A rapid screening assay for measuring urinary androsterone and etiocholanolone δ13C (‰) values by gas chromatography/combustion/isotope ratio mass spectrometry

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作者
Aguilera, Rodrigo [1 ,3 ]
Chapman, Thomas E. [1 ]
Catlin, Don H. [1 ,2 ]
机构
[1] UCLA Olympic Analytical Laboratory, Department of Molecular and Medical Pharmacology, University of California at Los Angeles, 2122 Granville Avenue, Los Angeles, CA 90025-6106, United States
[2] Department of Medicine, University of California at Los Angeles, 2122 Granville Avenue, Los Angeles, CA 90025-6106, United States
[3] UCLA Olympic Analytical Laboratory, 2122 Granville Avenue, Los Angeles, CA 90025-6106, United States
关键词
Body fluids - Gas chromatography - Mass spectrometry - Phase separation - Screening;
D O I
10.1002/1097-0231(20001215)14:233.0.CO;2-L
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摘要
A gas chromatography/combustion/isotope ratio mass spectrometry (GC/C/IRMS) method is described and validated for measurement of δ13C 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 δ13C values from -25‰ (baseline) to -31‰. Two weeks after testosterone administration was discontinued, the δ13C 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
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