individuals, using capillary column gas-liquid chromatography. Aliquots of 24 h urine collections and morning spot urine samples were examined. The daily excretion pattern of most of the major steroid metabolites was fairly consistent from day to day (i.e. 3α-hydroxy-5α-androstane-17-one, androsterone; 3α-hydroxy-5β-androstane-17-one, etiocheolanolone; 3α, 17α,21-trihydroxy-5β-pregnane-11,20-dione, THE; 3α,11β,17α,21-tetrahydroxy-5β-pregnane-20-one, THF; 3α,11β,17α,21-tetrahydroxy-5α-pregnane-20-one; allo-THF; 3α,17α,20α,21-tetrahydroxy-5β-pregnane-11-one, cortolone; 3α,17α,20β,21-tetrahydroxy-5β-pregnane-11-one, β-cortolone; 5β-pregnane-3α,11β,17α,20α,21-pentol, cortol; 5β-pregnane-3α,11β,17α,20β,21-pentol,β-cortol), while certain other steroid metabolites had a less consistent excretion pattern (3β-hydroxy-5-androstene-17-one, for example). Advantages and disadvantages of using capillary columns for the automated metabolic profile analysis of urinary steroids by reverse library search of selected mass chromatograms.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
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