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气相色谱/燃烧/同位素比率质谱法检测天然皮质类固醇的外源性摄入:在体育赛事中滥用情况的应用

Detection of exogenous intake of natural corticosteroids by gas chromatography/combustion/isotope ratio mass spectrometry: application to misuse in sport.

作者信息

Bourgogne E, Herrou V, Mathurin J C, Becchi M, de Ceaurriz J

机构信息

Laboratoire National de Dépistage du Dopage, 143 avenue R. Salengro, 92290 Chatenay Malabry, France.

出版信息

Rapid Commun Mass Spectrom. 2000;14(24):2343-7. doi: 10.1002/1097-0231(20001230)14:24<2343::AID-RCM171>3.0.CO;2-Z.

DOI:10.1002/1097-0231(20001230)14:24<2343::AID-RCM171>3.0.CO;2-Z
PMID:11114048
Abstract

A detailed procedure for the analysis of exogenous hydrocortisone and cortisone in urine by gas chromatography/combustion/isotope ratio mass spectrometry (GC/C/IRMS) is proposed. As urinary levels of hydrocortisone are rather low for GC/C/IRMS analysis, the focus is on the main corticosteroid metabolites, tetrahydrocortisone (THE) and tetrahydrocortisol (THF). Following different solid phase extraction purifications, THE and THF are oxidized to 5beta-androstanetrione before analysis by GC/C/IRMS. Significant differences in delta(13)C per thousand values of synthetic natural corticosteroids and endogenous human corticosteroids have been observed. Therefore, a positive criterion, to detect exogenous administration of synthetic corticosteroids in anti-doping control, is proposed.

摘要

提出了一种通过气相色谱/燃烧/同位素比值质谱法(GC/C/IRMS)分析尿液中外源性氢化可的松和可的松的详细程序。由于GC/C/IRMS分析的尿液中氢化可的松水平相当低,重点是主要的皮质类固醇代谢物,四氢可的松(THE)和四氢皮质醇(THF)。经过不同的固相萃取纯化后,THE和THF在通过GC/C/IRMS分析之前被氧化为5β-雄甾三酮。已观察到合成天然皮质类固醇和内源性人类皮质类固醇的千分比δ(13)C值存在显著差异。因此,提出了一种在反兴奋剂控制中检测合成皮质类固醇外源性给药的阳性标准。

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