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5918028 
Journal Article 
The determination of delta-5-androstenediol and its sulphate in serum and urine by gas chromatography-mass spectrometry 
Dikkeschei, LD; Wolthers, BG; Willemse, PH; van der Pol, H; de Ruyter-Buitenhuis, AW; Nagel, GT 
1993 
Yes 
Clinical Endocrinology
ISSN: 0300-0664
EISSN: 1365-2265 
39 
4 
469-474 
English 
8287574 
WOS:A1993MA08800013 
OBJECTIVES: 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.

DESIGN: An analytical procedure using HPLC and gas chromatography-mass spectrometry was devised and tested for its reliability.

MEASUREMENTS: 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.