de Albuquerque Cavalcanti Gustavo, Rodrigues Lucas Martins, Dos Santos Leonardo, Zheng Xin, Gujar Amit, Cole Jason, Padilha Monica Costa, de Aquino Neto Francisco Radler
Brazilian Doping Control Laboratory- LBCD-LADETEC, Federal University of Rio de Janeiro-UFRJ, Rio de Janeiro, Brazil.
Thermo Fisher Scientific, Austin, Texas, USA.
Drug Test Anal. 2018 Mar;10(3):507-517. doi: 10.1002/dta.2227. Epub 2017 Jul 27.
This is a first look at a non-targeted screening method based on Orbitrap gas chromatography-mass spectrometry (GC-MS) technology for a large number of banned compounds in sports found in urine, including exogenous anabolic steroids, β-agonists, narcotics, stimulants, hormone modulators, and diuretics. A simple sample preparation was processed in four steps: an enzymatic hydrolysis, liquid-liquid extraction, evaporation, and trimethylsilylation. All compounds were able to meet the World Anti-Doping Agency's sensitivity criteria with mass accuracies less than 1 ppm and with sufficient points across the peak by running the Orbitrap GC-MS in full-scan mode. In addition, we discuss our initial findings of using a full-scan selected ion monitoring-tandem mass spectrometry (SIM-MS/MS) approach as a way to obtain lower detection limits and reach desirable selectivity for some exogenous anabolic steroids.
这是首次对基于轨道阱气相色谱-质谱联用(GC-MS)技术的非靶向筛查方法进行研究,该方法用于检测尿液中发现的大量体育赛事禁用化合物,包括外源性合成代谢类固醇、β-激动剂、麻醉药品、兴奋剂、激素调节剂和利尿剂。简单的样品制备过程分四个步骤进行:酶解、液液萃取、蒸发和三甲基硅烷化。通过在全扫描模式下运行轨道阱GC-MS,所有化合物的质量准确度均低于1 ppm,峰上有足够的点数,能够满足世界反兴奋剂机构的灵敏度标准。此外,我们还讨论了使用全扫描选择离子监测串联质谱(SIM-MS/MS)方法的初步研究结果,该方法可用于获得更低的检测限,并对某些外源性合成代谢类固醇实现理想的选择性。