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基于气相色谱-电子轰击-混合四极杆-轨道阱质谱法筛选掺杂化合物的非靶向采集策略:聚焦外源性合成代谢类固醇

Non-targeted acquisition strategy for screening doping compounds based on GC-EI-hybrid quadrupole-Orbitrap mass spectrometry: A focus on exogenous anabolic steroids.

作者信息

de Albuquerque Cavalcanti Gustavo, Rodrigues Lucas Martins, Dos Santos Leonardo, Zheng Xin, Gujar Amit, Cole Jason, Padilha Monica Costa, de Aquino Neto Francisco Radler

机构信息

Brazilian Doping Control Laboratory- LBCD-LADETEC, Federal University of Rio de Janeiro-UFRJ, Rio de Janeiro, Brazil.

Thermo Fisher Scientific, Austin, Texas, USA.

出版信息

Drug Test Anal. 2018 Mar;10(3):507-517. doi: 10.1002/dta.2227. Epub 2017 Jul 27.

DOI:10.1002/dta.2227
PMID:28600878
Abstract

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.

摘要

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。

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