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Cited by 60Analytical Chemistry and ChromatographyDoping in SportsAnalytical Methods in Pharmaceuticals

Analysis of glucuronide and sulfate steroids in urine by ultra-high-performance supercritical-fluid chromatography hyphenated tandem mass spectrometry

Doué, Mickael, Dervilly-Pinel, Gaud, Pouponneau, Karinne, Monteau, Fabrice, Le Bizec, Bruno·2015·Analytical and Bioanalytical Chemistry
DOI 10.1007/s00216-015-8573-x
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Abstract

Profiling conjugated urinary steroids to detect anabolic-steroid misuse is recognized as an efficient analytical strategy in both chemical-food-safety and anti-doping fields. The relevance and robustness of such profiling rely on the analysis of glucuronide and sulfate steroids, which is expected to have properties including accuracy, specificity, sensitivity, and, if possible, rapidity. In this context, the ability of ultra-high-performance supercritical-fluid chromatography (UHPSFC) hyphenated tandem mass spectrometry (MS-MS) to provide reliable and accurate phase II analysis of steroids was assessed. Four stationary phases with sub-2 μm particles (BEH, BEH 2-ethyl-pyridine, HSS C18 SB, and CSH fluorophenyl) were screened for their capacity to separate several conjugated steroid isomers. Analytical conditions including stationary phase, modifier composition and percentage, back pressure, column temperature, and composition and flow rate of make-up solvent were investigated to improve the separation and/or the sensitivity. Thus, an analytical procedure enabling the analysis of eight glucuronide and 12 sulfate steroids by two different methods in 12 and 15 min, respectively, was optimized. The two procedures were evaluated, and UHPSFC-MS-MS analysis revealed its ability to provide sensitive (limits of quantification: 0.1 ng mL(-1) and 0.5 ng mL(-1) for sulfate and glucuronide steroids, respectively) and reliable quantitative performance (R(2) > 0.995, RSD < 20%, and bias < 30%) through the use of suitable labeled internal standards. Comparison with UHPLC-MS-MS was performed, and UHPSFC-MS-MS obtained better performance in terms of sensitivity. Finally, as a proof of concept, this so-called green technology was used in a chemical-food-safety context to profile steroid conjugates in urine samples from bovines treated with estradiol. Graphical Abstract Glucuronide and sulfate steroids analysis in urine by ultra-high performance supercritical fluid chromatography hyphenated tandem mass spectrometry.

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Crossref · 10.1007/s00216-015-8573-x

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  • To date only a limited number of methods for the simultaneous measurement of free, sulfated and glucuronidated androgens have been established, although significant progress has been made.

    “but to date only a limited number of methods for the simultaneous measurement of free, sulfated and glucuronidated androgens have been established, although significant progress has been made (Badoud et al., 2011, Doue et al., 2015, Galuska et al., 2013).”

    From Intracrine androgen biosynthesis, metabolism and action revisited (2018) · cites this paper as Doue et al., 2015

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Authors
Doué, M., Dervilly-Pinel, G., Pouponneau, K., Monteau, F., & Le Bizec, B.
Affiliations
Laboratoire D'étude des Résidus et Contaminants Dans les Aliments (FR)
ORCID
Doué, Mickael
Venue
Analytical and Bioanalytical Chemistry
Publisher
Springer Science and Business Media LLC
Published
2015-03-04
Volume
407
Issue
15
Pages
4473-4484
ISSN
  • 1618-2642 (ISSN-L)
  • 1618-2650
DOI
10.1007/s00216-015-8573-x
OpenAlex
W2070779738
Cited by
60
References
29
Citations by year
2025: 4 · 2024: 4 · 2023: 5 · 2022: 6 · 2021: 7 · 2020: 7 · 2019: 2 · 2018: 12 · 2017: 6 · 2016: 7
FWCI
3.71
Type
journal article
Language
en
Open access
closed
Licence
www.springer.com/tdm (tdm)
Locations
  • Analytical and Bioanalytical Chemistry (publishedVersion)
  • PubMed (publishedVersion)
Topics
  • Physical Sciences › Chemistry › Spectroscopy › Analytical Chemistry and Chromatography
  • Social Sciences › Sociology and Political Science › Doping in Sports
  • Physical Sciences › Chemistry › Analytical Chemistry › Analytical Methods in Pharmaceuticals
Keywords
ultra-high performance supercritical fluid chromatography, tandem mass spectrometry, food safety, anti-doping
MeSH terms
Animals, Cattle, Chromatography, High Pressure Liquid, Estradiol, Steroids, Sulfates, Glucuronides, Anabolic Agents, Tandem Mass Spectrometry, Limit of Detection

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