Development and validation of liquid chromatography-silver ion coordination ionspray tandem mass spectrometric method for the simultaneous analysis of steroids in human urine
- Development and validation of liquid chromatography-silver ion coordination ionspray tandem mass spectrometric method for the simultaneous analysis of steroids in human urine
- 김소희; 차은주; 이강미; 김호준; 권오승; 이재익
- Issue Date
- 32nd Manfred Donike Workshop
- Anabolic androgenic steroids (AAS) are extensively abused to improve performance in sports and one of the most frequently detected substances in doping analysis. In our previous report (29th Manfred Donike Workshop, 2011), we reported the simultaneous ionization and detection technology for analysis of AAS by ultra-fast liquid chromatography coupled to silver ion coordination ionspray tandem mass spectrometry (UFLC-Ag+CIS/MS/MS). Ag+CIS/MS/MS is a powerful analytical technique for analysis of target substances at the same time. In this study, the analytical method using UFLC-Ag+CIS/MS/MS has been optimized and validated for the analysis of 95 AAS (73 exogenous AAS and 22 endogenous AAS). The validation results showed the intra- (0.8-9.2%) and inter-day (2.5-14.9%) precisions, limits of detection (0.0005-2.5 ng/mL), matrix effect (69.7-100.8%.) for screening analysis and the limits of detection (0.1-2.5 ng/mL) for confirmation analysis. These results revealed that the present methods were very high sensitive. Especially, the LODs of 8 substances were 0.0005 to 0.005 ng/mL. The LODs of 36 analytes were 0.01 to 0.05 ng/mL and 32 analytes were 0.1 to 0.5 ng/mL. The present method seems to be useful for the detection of the trace levels of AAS in human urine.
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