Quantification of urinary steroids by supported liquid extraction with GC-MS/MS: Unravelling cyclic fluctuations of steroid profiling in regular menstrual cycle

Liu, Mengpan; Ge, Yuqi; Xu, Xin; Liao, Lei

doi:10.1016/j.jpba.2022.114789

Cited by 3 publications

(1 citation statement)

References 31 publications

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“…After a mild and stable derivatization procedure, the synthesized trimethylsilylated hydroxyls decrease the boiling point of targets (e.g., androgens, estrogens, and progestogens) and enhance the gas chromatography performance of targets. Due to these advantages of MSTFA, it has been applied in various different fields for over half a century, especially in anti-doping analysis [ 26 , 30 , 31 , 32 ]. However, the structure of glucocorticoids and androgens, estrogens, or progestogens are different, especially at the C 17 and C 11 positions ( Table 1 ).…”

Section: Resultsmentioning

confidence: 99%

Derivatization-Enhanced Analysis of Glucocorticoids for Structural Characterization by Gas Chromatography-Orbitrap High-Resolution Mass Spectrometry

Ge,

Liu,

Deng

et al. 2023

Molecules

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Glucocorticoids are classified in section S9 of the Prohibited List of the World Anti-Doping Agency, due to a potential risk to improving physical performance and causing harm to the health of athletes. Based on the similar physiological actions of glucocorticoids, both differentiating known glucocorticoids and identifying unknown glucocorticoids are important for doping control. Gas chromatography coupled with mass spectrometry plays an important role in structural characterization because of abundant structural diagnostic ions produced by electron ionization. It also provides a chance to study the fragmentation patterns. Thus, an enhanced derivatization procedure was optimized to produce trimethylsilylated glucocorticoids and structural diagnostic ions of nineteen trimethylsilylated glucocorticoids were obtained by gas chromatography-orbitrap high-resolution mass spectrometry. In our study, glucocorticoids were classified as: 3-keto-4-ene, 1,4-diene-3-keto, 3α-hydroxy with saturated A-ring, 21-hydroxy-20-keto and halo substituent glucocorticoids based on their structural difference. Structural diagnostic ions that contributed to structural characterization were specifically presented and the fragment patterns were demonstrated according to the above categories. This study not only gave new insights into the structural characterization of these glucocorticoids but also provided evidence for tracing unknown glucocorticoids or chemically modified molecules.

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