title: The determination of delta-5-androstenediol and its sulphate in serum and urine by gas chromatography-mass spectrometry.
abstract: OBJECTIVE
  We developed an assay for delta-5-androstenediol (adiol) and delta-5-androstenediol-3-sulphate (adiol-3S) in serum and adiol and total adiol sulphate (adiol-S) in urine.
  
  
  METHODS
  An analytical procedure using HPLC and gas chromatography-mass spectrometry was devised and tested for its reliability.
  
  
  METHODS
  After addition of deuterated androstenediol as internal standard, serum and urine samples were extracted. Steroid sulphates were hydrolysed. The extracts and hydrolysates were purified on HPLC, adiol was derivatized using heptafluorobutyric anhydride and finally quantified by gas chromatography-mass spectrometry.
  
  
  RESULTS
  The assay is accurate and reproducible. The coefficient of variation (CV) for the determination of adiol in serum samples is 4% (intra-assay) and 9% (interassay) and for urine samples 3 and 8% respectively. The intra-assay CV for the adiol-3S analyses is 5% for serum and 2% for urine samples while the interassay CV values for adiol-3S are 10% for serum and 7% for urine samples. The recovery of adiol and adiol-3S from serum and urine samples is 97%.
  
  
  CONCLUSIONS
  The developed assay meets the analytical demands needed for clinical applications.
authors.affiliation: Central Laboratory for Clinical Chemistry, University Hospital, Groningen, The Netherlands.
authors.forename: L D
authors.initials: LD
authors.lastname: Dikkeschei
authors.forename: B G
authors.initials: BG
authors.lastname: Wolthers
authors.forename: P H
authors.initials: PH
authors.lastname: Willemse
authors.forename: H
authors.initials: H
authors.lastname: van der Pol
authors.forename: A W
authors.initials: AW
authors.lastname: de Ruyter-Buitenhuis
authors.forename: G T
authors.initials: GT
authors.lastname: Nagel
mesh_terms: D015114:Androstenediol / Q000031:analogs & derivatives / Q000032:analysis* / Q000097:blood / Q000652:urine; D002138:Calibration; D002851:Chromatography, High Pressure Liquid / Q000379:methods; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods; D006801:Humans; D015203:Reproducibility of Results
chemical_list: C033537:5-androstene-3 beta,17 beta-diol sulfate; D015114:Androstenediol