Validation of an ultra-sensitive detection method for steroid esters in plasma for doping analysis using positive chemical ionization GC-MS/MS

Renterghem, Pieter Van; Viaene, Wouter; Gansbeke, Wim Van; Barrabin, Juliana; Iannone, Michele; Polet, Michaël; T’Sjoen, Guy; Deventer, Koen; Eenoo, Peter Van

doi:10.1016/j.jchromb.2020.122026

Cited by 28 publications

(23 citation statements)

References 30 publications

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“…injection of a single dose of 1000 mg testosterone (Nebido ® ). 157 Analytical techniques for testosterone measurement in humans…”

Section: Detection Of Testosterone Doping In Forensic Casesmentioning

confidence: 99%

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Testosterone Use and Abuse : Methodological Aspects in Forensic Toxicology and Clinical Diagnostics

Lood

2021

Linköping University Medical Dissertations

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Abuse of anabolic androgenic steroids (AAS) is widespread in society and is today a major public health problem, associated with mental and somatic adverse effects and risk behavior, such as use of other illicit drugs and criminality. Testosterone, the most important endogenous male androgen, is therapeutically used in replacement therapy but is also extensively used as a doping agent. Traditionally, testosterone abuse is detected in urine in forensic cases and in serum in clinical diagnosis and monitoring, and free bioavailable serum testosterone is calculated by formulas. Salivary testosterone is however an attractive biomarker, as testosterone in saliva is supposed to reflect free testosterone in serum.

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“…injection of a single dose of 1000 mg testosterone (Nebido ® ). 157 Analytical techniques for testosterone measurement in humans…”

Section: Detection Of Testosterone Doping In Forensic Casesmentioning

confidence: 99%

“…This would be an unambiguous proof of illegal administration of testosterone, independently on endogenous testosterone levels and genetic variations. 156,157 It would also be of clinical interest to evaluate whether the serum levels of the ester TU have a potential role in monitoring androgen therapy.…”

Section: Future Perspectivesmentioning

confidence: 99%

Testosterone Use and Abuse : Methodological Aspects in Forensic Toxicology and Clinical Diagnostics

Lood

2021

Linköping University Medical Dissertations

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“…Moreover, the testing of serum (or plasma) for T and nandrolone esters supports anti‐doping efforts as the mere presence of any of these exogenous analytes would corroborate the administration of a prohibited substance. An improved testing strategy for nine T esters and two nandrolone esters from NaF plasma was reported by Van Renterghem et al, based on LLE of 500 μl of plasma, concentration, HPLC fractionation, concentration of the collected fraction, and subsequent trimethylsilylation for GC‐CI‐MS/MS analysis 82 . The GC was equipped with a HP5MS capillary column (12 m × 0.25 mm inner diameter, 0.25 μm film thickness), the CI gas was ammonia, and the MS was a QqQ apparatus operated in MRM mode.…”

Section: Anabolic Agentsmentioning

confidence: 99%

“…esters and two nandrolone esters from NaF plasma was reported by Van Renterghem et al, based on LLE of 500 μl of plasma, concentration, HPLC fractionation, concentration of the collected fraction, and subsequent trimethylsilylation for GC-CI-MS/MS analysis 82. The GC was equipped with a HP5MS capillary column (12 m × 0.25 mm inner diameter, 0.25 μm film thickness), the CI gas was ammonia, and the MS was a QqQ apparatus operated in MRM mode.…”

mentioning

confidence: 96%

Annual banned‐substance review: Analytical approaches in human sports drug testing 2019/2020

Thevis

Kuuranne

Geyer

2020

Drug Testing and Analysis

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Analytical chemistry-based research in sports drug testing has been a dynamic endeavor for several decades, with technology-driven innovations continuously contributing to significant improvements in various regards including analytical sensitivity, comprehensiveness of target analytes, differentiation of natural/ endogenous substances from structurally identical but synthetically derived compounds, assessment of alternative matrices for doping control purposes, and so forth. The resulting breadth of tools being investigated and developed by anti-doping researchers has allowed to substantially improve anti-doping programs and data interpretation in general. Additionally, these outcomes have been an extremely valuable pledge for routine doping controls during the unprecedented global health crisis that severely affected established sports drug testing strategies. In this edition of the annual banned-substance review, literature on recent developments in antidoping published between October 2019 and September 2020 is summarized and discussed, particularly focusing on human doping controls and potential applications of new testing strategies to substances and methods of doping specified the World Anti-Doping Agency's 2020 Prohibited List.

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“…With regard to sample treatment for biological matrices, proteins (up to 80 g L −1 ) are the major interferents in plasmatic steroids determination, calling for pretreatments such as sample dilution and proteins precipitation [ 5 , 6 , 7 , 8 , 9 , 10 , 11 , 12 , 13 ] before extraction that is done, for instance, by solid-phase extraction (SPE) [ 5 , 7 , 8 , 9 , 12 , 13 ]. Quantitation is today mainly performed by high-performance liquid chromatography coupled with mass spectrometry detection (HPLC–MS), which ensures selective and sensitive determination [ 7 , 8 , 9 , 12 , 14 , 15 , 16 ]; some methods also involving gas chromatography coupled with MS detection have been proposed, necessarily requiring analytes derivatization before analysis [ 13 , 17 ].…”

Section: Introductionmentioning

confidence: 99%

Magnetic Micro-Solid-Phase Extraction Using a Novel Carbon-Based Composite Coupled with HPLC–MS/MS for Steroid Multiclass Determination in Human Plasma

et al. 2021

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A micron-sized sorbent, Magn-Humic, has been prepared by humic acids pyrolysis onto silica-coated magnetite. The material was characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersive spectroscopy (EDS), thermogravimetric analysis (TGA), and Brunauer, Emmett, and Teller (BET) surface area measurements and applied for simultaneous magnetic solid-phase extraction (MSPE) of glucocorticoids, estrogens, progestogens, and androgens at ng mL−1 levels from human plasma followed by high-performance liquid chromatography coupled with mass spectrometry (HPLC–MS/MS). Due to the low affinity for proteins, steroids extraction was done with no need for proteins precipitation/centrifugation. As highlighted by a design of experiments, MSPE was performed on 250 µL plasma (after 1:4 dilution) by 50 mg Magn-Humic (reusable for eight extractions) achieving quantitative recovery and satisfying clean-up. This was improved by washing (2 mL 2% v/v formic acid) prior to analytes elution by 0.5 mL 1:1 v/v methanol-acetonitrile followed by 0.5 mL methanol; eluate reduction to 0.25 mL compensated the initial sample dilution. The accuracy was assessed in certified blank fetal bovine serum and in human plasma, gaining satisfactory recovery in the range 65–122%, detection limits in the range 0.02–0.3 ng mL−1 (0.8 ng mL−1 for 17-β-estradiol) and suitable inter-day precision (relative standard deviation (RSD) <14%, n = 3). The method was evaluated in terms of selectivity, sensitivity, matrix-effect, instrumental carry-over, and it was applied to human plasma samples.

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Validation of an ultra-sensitive detection method for steroid esters in plasma for doping analysis using positive chemical ionization GC-MS/MS

Cited by 28 publications

References 30 publications

Testosterone Use and Abuse : Methodological Aspects in Forensic Toxicology and Clinical Diagnostics

Testosterone Use and Abuse : Methodological Aspects in Forensic Toxicology and Clinical Diagnostics

Annual banned‐substance review: Analytical approaches in human sports drug testing 2019/2020

Magnetic Micro-Solid-Phase Extraction Using a Novel Carbon-Based Composite Coupled with HPLC–MS/MS for Steroid Multiclass Determination in Human Plasma

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