Doping Control Laboratory of Athens, Institute of Biosciences and Applications, National Centre for Scientific Resarch "Demokritos", Maroussi, Greece.
Faculty of Biology, School of Science, National and Kapodistrian University of Athens, Athens, Greece.
Biomed Chromatogr. 2021 Aug;35(8):e5114. doi: 10.1002/bmc.5114. Epub 2021 Apr 11.
Salmeterol and fluticasone are included in the Prohibited List annually issued by the World Anti-Doping Agency. While for other permitted beta-2 agonists a threshold has been established, above which any finding constitutes an Adverse Analytical Finding, this is not the case with salmeterol. The salmeterol metabolite, α-hydroxysalmeterol, has been described as a potentially more suitable biomarker for the misuse of inhaled salmeterol. In this study, a new and rapid UHPLC-QTOF-MS method was developed and validated for the simultaneous quantification of salmeterol, α-hydroxysalmeterol and fluticasone in human urine and plasma, which can be used for doping control. The analytes of interest were extracted by means of solid phase extraction and were separated on a Zorbax Eclipse Plus C column. Detection was performed in a quadrupole time-of-flight mass spectrometer equipped with an electrospray ionization source, in positive mode for the detection of salmeterol and its metabolite and in negative mode for the detection of fluticasone. Method was validated over a linear range from 0.10 to 2.00 ng/ml for salmeterol and fluticasone, and from 1.00 to 20.0 ng/ml for α-hydroxysalmeterol, in urine, whereas in plasma, the linear range was from 0.025 to 0.500 ng/ml for salmeterol and fluticasone, respectively.
沙美特罗和氟替卡松每年都被世界反兴奋剂机构列入禁用清单。虽然对于其他允许使用的β2-激动剂，已经确定了一个阈值，超过这个阈值的任何发现都构成了不利的分析结果，但沙美特罗并非如此。沙美特罗的代谢物α-羟沙美特罗已被描述为一种更适合用于检测吸入用沙美特罗滥用的潜在生物标志物。在这项研究中，开发并验证了一种新的快速 UHPLC-QTOF-MS 方法，用于同时定量检测人尿液和血浆中的沙美特罗、α-羟沙美特罗和氟替卡松，可用于兴奋剂控制。通过固相萃取提取感兴趣的分析物，并在 Zorbax Eclipse Plus C 柱上进行分离。在配备电喷雾电离源的四极杆飞行时间质谱仪中以正模式检测沙美特罗及其代谢物，以负模式检测氟替卡松进行检测。该方法在尿液中沙美特罗和氟替卡松的线性范围为 0.10-2.00 ng/ml，α-羟沙美特罗的线性范围为 1.00-20.0 ng/ml；而在血浆中，沙美特罗和氟替卡松的线性范围分别为 0.025-0.500 ng/ml。
