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Fast and Sensitive Screening of Oxandrolone and Its Major Metabolite 17-Epi-Oxandrolone in Human Urine by UHPLC-MS/MS with On-Line SPE Sample Pretreatment
J. Galba, J. Piešťanský, A. Kováč, D. Olešová, O. Cehlár, M. Kertys, P. Kozlík, P. Chaľová, B. Tirčová, K. Slíž, P. Mikuš
Jazyk angličtina Země Švýcarsko
Typ dokumentu časopisecké články
Grantová podpora
APVV-15-0585
Agency for Science, Technology and Research
APVV-18-0340
Agency for Science, Technology and Research
VEGA 1/0463/18
Agentúra Ministerstva Školstva, Vedy, Výskumu a Športu SR
KEGA 027UK-4/2020
Kultúrna a Edukacná Grantová Agentúra MŠVVaŠ SR
Free Medical Journals od 1997
PubMed Central od 2001
Europe PubMed Central od 2001
ProQuest Central od 1997-01-01
Open Access Digital Library od 1997-01-01
Medline Complete (EBSCOhost) od 2009-03-01
Health & Medicine (ProQuest) od 1997-01-01
Odkazy
PubMed
33477515
DOI
10.3390/molecules26020480
Knihovny.cz E-zdroje
- MeSH
- analýza moči metody MeSH
- extrakce na pevné fázi metody MeSH
- lidé MeSH
- oxandrolon izolace a purifikace metabolismus moč MeSH
- tandemová hmotnostní spektrometrie metody MeSH
- vysokoúčinná kapalinová chromatografie metody MeSH
- Check Tag
- lidé MeSH
- Publikační typ
- časopisecké články MeSH
Oxandrolone, a synthetic testosterone analog, is used for the treatment of several diseases associated with weight loss. Unfortunately, oxandrolone is abused by many athletes and bodybuilders due to its strong anabolic effect. We have developed and validated a highly sensitive and rapid on-line SPE-UHPLC-MS/MS method for the determination of oxandrolone and simultaneous identification of its major metabolite 17-epi-oxandrolone in urine matrices. Enrichment of the analytes via an integrated solid-phase extraction was achieved using an Acquity UPLC BEH C18 Column. Subsequently, the chromatographic separation of the on-line preconcentrated sample fraction was achieved using an Acquity HSS T3 C18 Column. For the structural identification of these analytes, a high-resolution mass spectrometer Synapt-G2Si coupled to the Acquity M-class nano-LC system with ionKey source was used. A highly sensitive determination of oxandrolone was achieved using a tandem quadrupole mass spectrometer XEVO TQD. The method was successfully validated in the linear range of oxandrolone from 81.63 pg·mL-1 (limit of quantification, LOQ) to 5000 pg·mL-1 in the human urine matrix. It was applied to the analysis of real urine samples obtained from a healthy volunteer after the oral administration of one dose (10 mg) of oxandrolone. Concentration vs. time dependence was tested in the time interval of 4 h-12 days (after oral administration) to demonstrate the ability of the method to detect the renal elimination of oxandrolone from the human body. Favorable performance parameters along with successful application indicate the usefulness of the proposed method for its routine use in antidoping control labs.
Biomedical Research Center of the Slovak Academy of Sciences in Bratislava 84510 Bratislava Slovakia
Institute of Neuroimmunology Slovak Academy of Sciences Dubravska cesta 9 84510 Bratislava Slovakia
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- $a Galba, Jaroslav $u Department of Pharmaceutical Analysis and Nuclear Pharmacy, Faculty of Pharmacy, Comenius University in Bratislava, Odbojarov 10, 832 32 Bratislava, Slovakia $u Biomedical Research Center of the Slovak Academy of Sciences in Bratislava, 84510 Bratislava, Slovakia
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- $a Oxandrolone, a synthetic testosterone analog, is used for the treatment of several diseases associated with weight loss. Unfortunately, oxandrolone is abused by many athletes and bodybuilders due to its strong anabolic effect. We have developed and validated a highly sensitive and rapid on-line SPE-UHPLC-MS/MS method for the determination of oxandrolone and simultaneous identification of its major metabolite 17-epi-oxandrolone in urine matrices. Enrichment of the analytes via an integrated solid-phase extraction was achieved using an Acquity UPLC BEH C18 Column. Subsequently, the chromatographic separation of the on-line preconcentrated sample fraction was achieved using an Acquity HSS T3 C18 Column. For the structural identification of these analytes, a high-resolution mass spectrometer Synapt-G2Si coupled to the Acquity M-class nano-LC system with ionKey source was used. A highly sensitive determination of oxandrolone was achieved using a tandem quadrupole mass spectrometer XEVO TQD. The method was successfully validated in the linear range of oxandrolone from 81.63 pg·mL-1 (limit of quantification, LOQ) to 5000 pg·mL-1 in the human urine matrix. It was applied to the analysis of real urine samples obtained from a healthy volunteer after the oral administration of one dose (10 mg) of oxandrolone. Concentration vs. time dependence was tested in the time interval of 4 h-12 days (after oral administration) to demonstrate the ability of the method to detect the renal elimination of oxandrolone from the human body. Favorable performance parameters along with successful application indicate the usefulness of the proposed method for its routine use in antidoping control labs.
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