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Analytical chemistry1996; 68(1); 118-123; doi: 10.1021/ac950566j

A partially automated pretreatment module for routine analyses for seventeen non-steroid antiinflammatory drugs in race horses using gas chromatography/mass spectrometry.

Abstract: A partially automated module for the routine determination of illicit non-steroid antiinflammatory drugs (NSAIDs) in biological fluids from race horses was built, tested, refined, and shown to work. This pretreatment module retains 17 NSAIDs on an Amberlite XAD-2 column before back-elution derivatization with methyl iodide in acetonitrile. Methylated derivatives are manually injected into a gas chromatograph connected to a mass spectrometer. The quantification limits thus achieved are 50-100 ng/mL in 1 mL of urine or plasma. The proposed method is more expeditious than its manual liquid-liquid and liquid-solid extraction counterparts and is similar in speed to a typical gas chromatographic program.
Publication Date: 1996-01-01 PubMed ID: 8779428DOI: 10.1021/ac950566jGoogle Scholar: Lookup
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  • Journal Article
  • Research Support
  • Non-U.S. Gov't

Summary

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The research article presents the development and testing of a partially automated system used to analyze non-steroid anti-inflammatory drugs (NSAIDs) in race horses’ biological fluids using a gas chromatography/mass spectrometry method.

Development and Testing of the Pretreatment Module

  • The scientists developed a system to automatically detect illegal use of NSAIDs in race horses. NSAIDs can be used to mask pain and thus can be used to cheat in horse racing.
  • The developed method entails the use of a pretreatment module that automatically isolates and purifies samples using an Amberlite XAD-2 column. This involves retaining the 17 NSAIDs on the column before applying back-elution derivatization with methyl iodide in acetonitrile.
  • This method was rigorously tested and refined, demonstrating its effectiveness and reliability in isolating and identifying NSAIDs from biological samples.

Application and Injection into Gas Chromatograph/Mass Spectrometer

  • Following the automatic pretreatment process, the methylated derivatives of the purified samples are manually injected into a gas chromatograph that is connected to a mass spectrometer.
  • The gas chromatograph and mass spectrometer work together to identify and quantify the presence of specific NSAIDs in the samples.
  • The proposed method is capable of detecting and measuring NSAIDs at concentrations of 50-100 ng/mL in 1 mL samples of urine or plasma.

Comparison with Other Techniques

  • The study further compares the proposed method with existing methods and confirms its superiority in terms of speed and efficiency.
  • Compared to common liquid-liquid or liquid-solid extraction methods that are manually performed, the proposed automated pretreatment module proves to be faster and more expeditious.
  • In terms of speed, it is comparable to a typical gas chromatographic program, making it a viable alternative for practical implementation in the detection of illicit use of NSAIDs in horse racing.

Cite This Article

APA
Cárdenas S, Gallego M, Valcárcel M, Ventura R, Segura J. (1996). A partially automated pretreatment module for routine analyses for seventeen non-steroid antiinflammatory drugs in race horses using gas chromatography/mass spectrometry. Anal Chem, 68(1), 118-123. https://doi.org/10.1021/ac950566j

Publication

ISSN: 0003-2700
NlmUniqueID: 0370536
Country: United States
Language: English
Volume: 68
Issue: 1
Pages: 118-123

Researcher Affiliations

Cárdenas, S
  • Department of Analytical Chemistry, Faculty of Sciences, University of Córdoba, Spain.
Gallego, M
    Valcárcel, M
      Ventura, R
        Segura, J

          MeSH Terms

          • Animals
          • Anti-Inflammatory Agents, Non-Steroidal / analysis
          • Anti-Inflammatory Agents, Non-Steroidal / blood
          • Anti-Inflammatory Agents, Non-Steroidal / urine
          • Autoanalysis
          • Doping in Sports
          • Gas Chromatography-Mass Spectrometry
          • Horses / metabolism

          Citations

          This article has been cited 1 times.
          1. Pulgarín JA, Molina AA, Ferreras FM. Simultaneous determination of mefenamic and tolfenamic acids in real samples by terbium-sensitized luminescence. J Fluoresc 2012 Nov;22(6):1483-92.
            doi: 10.1007/s10895-012-1085-6pubmed: 22752433google scholar: lookup