Project Start Date: 2008
Dr. Tom Brenna
Dr. Herbert Tobias
Dr. Brenna and Dr. Tobias seek to improve the efficiency and accuracy of steroid detection in urine via the coupling of comprehensive 2D Gas Chromatography (GCxGC) with isotope ration mass spectrometry (IRMS). While Dr. Brenna’s initial research (funded by the PCC in 2008) ran into technological challenges which precluded routine use of his important findings (including reactor system leaks at the required 108 degrees Celsius), PCC TRF funding has enabled R&D efforts to design equipment capable of withstanding the high temperatures required for wide scale, highly precise isotope analyses of steroids and other doping agents using the novel method designed by Brenna and Tobias. The new reactor design functions in the fast GC-C-IRMS system without leaks and demonstrates good peak fidelity of fast GC Chromatographic peaks. Furthermore, initial characterization of steroid carbon isotope rations is promising, with additional evaluation currently underway.
Potential IRMS Steroidome Benefits:
- Cost savings and increased efficiency through increased sample throughpout on a given instrument
- Decreased detection limits, allowing for routine testing of multiple PEDs
Evaluation of the micro-reactor prototype is in progress. Once the evaluation process is complete, TRF funding will facilitate the production of a faster electronic card and software development to achieve efficient adoption into labs through inexpensive modification of existing equipment.
TOBIAS, H.J., ZHANG, Y., AND BRENNA, J.T. HIGHLY SENSITIVE AND SELECTIVE ANALYSIS OF URINARY STEROIDS BY COMPREHENSIVE TWODIMENSIONAL AS CHROMATOGRAPHY COMBINED WITH POSITIVE CHEMICAL IONIZATION QUADRUPOLE MASS SPECTROMETRY. ANALYST. 137(13): 3102–3110.DOI: 10.1039/C2AN35087D, 2012.
ZHANG, Y., TOBIAS, H.J., AUCHUS, R.J., AND BRENNA, J.T. COMPREHENSIVE 2-DIMENSIONAL GAS CHROMATOGRAPHY FAST QUADRUPOLE MASS SPECTROMETRY (GC × GC-QMS) FOR URINARY STEROID PROFILING: MASS SPECTRAL CHARACTERISTICS WITH CHEMICAL IONIZATION. DRUG TESTING AND ANALYSIS. 3: 857–867. DOI:10.1002/DTA.380, 2011.
TOBIAS, H.J., ZHANG, Y., AUCHUS, R.J., AND BRENNA, J.T. DETECTION OF SYNTHETIC TESTOSTERONE USE BY NOVEL COMPREHENSIVE TWODIMENSIONAL GAS CHROMATOGRAPHY COMBUSTION–ISOTOPE RATIO MASS SPECTROMETRY. ANALYTICAL CHEMISTRY. 83 (18), PP 7158-7165. DOI: 10.1021/AC2015849, 2011.
TOBIAS, H.J., SACKS, G.L., ZHANG, Y., AND BRENNA, J.T. COMPREHENSIVE TWO-DIMENSIONAL GAS CHROMATOGRAPHY COMBUSTION ISOTOPE RATIO MASS SPECTROMETRY. ANALYTICAL CHEMISTRY. 80 (22), PP 8613–8621. DOI: 10.1021/AC801511D, 2008.