Specificity and selectivity improvement in doping analysis using comprehensive two-dimensional gas chromatography coupled with time-of-flight mass spectrometry

Abstract

Recebido em 5/9/11; aceito em 21/11/11; publicado na web em 31/1/12Comprehensive two-dimensional gas chromatography coupled with time-of-flight mass spectrometry was used for the identification of forty doping agents. The improvement in the specificity was remarkable, allowing the resolution of analytes that could not be done by one-dimensional chromatographic systems. The sensitivity observed for different classes of prohibited substances was clearly below the value required by the World Anti-Doping Agency. In addition time-of-flight mass spectrometry gives full spectrum for all analytes without any interference from the matrix, resulting in selectivity improvements. These results could support the implementation of an exhaustive monitoring approach for hundreds of doping agents in a single injection.

Application of comprehensive 2D chromatography in the anti-doping field: Sample identification and quantification

“…Barbosa et al used a similarly complex heating program to successfully separate 40 doping agents (from different pharmacological classes) and their metabolites. [33] This included AAS and their metabolites (S1, including clenbuterol, designated an 'other anabolic agent'), β2-agonists (S3), aromatase inhibitors and selective estrogen receptor modulators (both S4, Hormone and Metabolic Modulators), diuretics & masking agents (S5), stimulants (S6), narcotics (S7) and cannabinoids (S8) plus a drug used for the enhancement of oxygen uptake, transport or delivery (prohibited methods category 'M1'). However, the authors purposefully worked at a concentration 10 times higher than the WADA MRPL (for steroids) as their intention for this article was to highlight the improvement in resolution and sensitivity rather than detection limits, which they suggested had been demonstrated in other papers.…”

“…Barbosa et al used this model to accelerate their initial optimisation. [33] GCxGC-MS for steroid analysis is not just confined to biological matrices. Other research reported includes wastewater [44,45] and coconut [46] / vegetable oils.…”