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 4 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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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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Detection of Over 110 Anabolic–Androgenic Steroids, Corticosteroids and/or Their Esters in Horse Hair Using Ultra‐High‐Performance Liquid Chromatography–High‐Resolution Mass Spectrometry and Gas Chromatography–Tandem Mass Spectrometry After Solid‐Supported Liquid Extraction

So,

Kwok,

Ching

et al. 2024

Drug Testing and Analysis

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Anabolic–androgenic steroids (AAS) are banned substances in both human and equine sports. They are often administered intramuscularly to horses in esterified forms for the purpose of extending their duration of action. As such, the detection of intact esters of endogenous steroids in hair is particularly advantageous, as it can provide unequivocal proof of their external origin. Compared with urine and blood matrices, hair in general allows a longer detection window as long as the administered drug can be incorporated into hair and has not degraded. This can be useful in doping control of equine sports, where the timing of sample collection may be critical due to the transient nature of AAS in other biological fluids. This paper describes the detection of AAS and/or their esters, as well as corticosteroids, in horse hair using ultra‐high‐performance liquid chromatography–high‐resolution mass spectrometry (UPLC‐HRMS) and gas chromatography–tandem mass spectrometry (GC‐MS/MS) after solid‐supported liquid extraction (SLE) at basic pH. The developed UPLC‐HRMS and GC‐MS/MS methods in combination allowed the detection of 117 AAS, corticosteroids and/or their esters with estimated limits of detection down to sub‐ppb levels and with good inter‐day precision. Method applicability has been demonstrated through the detections of (i) boldenone undecylenate, nandrolone phenylpropionate and trenbolone acetate in three proficiency testing hair samples and (ii) nandrolone as a metabolite in a post‐administration hair sample collected from a castrated horse having been administered nandrolone decanoate.

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Towards Improved Steroid Hormone Analysis: The Shift from Immunoassays to Mass Spectrometry

Deng,

Bi,

Zheng

et al. 2024

J. Anal. Test.

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

Cited by 4 publications

References 31 publications

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

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

Detection of Over 110 Anabolic–Androgenic Steroids, Corticosteroids and/or Their Esters in Horse Hair Using Ultra‐High‐Performance Liquid Chromatography–High‐Resolution Mass Spectrometry and Gas Chromatography–Tandem Mass Spectrometry After Solid‐Supported Liquid Extraction

Towards Improved Steroid Hormone Analysis: The Shift from Immunoassays to Mass Spectrometry

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