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Comparison of gas chromatography/quadrupole time-of-flight and quadrupole Orbitrap mass spectrometry in anti-doping analysis: I. Detection of anabolic-androgenic steroids

机译:气相色谱/四极其飞行时间和四极氧覆盆子质谱法的抗掺杂分析中的比较:I.检测合成雄激素类固醇的检测

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Rationale Methods The World Anti-Doping Agency (WADA) encourages drug-testing laboratories to develop screening methods that can detect as many doping substances as possible in urine. The use of full-scan high-resolution acquisition (FS/HR) with gas chromatography/mass spectrometry (GC/MS) for the detection of known and unknown trimethylsilyl (TMS) derivatives of anabolic-androgenic steroids (AAS) provides anti-doping testing bodies with a new analytical tool. The AAS were extracted from urine samples by generic liquid-liquid extraction, after enzymatic hydrolysis, and TMS derivatization. The extracted urine was analyzed by GC/Q-TOF and GC/Q-Orbitrap to compare the performance of the two instrument types for the detection of 46 AAS in human urine. The quantitation of endogenous anabolic steroids and the ability of the two analytical platforms to comply with the requirements for testing as part of the WADA Athlete Biological Passport (ABP) were also assessed. Results Conclusions The data presented show that the analytical performance for both instruments complies with the WADA specifications. The limits of detection (LODs) for both instruments are well below the WADA 50% Minimum Required Performance Levels. The mass errors in the current study for the GC/Q-Orbitrap platform are lower than those obtained for the GC/Q-TOF instrument. The data presented herein proved that both molecular profiling platforms can be used for antidoping screening. The mass accuracies are excellent in both instruments; however, the GC/Q-Orbitrap performs better as it provides higher resolution than the GC/Q-TOF platform.
机译:理由方法世界反兴奋剂机构(WADA)鼓励药物测试实验室开发筛查方法,可以在尿液中检测尽可能多的掺杂物质。使用具有气相色谱/质谱(GC / MS)的全扫描高分辨率采集(FS / HR)用于检测的是有代谢雄激素类固醇(AAS)的已知和未知的三甲基甲硅烷基(TMS)衍生物(AAS)提供防掺杂使用新的分析工具测试机构。通过通用液 - 液萃取,酶水解后,从尿液样品中提取Aas,并酶促衍生化。通过GC / Q-TOF和GC / Q-orbitrap分析所提取的尿液,以比较两种仪器类型的性能,用于检测人尿中的46 AAs。还评估了内源性合成代谢类固醇的定量以及两种分析平台符合测试要求作为WADA运动员生物护照(ABP)的要求。结果结论所提出的数据表明,两种仪器的分析性能符合WADA规范。两种仪器的检测极限(LOD)远低于WADA 50%所需的性能水平。 GC / Q-orbitrap平台目​​前研究中的质量误差低于GC / Q-TOF仪器的研究。本文呈现的数据证明,两种分子分析平台可用于抗化筛选。仪器两种仪器都有优异的型号;然而,GC / Q-Orbitrap比GC / Q-TOF平台提供更高的分辨率更好。

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