Novel gas chromatography-electrospray ionization/orbitrap mass spectrometry (GC-ESI/HRMS) for ionization and analysis of steroids
- Novel gas chromatography-electrospray ionization/orbitrap mass spectrometry (GC-ESI/HRMS) for ionization and analysis of steroids
- 차은주; 이재익
- Issue Date
- 제111회 대한화학회 학술발표회
- Anabolic steroids are extensively abused to improve performance in sports. Gas chromatography-electron impact ionization/mass spectrometry (GC-EI/MS) method has been generally used for the detection of steroids. But conventional methods using the GC-EI/MS have technical bottleneck such as the hard ionization of electron impact ion source. Recently, even though the analytical methods using liquid chromatography-electrospray ionization/tandem mass spectrometry (LC-ESI/MS/MS) have been developed, the LC-ESI/MS/MS methods have also several bottlenecks such as the simultaneous ionization in single ion source and the chromatographic separation. Therefore, in this study, the novel gas chromatography-electrospray ionization/orbitrap mass spectrometry (GC-ESI/HRMS) instrument system was developed to overcome these bottlenecks by combining the GC and ESI source, and applied to the analysis of steroids. GC and ESI source were interfaced by homemade heated column transfer line and the distance, angle, spray solvent, acid modifier and ion source parameters such as gas, temperature and voltage were optimized to improve the ionization efficiency. After the extraction from spiked urine sample, 86 anabolic agents (64 exogenous substances and 22 endogenous substances) were converted into trimethylsilyl (TMS) derivatives and analyzed by GC-ESI/HRMS to demonstrate the sensitivity, selectivity, ionization effect of TMS-derivatives and chromatographic resolution. The results revealed that the present GC-ESI/HRMS system and analytical method are suitable for identification of anabolic steroids in human urine for doping control.
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