Improvement in steroid screening for doping control with special emphasis on stanozolol.
Improvement in steroid screening for doping control with special emphasis on stanozolol.
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DOI：
10.1016/s0021-9673(02)01801-0
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发表时间：
2003-01
期刊：
影响因子：
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通讯作者：
Andréas Huenerbein;M. A. Sípoli Marques;A. Pereira;F. R. de Aquino Neto
中科院分区：
文献类型：
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作者：
Andréas Huenerbein;M. A. Sípoli Marques;A. Pereira;F. R. de Aquino Neto
国际奥委会医学委员会禁止使用合成代谢雄激素和β2-激动剂来提高运动成绩。在这项工作中，我们选择了合成代谢类雄激素及其代谢物的例子来评估一些三甲基硅基衍生物的GC-MS分析。目的是设置最佳的GC条件，以提高在整个分析物洗脱温度范围内的检测。将初始柱温改为105C或140C，然后是40Cmin−1到200°C，然后是15Cmin−1到300°C。使用140C作为初始烘箱温度，可以获得较窄的初始分析物分布，在不损失衍生代谢物信号的情况下，对于在色谱图开始时洗脱的化合物，如克伦特罗、马布特罗、环氧亚甲基二醇和去甲雄酮。随后，洗脱分析物，如司坦唑醇代谢物、呋喃唑醇和氧雄酮不受影响。温度低于140°C，导致一些分析物(主要是司坦唑醇相关结构)的部分衍生化。因此，对衍生化条件的评价分为三个步骤，即小瓶、汽化室和毛细管柱，对其进行了彻底的评估。新的程序温度提高了一些化合物的信噪比，并对内源化合物显示了足够的分辨率。还利用所提出的方法获得了执行兴奋剂控制所需的一些困难的关键分离。
The Medical Commission of the International Olympic Committee forbids the use of anabolic androgenic steroids and β2-agonists to improve athletic performance. In this work we have selected examples of anabolic androgenic compounds and their metabolites to evaluate the GC–MS analysis of some trimethylsilyl derivatives. The aim is to set the best GC conditions to improve the detection within the whole range of analyte elution temperatures. The initial column temperature was changed to 105 or 140°C followed by 40°Cmin−1to 200°C and then 15°Cmin−1to 300°C. Using 140°C as the initial oven temperature it was possible to obtain narrower initial analyte distributions for the compounds that elutes at the beginning of the chromatogram as clenbuterol, mabuterol, epimethylenediol and norandrosterone, without loss of derivatized metabolites signal. Later, eluting analytes, such as the stanozolol metabolites, furazabol and oxandrolone were not affected. Temperatures below 140°C, resulted in partial derivatization for some analytes mainly stanozolol related structures. Therefore evaluation of derivatization conditions as occurring in three steps, the vial, vaporization chamber and capillary column, was thoroughly assessed. The new program temperature improves the signal-to-noise ratio for some compounds and shows adequate resolution for endogenous compounds. Some of the difficult key separations necessary for doping control enforcement were also obtained with the proposed method.