Optimization of the extraction and analysis of natural androgen steroids and their metabolites in urine by GC/MS and GC/FID - Archive ouverte HAL Accéder directement au contenu
Article Dans Une Revue Analytical Letters Année : 2012

Optimization of the extraction and analysis of natural androgen steroids and their metabolites in urine by GC/MS and GC/FID

Résumé

A multiresidue method was developed for screening, quantification, and confirmation of nine natural androgen steroids and their metabolites in urine. Steroids were first extracted from urine by solid phase extraction, enzymatically deglucuronated, re-extracted using a liquid/liquid extraction for purification, and finally acetylated for GC/MS and GC/FID analysis. Each step of sample preparation, as well as analysis, was optimized: solid phase extraction, liquid/liquid extraction, and derivatization reaction ... Therefore, a rugged sample preparation procedure was developed leading to extracts of sufficient purity (recoveries >66% and few matrix compounds). The whole methodology allowed reliable detection and quantification of the nine steroids at low concentration levels. Linearity and repeatability were established and were found to be satisfactory (R-2 > 0.996, RSD < 11%). Finally, the method was applied to quantify compounds of interest in real samples collected from healthy volunteers and patients treated with 4-androstenedione or dehydroepiandrosterone.
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Dates et versions

hal-00727420 , version 1 (03-09-2012)

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Estelle Pujos, Cécile Cren-Olivé, Patrick Goetinck, Marie-Magdeleine Flament-Waton, Marie-Florence Grenier-Loustalot. Optimization of the extraction and analysis of natural androgen steroids and their metabolites in urine by GC/MS and GC/FID. Analytical Letters, 2012, 45 (4), pp.356-366. ⟨10.1080/00032719.2011.644735⟩. ⟨hal-00727420⟩
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