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Simultaneous determination of ibuprofen and its metabolites in complex equine urine matrices by GC-EI-MS in excretion study in view of doping control

Artykuł
Czasopismo : Journal of Pharmaceutical and Biomedical Analysis   Tom: 152, Strony: 279-288
Emilia Waraksa [1] , [2] , Marzena Wójtowicz-Zawadka [3] , Dorota Kwiatkowska [3] , Anna Jarek [3] , Anna Małkowska [4] , Robert Wrzesień [5] , Jacek Namieśnik [1]
2018-02-05 angielski
Liczba arkuszy: 1
Identyfikatory
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Cechy publikacji
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  • Oryginalny artykuł naukowy
  • Zrecenzowana naukowo
Dyscypliny naukowe
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Chemia
Słowa kluczowe
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Abstrakty ( angielski )
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A novel assay for the simultaneous determination of ibuprofen (IBU) and its four probable metabo-lites, 1-hydroxyibuprofen (1-OH IBU), 2-hydroxyibuprofen (2-OH IBU), 3-hydroxyibuprofen (3-OH IBU)and carboxyibuprofen (CBX IBU) in equine urine samples with the application of Gas Chromatography-Electron Ionization-Mass Spectrometry (GC-EI-MS) has been developed and elaborated. The newapproach for sample preparation including minimizing matrix effects by the application of weak cationexchange solid-phase extraction together with strong cation exchange solid-phase extraction has beenapplied. The GC-EI-MS method was validated to demonstrate specificity, matrix effect, linearity, limitof detection (LOD) and quantification (LOQ), precision, trueness, carry-over and stability by using thematrix-matched quality control samples. Additionally, extraction yield was evaluated. The assay achievedthe LOQ of 1.75 ?g mL−1, 0.62 ?g mL−1, 4.15 ?g mL−1, 0.58 ?g mL−1and 4.04 ?g mL−1for IBU, 1-OH IBU,2-OH IBU, 3-OH IBU and CBX IBU, respectively. The developed method has been successfully applied tothe excretion study in horses, in which a single oral IBU dose was administered to twelve horses (maresand geldings) and equine urine samples were collected for 5 or 6 days after the drug administration. Dataon the detection and determination of three IBU metabolites, 2-OH IBU, 3-OH IBU and CBX IBU in equineurine samples has been presented for the first time. The obtained results indicated the rapid excretionof IBU and its metabolites that were detectable only in the first day after the drug administration. IBUwas mainly the most abundant compound detected in equine urine samples (with two exceptions in thecase of samples collected from two horses, for which the highest instrumental responses were obtainedfor CBX IBU). The received results have indicated that two major IBU metabolites, CBX IBU and 2-OH IBUcan be important markers for the IBU abuse in view of doping control in equestrian sports.
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