Rapid screening of beta-adrenergic agents and related compounds in human urine for anti-doping purpose using capillary electrophoresis with dynamic coating.
This paper presents a capillary electrophoresis method, developed for the detection, in human urine, of beta-adrenergic agents and phenolalkylamines. The electrophoretic separation is achieved in less than 10 min and is based on the use of CEofix kit, for the dynamic capillary coating. The effects of accelerator buffer pH and separation voltage were investigated. The optimum buffer pH was found to be 2.5 for beta2-agonists and 6.2 for beta-blockers and phenoalkylamines with a separation voltage of 15 kV. Urine samples spiked with the compounds here studied were treated according to the standard procedure (SPE and evaporation to dryness) and analyzed by CE interfaced with an UV diode-array, set at 195 and 210 nm. The quantitative validation results, obtained analyzing samples at three different concentrations, show a good precision of peak areas that do not exceed 5% for intra-day assays and 10% for inter-day assays. Good linearity (r(2) > 0.995) was obtained within the 50-500 ng/mL concentration range. The qualitative validation data show a relative migration times (MTs) variation lower than 1%. The analytes were clearly distinguishable in urine, with LOD and LOQ in the range of 10-80 and 40-100 ng/mL, respectively.
Mazzarino
Monica
M
Laboratorio Antidoping, Federazione Medico Sportiva Italiana, Rome, Italy.
de la Torre
Xavier
X
Mazzei
Franco
F
Botrè
Francesco
F
D000318:Adrenergic beta-Agonists / Q000737:chemistry / Q000652:urine*; D000319:Adrenergic beta-Antagonists / Q000737:chemistry / Q000652:urine*; D000588:Amines / Q000737:chemistry; D004300:Doping in Sports; D019075:Electrophoresis, Capillary / Q000295:instrumentation / Q000379:methods; D006801:Humans; D015394:Molecular Structure; D010636:Phenols / Q000737:chemistry; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D015813:Substance Abuse Detection / Q000379:methods*
D000318:Adrenergic beta-Agonists; D000319:Adrenergic beta-Antagonists; D000588:Amines; D010636:Phenols