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Correction of the urinary testosterone to epitestosterone ratio measurement in antidoping analyses by chromatographic and mass spectrometric techniques
Drug Testing and Analysis ( IF 2.6 ) Pub Date : 2023-02-11 , DOI: 10.1002/dta.3456
Dayamín Martínez Brito 1, 2 , Teresa Correa Vidal 1 , Xavier de la Torre 2 , Rodny Montes de Oca Porto 1 , Francesco Botrè 2, 3
Affiliation  

The ratio of testosterone (T) to epitestosterone (E) determined in urine samples is the main biomarker used to prove T and precursors abused by athletes. Analytically, the correction of the ratio is required by the World Anti-Doping Agency. This work describes a series of experiments aimed to study when it is appropriate to correct the T/E ratio value, using different mass spectrometric techniques since only reports on GC-MS exist. Analyses using external calibrators, controls, and routine samples were performed by three different techniques GC-MS, GC-MSn, and LC-MSn. A statistical comparison of the T/E was performed after the application of two corrections previously published: Isotopic contribution peak area correction (corr_1) and use of a verified internal deuterated internal standard (TD3/ED3) correction (corr_2) and the ratio based on T and E concentrations. The use of external calibration samples introduces biases that influence not only the T and E concentrations but also the T/E ratio, even when both methods of correction are applied. The correction after applying corr_1 method barely contributed to the accuracy of the T/E calculation. Nevertheless, the application of the corr_2 method increased the accuracy between 5% and 6% when comparing theoretical and experimental T/E values. Finally, the best results were obtained by the ratio calculated directly from the estimated concentrations of T and E. Attention must be paid when the T/E is measured by LC-MSn since different acquisition modes produced significantly different results, even in MS/MS when the same transition is used for T and E.

中文翻译:


通过色谱和质谱技术校正反兴奋剂分析中尿睾酮与表睾酮比率测量值



尿液样本中测定的睾酮 (T) 与表睾酮 (E) 的比率是用于证明运动员滥用 T 和前体的主要生物标志物。分析认为,该比例的修正是世界反兴奋剂机构要求的。这项工作描述了一系列实验,旨在研究何时适合使用不同的质谱技术来校正 T/E 比值,因为仅存在有关 GC-MS 的报告。使用外部校准品、对照品和常规样品的分析通过三种不同的技术 GC-MS、GC-MS n和 LC-MS n进行。在应用先前发布的两种校正后,对 T/E 进行了统计比较:同位素贡献峰面积校正 ( corr_1 ) 和使用经过验证的内部氘代内标 (TD3/ED3) 校正 ( corr_2 ) 以及基于T 和 E 浓度。使用外部校准样品会引入偏差,不仅影响 T 和 E 浓度,而且影响 T/E 比,即使同时应用两种校正方法也是如此。应用corr_1方法后的修正对T/E计算的准确性几乎没有贡献。尽管如此,在比较理论和实验 T/E 值时, corr_2方法的应用将精度提高了 5% 到 6%。最后,通过直接根据 T 和 E 的估计浓度计算的比率获得了最佳结果。通过 LC- MS测量 T/E 时必须注意,因为不同的采集模式会产生显着不同的结果,即使在 MS/当 T 和 E 使用相同的转换时为 MS。
更新日期:2023-02-11
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