Sensitivity of GC-EI/MS, GC-EI/MS/MS, LC-ESI/MS/MS, LC-Ag(+) CIS/MS/MS, and GC-ESI/MS/MS for analysis of anabolic steroids in doping control.
This study compared the sensitivity of various separation and ionization methods, including gas chromatography with an electron ionization source (GC-EI), liquid chromatography with an electrospray ionization source (LC-ESI), and liquid chromatography with a silver ion coordination ion spray source (LC-Ag(+) CIS), coupled to a mass spectrometer (MS) for steroid analysis. Chromatographic conditions, mass spectrometric transitions, and ion source parameters were optimized. The majority of steroids in GC-EI/MS/MS and LC-Ag(+) CIS/MS/MS analysis showed higher sensitivities than those obtained with other analytical methods. The limits of detection (LODs) of 65 steroids by GC-EI/MS/MS, 68 steroids by LC-Ag(+) CIS/MS/MS, 56 steroids by GC-EI/MS, 54 steroids by LC-ESI/MS/MS, and 27 steroids by GC-ESI/MS/MS were below cut-off value of 2.0 ng/mL. LODs of steroids that formed protonated ions in LC-ESI/MS/MS analysis were all lower than the cut-off value. Several steroids such as unconjugated C3-hydroxyl with C17-hydroxyl structure showed higher sensitivities in GC-EI/MS/MS analysis relative to those obtained using the LC-based methods. The steroids containing 4, 9, 11-triene structures showed relatively poor sensitivities in GC-EI/MS and GC-ESI/MS/MS analysis. The results of this study provide information that may be useful for selecting suitable analytical methods for confirmatory analysis of steroids.
Doping Control Center, Korea Institute of Science and Technology, Hwarang-ro 14-gil 5, Seongbuk-gu, Seoul, 136-791, Korea.|Department of Chemistry, Research Institute for Natural Sciences, Korea University, 145, Anam-ro, Seongbuk-gu, Seoul, 136-701, Korea.
Eunju
E
Cha
Doping Control Center, Korea Institute of Science and Technology, Hwarang-ro 14-gil 5, Seongbuk-gu, Seoul, 136-791, Korea.
Sohee
S
Kim
Doping Control Center, Korea Institute of Science and Technology, Hwarang-ro 14-gil 5, Seongbuk-gu, Seoul, 136-791, Korea.
Ho Jun
HJ
Kim
Doping Control Center, Korea Institute of Science and Technology, Hwarang-ro 14-gil 5, Seongbuk-gu, Seoul, 136-791, Korea.
Kang Mi
KM
Lee
Doping Control Center, Korea Institute of Science and Technology, Hwarang-ro 14-gil 5, Seongbuk-gu, Seoul, 136-791, Korea.
Ki Hun
KH
Kim
Doping Control Center, Korea Institute of Science and Technology, Hwarang-ro 14-gil 5, Seongbuk-gu, Seoul, 136-791, Korea.
Oh-Seung
OS
Kwon
Doping Control Center, Korea Institute of Science and Technology, Hwarang-ro 14-gil 5, Seongbuk-gu, Seoul, 136-791, Korea.
Jaeick
J
Lee
D045930:Anabolic Agents / Q000652:urine*; D002138:Calibration; D002853:Chromatography, Liquid / Q000592:standards; D004300:Doping in Sports; D008401:Gas Chromatography-Mass Spectrometry / Q000592:standards; D006801:Humans; D057230:Limit of Detection; D058573:Performance-Enhancing Substances / Q000652:urine*; D011237:Predictive Value of Tests; D012015:Reference Standards; D015203:Reproducibility of Results; D021241:Spectrometry, Mass, Electrospray Ionization / Q000592:standards; D013256:Steroids / Q000652:urine*; D015813:Substance Abuse Detection / Q000379:methods* / Q000592:standards; D053719:Tandem Mass Spectrometry / Q000592:standards; D016482:Urinalysis
D045930:Anabolic Agents; D058573:Performance-Enhancing Substances; D013256:Steroids
anabolic steroids; doping control; gas chromatography-mass spectrometry; ionization; liquid chromatography-tandem mass spectrometry; sensitivity