Analysis of corticosteroids in hair by Liquid chromatography-electrospray ionization mass spectrometry
Analysis of corticosteroids in hair by Liquid chromatography-electrospray ionization mass spectrometry
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DOI：
10.1016/s0378-4347(00)00085-2
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发表时间：
2000-04-14
期刊：
影响因子：
--
通讯作者：
Pépin, G
中科院分区：
文献类型：
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作者：
Bévalot, F;Gaillard, Y;Pépin, G
本研究描述了一种定量测定头发中最常见的皮质类固醇兴奋剂的运动员非法使用的验证方法。通过甲醇提取，然后在C-18柱上进行固相提取，从50毫克粉状头发中提取皮质类固醇。提取后，用50 μ l乙腈复溶干燥的残留物，并进样至液相色谱仪中。在反相C-18柱上进行液相色谱分离，以pH 3的甲酸盐缓冲液-乙腈二元梯度作为移动的流动相。采用电喷雾电离质谱仪在负离子和选择离子监测模式下进行检测。在头发中达到的灵敏度限度为0.1纳克/毫克。在反兴奋剂控制期间收集的头发样本的应用程序和尿液，收集在同一时间，在同一运动员获得的结果进行比较，显示了两个矩阵的兴趣和互补性。毛发分析可以允许在对照之前的一个大时期检测皮质类固醇，以及检测作为前药施用的天然皮质类固醇，如醋酸氢化可的松。(C)2000 Elsevier Science B. V.保留所有权利。
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.