A rapid and sensitive method for the quantitative analysis of ibuprofen and its metabolites in equine urine samples by gas chromatography with tandem mass spectrometry.
Abstract: Ibuprofen is widely used in human and veterinary medicine for the treatment of chronic pain as well as rheumatic and musculoskeletal disorders. However, the analgesic and anti-inflammatory properties of Ibuprofen have contributed to frequent drug abuse in equestrian sports. A sensitive and rapid gas chromatography with tandem mass spectrometry based method with a simple liquid-liquid extraction and derivatization requiring 200 μL volume of sample and 2 mL of extraction solvent for the simultaneous determination of ibuprofen and its metabolites was developed. The proposed procedure was optimized and validated according to the principles for bioanalytical methods. The assay achieved satisfactory validation parameters, namely, recovery (92.2-105%), interday accuracy (92.5-106%), and precision (0.3-4.4%) for all investigated compounds as well as limits of quantification of 50 ng/mL for ibuprofen, 2-hydroxyibuprofen, and carboxyibuprofen, 25 ng/mL for 1-hydroxyibuprofen and 100 ng/mL for 3-hydroxyibuprofen. The applicability of the method was evaluated by the analysis of five real urine samples collected from different horses after drug administration. In view of the low limits of quantification, high selectivity, repeatability, and recovery, the procedure can be utilized for laboratory applications, including the control of ibuprofen abuse in equestrian sports for anti-doping purposes and drug/pharmaceutical mentality investigations.
© 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.
Publication Date: 2018-08-28 PubMed ID: 30101517DOI: 10.1002/jssc.201800614Google Scholar: Lookup
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- Journal Article
Summary
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This research involves the development and validation of a sensitive, quick method for quantifying ibuprofen and its metabolites in horse urine, with the aim to regulate misuse of the drug in equestrian sports.
Objective and significance
- The main objective of the research was to create an efficient method for analyzing ibuprofen and its metabolites in equine urine.
- The intention of creating such a method is to maintain fair play in equestrian sports, as ibuprofen is widely misused due to its analgesic and anti-inflammatory properties.
- Ibuprofen is commonly used in medicine to manage chronic pain and rheumatic issues, in both, humans and horses.
Methodology
- Using gas chromatography with tandem mass spectrometry, a technique was developed to identify and measure ibuprofen and its metabolites in the urine samples.
- The procedure involves a simple liquid-liquid extraction and derivatization, requiring a minimal volume of the sample and extraction solvent.
- The method was also optimized and validated, keeping in line with principles governing bioanalytical methods.
Results and Validation
- The assay achieved satisfactory validation parameters like recovery (92.2-105%), interday accuracy (92.5-106%), and precision (0.3-4.4%) for all the compounds under investigation.
- Furthermore, limits of quantification were set for ibuprofen, 2-hydroxyibuprofen, carboxyibuprofen, 1-hydroxyibuprofen, and 3-hydroxyibuprofen.
- The developed method’s effectiveness was tested by analyzing urine samples from different horses who had been administered the drug.
Conclusion
- Given its low limits of quantification, high selectivity, repeatability, and recovery, this method is suitable for laboratory applications.
- Moreover, it can be instrumental in controlling ibuprofen misuse in equestrian sports and aiding drug/pharmaceutical investigations.
Cite This Article
APA
Waraksa E, Woźniak MK, Kłodzińska E, Wrzesień R, Bobrowska-Korczak B, Namieśnik J.
(2018).
A rapid and sensitive method for the quantitative analysis of ibuprofen and its metabolites in equine urine samples by gas chromatography with tandem mass spectrometry.
J Sep Sci, 41(20), 3881-3891.
https://doi.org/10.1002/jssc.201800614 Publication
Researcher Affiliations
- Faculty of Chemistry, Department of Analytical Chemistry, Gdańsk University of Technology, Gdańsk, Poland.
- Department of Analytical Chemistry and Instrumental Analysis, Institute of Sport - National Research Institute, Warsaw, Poland.
- Faculty of Chemistry, Department of Analytical Chemistry, Gdańsk University of Technology, Gdańsk, Poland.
- Department of Analytical Chemistry and Instrumental Analysis, Institute of Sport - National Research Institute, Warsaw, Poland.
- Central Laboratory of Experimental Animal, Medical University of Warsaw, Warsaw, Poland.
- Department of Bromatology, Medical University of Warsaw, Warsaw, Poland.
- Faculty of Chemistry, Department of Analytical Chemistry, Gdańsk University of Technology, Gdańsk, Poland.
MeSH Terms
- Animals
- Chromatography, Gas
- Horses
- Ibuprofen / metabolism
- Ibuprofen / urine
- Liquid-Liquid Extraction
- Molecular Structure
- Tandem Mass Spectrometry
Grant Funding
- 2016/21/N/ST4/02342 / Polish National Science Center
Citations
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