Open AccessQuantitative determination of major nandrolone metabolite in human urine by gas chromatography/mass spectrometry
Author(s) -
Pavel G. Shahoika,
Aliaksandr A. Ahabalayeu,
Olga N. Tchekhovskaya,
Yury G. Pakhadnia,
С. А. Беляев,
С. М. Лещев
Publication year - 2019
Publication title -
žurnal belorusskogo gosudarstvennogo universiteta. himiâ
Language(s) - English
Resource type - Journals
eISSN - 2617-3980
pISSN - 2520-257X
DOI - 10.33581/2520-257x-2019-1-78-85
Subject(s) - chromatography , chemistry , nandrolone , metabolite , urine , derivatization , detection limit , repeatability , gas chromatography–mass spectrometry , epitestosterone , mass spectrometry , solid phase extraction , gas chromatography , anabolism , steroid , biochemistry , hormone
Nandrolone is an anabolic androgenic steroid. The use of this substance is prohibited by World Anti-Doping Agency (WADA). In National Anti-Doping Laboratory, we have developed method for quantitative determination of major nandrolone metabolite – 19-norandrosterone in human urine by GC/MS technique (Agilent 7000). Proposed method includes sample preparation of urine samples with enzymatic hydrolysis, liquid-liquid extraction followed by derivatization step with MSTFA. Deuterated 19-norandrosterone has been used as internal standard. Total run time comprised 16 min. Lower limit of quantitation accounted for 1 ng/mL. Spiked urine samples were prepared by mixing blank urine with standard solutions of 19-norandrosterone in range 1–30 ng/mL, correlation coefficient larger than 0.99. Method was verified tofollowing validation parameters: selectivity, linearity, repeatability, accuracy, matrix effect, stability and robustness. Furthermore, measurement uncertainty was estimated. Thus, proposed method is able to detect threshold 19-norandrosterone in human urine and carry out its quantitation conforming WADA requirements.