Validation and application of a screening method for beta2-agonists, anti-estrogenic substances and mesocarb in human urine using liquid chromatography/tandem mass spectrometry.
Electrospray ionization (ESI) mass spectra of 15 anti-estrogenic substances, beta2-agonists and mesocarb were investigated in terms of fragmentation patterns. On the basis of this product ion information, a simultaneous screening method for anti-estrogenic substances, beta2-agonists and mesocarb was developed for doping control purposes. After hydrolysis, liquid-liquid extraction was adopted for the sample preparation. The recoveries for all compounds were 30 and 96%. A single liquid chromatography/tandem mass spectrometry (LC/MS/MS) analysis could be performed in 13 min for the analysis of 15 anti-estrogenic substances, beta2-agonists and mesocarb. A quantitative analysis was also validated. Inaccuracies were below +/-12% and precisions varied from 0 to 15.8%. The limit of detection was below 10 ng/mL except formestane (300 ng/mL) and aminoglutethimide (100 ng/mL). The validated method was applied for the analysis of excretion samples.
Kang
Min-Jung
MJ
Bioanalysis & Biotransformation Center, Korea Institute of Science and Technology, 130-650, Hawolgokdong 39-1, Seoul, Korea. mjkang1@kist.re.kr
Hwang
Yong Hee
YH
Lee
Won
W
Kim
Dong-Hyun
DH
D058666:Adrenergic beta-2 Receptor Agonists; D000318:Adrenergic beta-Agonists / Q000652:urine*; D000328:Adult; D000697:Central Nervous System Stimulants / Q000652:urine*; D002851:Chromatography, High Pressure Liquid; D004300:Doping in Sports / Q000379:methods; D020847:Estrogen Receptor Modulators / Q000652:urine*; D006801:Humans; D008297:Male; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods*; D015813:Substance Abuse Detection / Q000379:methods*; D013558:Sydnones / Q000652:urine*; D053719:Tandem Mass Spectrometry
D058666:Adrenergic beta-2 Receptor Agonists; D000318:Adrenergic beta-Agonists; D000697:Central Nervous System Stimulants; D020847:Estrogen Receptor Modulators; D013558:Sydnones; C009257:sidnocarb