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Direct injection horse urine analysis for the quantification and identification of threshold substances for doping control. III. Determination of salicylic acid by liquid chromatography/quadrupole time-of-flight mass spectrometry.

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  • Author(s): Vonaparti A;Vonaparti A; Lyris E; Panderi I; Koupparis M; Georgakopoulos C
  • Source:
    Analytical and bioanalytical chemistry [Anal Bioanal Chem] 2009 Nov; Vol. 395 (5), pp. 1403-10. Date of Electronic Publication: 2009 Sep 08.
  • Publication Type:
    Journal Article; Research Support, Non-U.S. Gov't; Validation Study
  • Language:
    English
  • Additional Information
    • Source:
      Publisher: Springer-Verlag Country of Publication: Germany NLM ID: 101134327 Publication Model: Print-Electronic Cited Medium: Internet ISSN: 1618-2650 (Electronic) Linking ISSN: 16182642 NLM ISO Abbreviation: Anal Bioanal Chem Subsets: MEDLINE
    • Publication Information:
      Original Publication: Heidelberg : Springer-Verlag, 2002-
    • Subject Terms:
      Chromatography, Liquid/*methods ; Doping in Sports/*methods ; Horses/*urine ; Mass Spectrometry/*methods ; Salicylic Acid/*urine; Animals ; Calibration ; Molecular Structure ; Salicylic Acid/chemistry ; Time Factors
    • Abstract:
      In equine sport, salicylic acid is prohibited with a threshold level of 750 microg mL(-1) in urine; hence, doping control laboratories have to establish quantitative and qualitative methods for its determination. A simple and rapid liquid chromatographic/mass spectrometric method was developed and validated for the quantification and identification of salicylic acid. Urine samples after 900-fold dilution and addition of the internal standard (4-methylsalicylic acid) were directly injected to the liquid chromatography/quadrupole time-of-flight mass spectrometry system. Electrospray ionization in negative mode with full scan acquisition mode and product ion scan mode were chosen for the quantification and identification of salicylic acid, respectively. Run time was 2.0 min. The tested linear range was 2.5-50 microg mL(-1) (after 100-fold sample dilution). The relative standard deviations of intra- and inter-assay analysis of salicylic acid in horse urine were lower than 2.5% and 2.8%, respectively. Overall accuracy (relative percentage error) was less than 3.3%. Method was applied to two real samples found to be positive for salicylic acid, demonstrating simplicity, accuracy, and selectivity.
    • Accession Number:
      O414PZ4LPZ (Salicylic Acid)
    • Publication Date:
      Date Created: 20090917 Date Completed: 20100430 Latest Revision: 20191210
    • Publication Date:
      20240513
    • Accession Number:
      10.1007/s00216-009-3047-7
    • Accession Number:
      19756547