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A rapid screening assay for measuring urinary androsterone and etiocholanolone δ 13 C (‰) values by gas chromatography/combustion/isotope ratio mass spectrometry
Author(s) -
Aguilera Rodrigo,
Chapman Thomas E.,
Catlin Don H.
Publication year - 2000
Publication title -
rapid communications in mass spectrometry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.528
H-Index - 136
eISSN - 1097-0231
pISSN - 0951-4198
DOI - 10.1002/1097-0231(20001215)14:23<2294::aid-rcm165>3.0.co;2-l
Subject(s) - chemistry , androsterone , chromatography , etiocholanolone , epitestosterone , urine , derivatization , gas chromatography , isotope ratio mass spectrometry , mass spectrometry , gas chromatography–mass spectrometry , androgen , biochemistry , steroid , hormone
A gas chromatography/combustion/isotope ratio mass spectrometry (GC/C/IRMS) method is described and validated for measurement of δ 13 C values of the acetate derivatives of urinary etiocholanolone and androsterone. The analysis was performed with only 2 mL of urine. The sample preparation consisted of deconjugation with β‐glucuronidase, solid phase extraction, and derivatization with acetic anhydride and pyridine. The within‐assay precision of two quality control (QC) urine samples ranged from 0.5 to 2.1 CV%. The between‐assay precision in the same QC urines ranged from 1.7 to 3.4 CV%. Administration of testosterone enanthate to a subject resulted in a 6‰ decrease in δ 13 C values from −25‰ (baseline) to −31‰. Two weeks after testosterone administration was discontinued, the δ 13 C values remained abnormally low while the urine testosterone/epitestosterone (T/E) ratio returned to less than 6. This relatively simple method is useful for rapidly screening a large number of urine samples, including those with T/E <6. Copyright © 2000 John Wiley & Sons, Ltd.