Detection of oxandrolone and its metabolite in urine by high-performance liquid chromatography-high-resolution mass spectrometry with atmospheric pressure chemical ionization and orbitrap detection after ceasing drug administration

Viryus, E. D.; Sobolevskii, T. G.; Rodchenkov, G. M.

doi:10.1134/s1061934809010079

Cited by 5 publications

(7 citation statements)

References 4 publications

Supporting

Mentioning

Contrasting

Order By: Relevance

“…As the very first step, the presence of glucuronide and sulfate metabolic forms of OXA in the real samples was examined in order to unify possible OXA forms for the best analyte recovery. For this purpose, the urine samples were hydrolyzed enzymatically using β-glucuronidase, which provides both β-glucuronidase and arylsulfatase activity [ 35 ], according to the procedure described previously [ 31 ]. There were found no significant differences in OXA concentrations between the hydrolyzed samples and the samples prepared according to the procedure described in Section 3.4.3 .…”

Section: Resultsmentioning

confidence: 99%

“…Viryus, et al [ 30 ] coupled high-resolution mass spectrometry (HRMS) (orbitrap) with HPLC via APCI for screening doping controls. The same group developed an HPLC-HRMS method enabling identification of OXA in the urine as long as two weeks after ending its 15-day administration [ 31 ]. Guddat, et al [ 32 ] used GC-MS/MS and LC-MS/MS for the identification of OXA and its metabolites in urine samples.…”

Section: Introductionmentioning

confidence: 99%

“…The most frequently employed sample clean-up procedure in these LC-MS analyses of urine samples containing OXA was liquid-liquid extraction (LLE). It was applied after sample hydrolysis and followed by evaporation of organic solvent and reconstitution by a mobile phase [ 27 , 29 , 30 , 31 , 32 ]. The solid-phase extraction (SPE), as sample preparation for an LC-MS/MS analysis of oxandrolone sulfate conjugates in urine, was described in 2016 by Rzeppa and Viet [ 33 ].…”

Section: Introductionmentioning

confidence: 99%

See 2 more Smart Citations

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

et al. 2021

View full text Add to dashboard Cite

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.

show abstract

Section: Resultsmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

See 1 more Smart Citation

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

et al. 2021

View full text Add to dashboard Cite

show abstract

“…Urine samples were treated as described elsewhere with minimal modifications. Briefly, 1 mL of phosphate buffer (0.8 M, pH 6.3) containing 3% of β‐glucuronidase and 1.5 µg of methyltestosterone as internal standard was added to 3 mL of urine.…”

Section: Expepimentalmentioning

confidence: 99%

High‐temperature high‐performance liquid chromatography on a porous graphitized carbon column coupled to an Orbitrap mass spectrometer with atmospheric pressure photoionization for screening exogenous anabolic steroids in human urine

Virus

Luzyanin

Ivanov

et al. 2015

Rapid Comm Mass Spectrometry

View full text Add to dashboard Cite

show abstract

“…Low detection limits (3 × 10 -13 -1.2 × 10 -12 g) have been achieved in real samples. [97][98][99][100][101] Researchers from ADC have developed an approach allowing the maximization of the number of compounds that can be determined with high sensitivity in a single run. 102 It involves so-called "wrong-way-round ionization" in ESI for the simultaneous detection of multiple classes of doping substances (stimulants, diuretics, b 2 -agonists, b-blockers, antiestrogens, glucocorticosteroids and anabolic agents) without the need to switch the polarity.…”

Section: Doping-controlmentioning

confidence: 99%

Mass Spectrometry in Russia

Заикин

Сысоев

2013

Eur J Mass Spectrom (Chichester)

View full text Add to dashboard Cite

The present review covers the main research in the area of mass spectrometry from the 1990s which was about the same time as the Russian Federation emerged from the collapse of the Soviet Union (USSR). It consists of two main parts-application of mass spectrometry to chemistry and related fields and creation and development of mass spectrometric technique. Both traditional and comparatively new mass spectrometric methods were used to solve various problems in organic chemistry (reactivity of gas-phase ions, structure elucidation and problems of identification, quantitative and trace analysis, differentiation of stereoisomers, derivatization approaches etc.), biochemistry (proteomics and peptidomics, lipidomics), medical chemistry (mainly the search of biomarkers, pharmacology, doping control), environmental, petrochemistry, polymer chemistry, inorganic and physical chemistry, determination of natural isotope ratio etc. Although a lot of talented mass spectrometrists left Russia and moved abroad after the collapse of the Soviet Union, the vitality of the mass spectral community proved to be rather high, which allowed the continuation of new developments in the field of mass spectrometric instrumentation. They are devoted to improvements in traditional magnetic sector mass spectrometers and the development of new ion source types, to analysis and modification of quadrupole, time-of-flight (ToF) and ion cyclotron resonance (ICR) analyzers. The most important achievements are due to the creation of multi-reflecting ToF mass analyzers. Special attention was paid to the construction of compact mass spectrometers, particularly for space exploration, of combined instruments, such as ion mobility spectrometer/mass spectrometer and accelerating mass spectrometers. The comparatively young Russian Mass Spectrometry Society is working hard to consolidate the mass spectrometrists from Russia and foreign countries, to train young professionals on new appliances and regularly holds conferences on mass spectrometry. For ten years, a special journal Mass-spektrometria has published papers on all disciplines of mass spectrometry.

show abstract

Detection of oxandrolone and its metabolite in urine by high-performance liquid chromatography-high-resolution mass spectrometry with atmospheric pressure chemical ionization and orbitrap detection after ceasing drug administration

Cited by 5 publications

References 4 publications

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

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

High‐temperature high‐performance liquid chromatography on a porous graphitized carbon column coupled to an Orbitrap mass spectrometer with atmospheric pressure photoionization for screening exogenous anabolic steroids in human urine

Mass Spectrometry in Russia

Contact Info

Product

Resources

About