Improvement in steroid screening for doping control with special emphasis on stanozolol.
The Medical Commission of the International Olympic Committee forbids the use of anabolic androgenic steroids and beta2-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 degrees C followed by 40 degrees C min(-1) to 200 degrees C and then 15 degrees C min(-1) to 300 degrees C. Using 140 degrees 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 degrees 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.
Huenerbein
Andréas
A
LABDOP-LADETEC, Instituto de Química, Ilha do Fundão, Centro de Tecnologia, Bloco A. sala 512, Universidade Federal do Rio de Janeiro, Rio de Janeiro 21949-900, RJ, Brazil. andreashuenerbein@student.uni-halle.de
Sipoli Marques
Marlice A
MA
Pereira
Alberto dos Santos
Ados S
de Aquino Neto
Francisco Radler
FR
D045930:Anabolic Agents / Q000032:analysis*; D004300:Doping in Sports; D008401:Gas Chromatography-Mass Spectrometry / Q000592:standards; D013197:Stanozolol / Q000032:analysis*; D015813:Substance Abuse Detection / Q000379:methods / Q000592:standards*
D045930:Anabolic Agents; D013197:Stanozolol