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The detection of 11 sympathomimetic alkylamines in urine was presented with a focus on human doping control is proposed using liquid chromatography tandem mass spectrometry (LC-QqQ) and high resolution mass spectrometry (LC-HRMS) as a screening tool after a dilute-and-shoot (DS) approach. For the LC-HRMS analyses, several compounds exhibited better limits of detection (L.O.D.) than the LC-QqQ. However, due to their small differences in structure, co-elution among the alkylamines was observed. Therefore, the chemical conversion of the alkylamines into an appropriate derivative for the confirmation analyses using gas chromatography-mass spectrometry (GC-MS) was evaluated. Five derivatization approaches were evaluated in an attempt to increase the analytical response and the confidence of the identification. The choice of the appropriated derivative for each alkylamine makes their spectra more easily interpretable, fulfills the WADA's rather strict identification criteria and enables the unequivocal identification of alkylamines in urine.

Luteinizing hormone (LH) can be used by athletes as an alternative way to take illicit advantage of androgenic effects, since it stimulates the secretion of testosterone by the Leydig cells. As consequence, LH use is illegal for male athletes and the hormone is included in the World Anti-Doping Agency (WADA) prohibited list. Since LH is an endogenous substance, the strategy used to allow the detection of LH abuse was the establishment of a reference value. All analyses were developed by IMMULITE ® , which was submitted to a complete validation performance with urine. The hormone showed to be stable at 4 °C and -20 °C for at least 40 days and for 10 days at room temperature and unstable after the second cycle of freezing and thawing. The reference population of male Brazilian athletes showed a cut-off value of 37.4 mIU mL-1. The results indicate the assay is suitable for application in doping control analysis. ]]>