TY - JOUR
T1 - Comprehensive two-dimensional gas chromatography improves separation and identification of anabolic agents in doping control
AU - Mitrevski, Blagoj
AU - Wilairat, Prapin
AU - Marriott, Philip
PY - 2010
Y1 - 2010
N2 - The application of comprehensive two-dimensional gas chromatography coupled to time-of-flight mass spectrometry (GC x GC-TOFMS) for the analysis of six anabolic agents (AAs) in doping control is investigated in this work. A non-polar-polar column configuration with 0.2 mu m film thickness (d(f)) second dimension (D-2) column was employed, offering much better spread of the components on D-2 when compared to the alternative 0.1 mu m d(r) D-2 column. The proposed method was tested on the key AA that the World Anti-Doping Agency (WADA) had listed at the low ngmL(-1) levels (clenbuterol, 19-norandrosterone, epimethendiol, 17 alpha-methyl-5 alpha-androstane-3 alpha, 17 beta-diol, 17 alpha-methyl-5 beta-androstane-3 alpha, 17 beta-diol and 3 -OH-stanozolol). The compounds were spiked in a blank urine extract obtained by solid-phase extraction, hydrolysis and liquid-liquid extraction; prior to analysis they were converted to the corresponding trimethylsilyl (TMS) derivatives.
AB - The application of comprehensive two-dimensional gas chromatography coupled to time-of-flight mass spectrometry (GC x GC-TOFMS) for the analysis of six anabolic agents (AAs) in doping control is investigated in this work. A non-polar-polar column configuration with 0.2 mu m film thickness (d(f)) second dimension (D-2) column was employed, offering much better spread of the components on D-2 when compared to the alternative 0.1 mu m d(r) D-2 column. The proposed method was tested on the key AA that the World Anti-Doping Agency (WADA) had listed at the low ngmL(-1) levels (clenbuterol, 19-norandrosterone, epimethendiol, 17 alpha-methyl-5 alpha-androstane-3 alpha, 17 beta-diol, 17 alpha-methyl-5 beta-androstane-3 alpha, 17 beta-diol and 3 -OH-stanozolol). The compounds were spiked in a blank urine extract obtained by solid-phase extraction, hydrolysis and liquid-liquid extraction; prior to analysis they were converted to the corresponding trimethylsilyl (TMS) derivatives.
UR - http://www.sciencedirect.com/science/article/pii/S0021967309016057
U2 - 10.1016/j.chroma.2009.10.075
DO - 10.1016/j.chroma.2009.10.075
M3 - Article
VL - 1217
SP - 127
EP - 135
JO - Journal of Chromatography A
JF - Journal of Chromatography A
SN - 0021-9673
IS - 1
ER -