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Studies on steroids

Journal of Chromatography B: Biomedical Sciences and Applications, ISSN: 0378-4347, Vol: 574, Issue: 1, Page: 1-7
1992
  • 10
    Citations
  • 0
    Usage
  • 11
    Captures
  • 3
    Mentions
  • 0
    Social Media
Metric Options:   Counts1 Year3 Year

Metrics Details

  • Citations
    10
    • Citation Indexes
      10
  • Captures
    11
  • Mentions
    3
    • References
      3
      • Wikipedia
        3

Article Description

A method for the determination of 4- and 6-hydroxylated bile acids with a vicinal glycol moiety in human urine by gas chromatography—mass spectrometry with negative ion chemical ionization detection is described. The 4β-hydroxylated bile acids labelled with 18 O and 2 H were prepared as internal standards by the exchange reaction of the carbonyl group on the steroid nucleus with H 2 18 O, followed by metal deuteride reduction. Bile acids in urine were extracted with a Sep-Pak C 18 cartridge and, after solvolysis and hydrolysis of the conjugated forms, transformed into pentafluorobenzyl ester diethylhydrogensilyl ether diethylsilylene derivatives. Subsequent resolution into individual 4- and 6-hydroxylated bile acids was carried out on a cross-linked fused-silica capillary column; a characteristic carboxylate anion, [M − PFB] −, was used to monitor each bile acid in the negative ion mode. The newly developed method was applied to the separation and determination of 4- and 6-hydroxylated bile acids in a urine specimen from a newborn infant.

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