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Micellar electrokinetic chromatography analysis of tetrahydrogestrinone and related anabolic androgenic steroids

机译:四氢孕酮和相关合成代谢雄激素类固醇的胶束电动色谱分析

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Tetrahydrogestrinone and related anabolic androgenic steroids (AASs) have been used extensively for performance enhancement (doping) in sports due to their ability to accelerate protein synthesis and improve physical performance (F.??C.??W. Wu, Clin. Chem., 1997, 43, 1289a€“1292). The separation of these AASs was performed by micellar electrokinetic chromatography (MEKC) using borate/borax buffer (200/50 mM, pH 8.6), with sodium cholate (40 mM) as a chiral additive. The analytes included two endogenous steroid hormones (testosterone and epitestosterone) and five synthetic anabolic steroids (methyltestosterone, nandrolone, gestrinone, dihydrogestrinone and tetrahydrogestrinone). Capillary electrophoresis parameters such as the concentration of additives, injection time, temperature, and applied voltage were investigated to improve the separation efficiency. A complete separation was achieved in less than 16 min under the optimized conditions. The RSDs of peak area and migration time were below 3.9% and 0.34%, respectively. The limit of detection (LOD) between 240 and 570 ng??mLa?’1 was obtained for each of the pure standards with a photodiode array (PDA) detector. Lower LODs could be reached when combining with preconcentration. After liquida€“liquid extraction, the recoveries of spiked urine samples were in the range from 88% to 99%.
机译:四氢孕酮和相关的合成代谢雄激素类固醇(AASs)由于其能够加速蛋白质合成和改善体能的能力而被广泛用于运动表现(兴奋剂)(F。?? C.??W。Wu,Clin。 ,1997,43,1289a-“ 1292)。通过使用硼酸盐/硼砂缓冲液(200/50 mM,pH 8.6)和胆酸钠(40 mM)作为手性添加剂的胶束电动色谱法(MEKC)进行这些AAS的分离。分析物包括两种内源性类固醇激素(睾丸激素和表睾酮)和五种合成代谢类固醇(甲基睾丸激素,nandrolone,孕酮,二氢孕酮和四氢孕酮)。研究了毛细管电泳参数,如添加剂浓度,进样时间,温度和施加电压,以提高分离效率。在最佳条件下,不到16分钟即可实现完全分离。峰面积和迁移时间的RSD分别低于3.9%和0.34%。使用光电二极管阵列(PDA)检测器获得的每个纯标准品的检测限(LOD)在240至570ngΔmLa?1之间。与预浓缩结合使用时,可以达到较低的LOD。液体提取后,加标尿液样品的回收率在88%至99%之间。

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