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Analytical biochemistry1985; 151(2); 292-298; doi: 10.1016/0003-2697(85)90178-2

Quantitative methodology for corticosteroids based on chemical oxidation to electrophilic products for electron capture-negative chemical ionization using capillary gas chromatography-mass spectrometry. I. Assessment of feasibility in the analysis of horse urine for dexamethasone.

Abstract: Sensitive and specific methodology based on capillary column gas chromatography-electron capture-negative chemical ionization-mass spectrometry has been developed for the quantitative analysis of corticosteroids from biological fluids. The feasibility of this method is demonstrated in the quantitative analysis of dexamethasone in horse urine following administration of the drug. A structurally similar compound, 6 alpha-methylprednisolone, is added to the urine as an internal standard. The free dexamethasone and the internal standard are extracted and oxidized to high-electron-affinity 1,4-androstadiene-3,11,17-trione structural analogs and then analyzed by capillary column gas chromatography-electron capture-negative chemical ionization-mass spectrometry.
Publication Date: 1985-12-01 PubMed ID: 4096369DOI: 10.1016/0003-2697(85)90178-2Google Scholar: Lookup
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  • Journal Article
  • Research Support
  • Non-U.S. Gov't
  • Research Support
  • U.S. Gov't
  • P.H.S.

Summary

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The research article reports on a newly developed methodology using capillary column gas chromatography-electron capture-negative chemical ionization-mass spectrometry for the quantitative analysis of corticosteroids like dexamethasone in biological fluids like horse urine.

Introduction

  • This study aims to establish an effective way to quantitatively analyse corticosteroids from biological fluids.
  • To assess the viability of this approach, the research looked into the analysis of dexamethasone in horse urine after the drug had been administered.

Methodology

  • A structurally akin compound, 6 alpha-methylprednisolone, was added to the horse urine as an internal standard.
  • The free dexamethasone and the internal standard were extracted from the urine for further analysis.
  • The extracted compounds were then oxidized to result in high-electron-affinity 1,4-androstadiene-3,11,17-trione structural analogs. This essentially makes the compounds more responsive to the electron capture process.

Analysis Approach

  • The oxidized compounds were then analysed using a capillary column gas chromatography-electron capture-negative chemical ionization-mass spectrometry (GC-ECNCI-MS) method.
  • The GC-ECNCI-MS is a method used to completely separate and identify different compounds in a sample.
  • In electron capture-negative chemical ionization, an electron is captured by the molecule, and the excess energy leads to fragmentation, which can be tracked by mass spectrometry.

Implication of the research

  • This research potentially opens up a new, more sensitive and specific method for the quantitative analysis of corticosteroids in biological fluids.
  • Rigorously examining for the presence of corticosteroids like dexamethasone in horse urine, for instance, can prevent potential misuse in equine sports.

Cite This Article

APA
Her GR, Watson JT. (1985). Quantitative methodology for corticosteroids based on chemical oxidation to electrophilic products for electron capture-negative chemical ionization using capillary gas chromatography-mass spectrometry. I. Assessment of feasibility in the analysis of horse urine for dexamethasone. Anal Biochem, 151(2), 292-298. https://doi.org/10.1016/0003-2697(85)90178-2

Publication

ISSN: 0003-2697
NlmUniqueID: 0370535
Country: United States
Language: English
Volume: 151
Issue: 2
Pages: 292-298

Researcher Affiliations

Her, G R
    Watson, J T

      MeSH Terms

      • Adrenal Cortex Hormones / analysis
      • Animals
      • Dexamethasone / urine
      • Feasibility Studies
      • Gas Chromatography-Mass Spectrometry / methods
      • Horses
      • Kinetics

      Grant Funding

      • GMS-28910 / NIGMS NIH HHS
      • RR-00480-16 / NCRR NIH HHS

      Citations

      This article has been cited 1 times.
      1. Cantrell MS, McDougal OM. Biomedical rationale for acrylamide regulation and methods of detection.. Compr Rev Food Sci Food Saf 2021 Mar;20(2):2176-2205.
        doi: 10.1111/1541-4337.12696pubmed: 33484492google scholar: lookup