Development and optimization of novel gas chromatography-electrospray ionization mass spectrometry for steroids analysis
- Development and optimization of novel gas chromatography-electrospray ionization mass spectrometry for steroids analysis
- 차은주; 김소희; 김희원; 류이슬; 최보경; 김호준; 이재익
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- Anabolic steroids are synthetic derivatives of the male hormone. Theses anabolic steroids have been frequently used to improve the athletic performance. Gas chromatography-mass spectrometry (GC-MS) with the electron impact ionization (EI) as trimethylsilyl (TMS)-derivatives of steroids is powerful analytical method, and it has been generally used for the detection of diverse steroids. However, these conventional methods using the GC-EI/MS have technical bottleneck such as excess energetic ionization process. Recently, various analytical methods have been developed using liquid chromatography-tandem mass spectrometry (LC-MS/MS) with electrospray ionization, but LC-MS/MS has also a bottleneck for ionization in steroid analysis. In this study, we developed novel gas chromatography-electrospray ionization/orbitrap mass spectrometry (GC-ESI/HRMS) instrument systems. The GC-ESI/HRMS instrument system was developed to overcome bottlenecks by combining the GC and ESI source. GC and ESI source were interfaced by homemade heated column transfer line and optimized the interface parameters such as distances between ESI needle and outlet of GC capillary column, angle, spray solvent, acid modifier and nebulizer gas flow to improve the ionization efficiency. Especially, the results of spray solvent flow gave rise to the concentration dependent mechanism (peak dilution effect). The results revealed that GC-ESI/HRMS technique provides a high chromatographic resolution, soft ionization process, and high selectivity.
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