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Journal of chromatography1992; 577(2); 221-227;

Thermospray liquid chromatography-mass spectrometry of corticosteroids.

Abstract: A high-performance liquid chromatographic method was developed for thermospray mass spectrometric analysis of steroidal hormones. Using a Nova-Pak C18 reversed-phase column and isocratic elution with a solvent comprised of 25 mM ammonium formate in 30% acetonitrile, corticosteroids were separated within 10 min. This solvent also permitted ultraviolet absorbance detection down to 220 nm with low-nanogram sensitivity. The use of acetonitrile was favourable for thermospray mass spectrometric analysis because mass spectra were obtained with a pseudomolecular ion as the base peak. A combination of liquid chromatography, ultraviolet absorbance detection and thermospray mass spectrometry provided a sensitive and reliable method for unequivocal confirmation of the presence of steroidal drugs in equine urine.
Publication Date: 1992-06-10 PubMed ID: 1400755
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  • Journal Article
  • Research Support
  • Non-U.S. Gov't

Summary

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The research article describes the development of an efficient method to analyze steroidal hormones using high-performance liquid chromatography coupled with thermospray mass spectrometry. The method allows the separation of corticosteroids within 10 minutes and confirms their presence in equine urine.

Development of the Method

  • Researchers developed a high-performance liquid chromatographic method for the thermospray mass spectrometric analysis of steroidal hormones.
  • The method utilized a Nova-Pak C18 reversed-phase column for the analysis. The reversed-phase column methodology means the column is hydrophobic, which helps in separating components based on polarity.
  • Isocratic elution was used with a specific solvent. This is a method where the composition of the solvent remains the same throughout the whole process.

Solvent Composition

  • The solvent consisted of 25 mM ammonium formate in 30% acetonitrile.
  • This solvent facilitated optimal ultraviolet absorbance detection down to 220 nm with low-nanogram sensitivity, which means the method is highly sensitive and efficient.
  • Acetonitrile proved to be beneficial for the thermospray mass spectrometric analysis as it enabled the generation of mass spectra with pseudomolecular ion as the base peak.

Analysis of Steroidal Drugs in Equine Urine

  • The application of the method to actual case scenarios was demonstrated by the confirmation of the presence of steroidal drugs in equine urine.
  • This fact indicates that the developed methodology is effectively applicable outside a controlled laboratory environment, thus demonstrating practical applicability.

Conclusion

  • In conclusion, the combination of liquid chromatography, ultraviolet absorbance detection, and thermospray mass spectrometry offers a sensitive and reliable method to confirm the existence of steroidal drugs.
  • The method developed in this study allows a separation time of just 10 minutes, making it an efficient choice for large-scale or time-sensitive applications.

Cite This Article

APA
Steffenrud S, Maylin G. (1992). Thermospray liquid chromatography-mass spectrometry of corticosteroids. J Chromatogr, 577(2), 221-227.

Publication

NlmUniqueID: 0427043
Country: Netherlands
Language: English
Volume: 577
Issue: 2
Pages: 221-227

Researcher Affiliations

Steffenrud, S
  • Analytical Toxicology and Drug Testing, Cornell University, Ithaca, NY 14850.
Maylin, G

    MeSH Terms

    • Adrenal Cortex Hormones / urine
    • Animals
    • Doping in Sports
    • Horses
    • Mass Spectrometry / methods
    • Spectrophotometry, Ultraviolet

    Citations

    This article has been cited 1 times.
    1. Reddy IM, Beotra A, Jain S, Ahi S. A simple and rapid ESI-LC-MS/MS method for simultaneous screening of doping agents in urine samples. Indian J Pharmacol 2009 Apr;41(2):80-6.
      doi: 10.4103/0253-7613.51347pubmed: 20336223google scholar: lookup