Analysis of corticosteroids in hair by Liquid chromatography-electrospray ionization mass spectrometry

被引:76
作者
Bévalot, F
Gaillard, Y
Lhermitte, MA
Pépin, G
机构
[1] Lab Expertises TOXLAB, F-75018 Paris, France
[2] Hop Calmette, Biochim Lab, F-59045 Lille, France
来源
JOURNAL OF CHROMATOGRAPHY B | 2000年 / 740卷 / 02期
关键词
corticosteroids; doping control; hair analysis;
D O I
10.1016/S0378-4347(00)00085-2
中图分类号
Q5 [生物化学];
学科分类号
071010 ; 081704 ;
摘要
The present study describes a confirmatory method for the quantitative determination in hair of the most common corticosteroids illegaly used as doping agents by athletes. Corticosteroids are extracted from 50 mg of powdered hairs by methanolic extraction follows by a solid-phase extraction on C-18 cartridge. After extraction, the dried residue is reconstituted with 50 mu l acetonitrile and injected in a liquid chromatograph. Liquid chromatography separation is performed on a reversed-phase C-18 column with a binary gradient of formiate buffer pH 3-acetonitrile as mobile phase. Detection is performed with an electrospray ionization mass spectrometer in negative ion and selected-ion monitoring mode. The limits of sensitivity achieved is 0.1 ng/mg in hair. Application to hair sample collected during an antidoping control and comparison to results obtain on urines, collected on the same athletes at the same time, shows the interest and the complementarity of both matrices. Hair analysis could allow the detection of corticosteroids on a large period preceding the control, and the detection of natural corticosteroids administered as pro-drug, like hydrocortisone acetate. (C) 2000 Elsevier Science B.V. All rights reserved.
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页码:227 / 236
页数:10
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