Several banned substances are illegally used by athletes in racemic mixtures for performance enhancement. These include clenbuterol, methyl hexaneamine, methamphetamines, and amphetamines. Clenbuterol is present in a large number of doping samples from Olympic and non-Olympic athletes that have adverse analytical findings (AAFs). In some cases, the presence of these substances could be the result of consumption of meat contaminated with clenbuterol. In other cases, the origin is not clear. In this study, 27 products with racemic clenbuterol were evaluated using a new analytical methodology for the resolution of R-(À) and S-(+)-enantiomers of clenbuterol by liquid chromatography-tandem mass spectrometry (LC-MS/MS) using a chiral column in 15 min with good separation. The method developed can also be used for the analysis of other biological matrices such as urine, serum, and meat. The resolution between two peaks' (R s ) value obtained using chromatographic data was 1.03. Both clenbuterol enantiomers were present in all products analyzed and the ratio was nearly 1. The origin of the product was not important for determining the presence of one or both enantiomers. All products displayed a 50:50 ratio of clenbuterol enantiomers. To the best of our knowledge, clenbuterol ratio determination of a large number of pharmaceutical preparations and black-market products has not been reported previously. The information shown could be used by national anti-doping organizations and the athletes with AAFs attributed to clenbuterol.
We developed and evaluated the properties of in‐house urine reference materials for the verification of laboratory refractometers, which are frequently used in clinical chemistry and doping testing laboratories. Urine was gathered from 26 healthy volunteers (16 male 30 ± 5 years old and 10 female 29 ± 4 years old), from which two urine batches were obtained: one with a low specific gravity (1.012± 0.003) and the other with a high specific gravity (1.027 ± 0.003). Homogeneity studies were conducted over 20 consecutive days. For short‐term stability studies, aliquots of both urine batches were stored at −20 ± 2°C; 3 ± 2°C; 20 ± 2°C; 45 ± 2°C for 0, 2, 7, 14 and 35 days, under both light and dark conditions. Similarly, another study was conducted to measure the long‐term stability of urine at −20 ± 2°C, over a 24‐month evaluation period. Our data showed that the urine was homogeneous and stable at −20 ± 2°C, 3 ± 2°C, 20 ± 2°C, and 45 ± 2°C under both light and dark conditions. In all cases, the urine was evaluated by specific gravity and no statistically significant differences (p ≤ 0.05) were recorded. Additionally, a proficiency test was conducted in collaboration with 15 ISO/IEC 17025 accredited laboratories, and z‐scores and performance factors were evaluated. These data indicate that this material could be used for the verification of refractometers.
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