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

Waraksa, Emilia; Wójtowicz-Zawadka, Marzena; Kwiatkowska, Dorota; Jarek, Anna; Małkowska, Anna; Wrzesień, R.; Namieśnik, Jacek

doi:10.1016/j.jpba.2018.02.004

Cited by 21 publications

(13 citation statements)

References 27 publications

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“…The compounds 2-OH IBU, 3-OH IBU, and CBX IBU were identified in all the investigated samples, and the concentrations of the unchanged IBU and its metabolites were quantitatively calculated ( Table 4). The IBU human metabolite, 1-OH IBU, was not detected in equine urine samples collected after the drug administration, which was consistent with the previous literature report [24]. Therefore, 1-OH IBU was confirmed to not be an equine metabolite of IBU.…”

Section: Applicability Of the Methodssupporting

confidence: 91%

“…To date, only one report on determination of IBU and its metabolites in equine urine was published . Summary of validation results obtained in this study along with other data published in the literature are shown in Table .…”

Section: Resultsmentioning

confidence: 62%

“…To date, there is a limited data concerning the determination of IBU and its metabolites in equine urine samples. The first attempt to detect and quantify these compounds was published by Waraksa et al [24]. The authors developed protocol based on WCX-SPE together with SCX-SPE followed by LLE as a sample preparation step, which can be successfully used by laboratories with GC-MS equipment.…”

Section: Introductionmentioning

confidence: 99%

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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

Waraksa

Woźniak

Kłodzińska

et al. 2018

J of Separation Science

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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.

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Section: Applicability Of the Methodssupporting

confidence: 91%

Section: Resultsmentioning

confidence: 62%

Section: Introductionmentioning

confidence: 99%

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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

Waraksa

Woźniak

Kłodzińska

et al. 2018

J of Separation Science

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“…95 Dichas muestras deben cumplir con dos de tres criterios para considerarse ilícitas: el riesgo potencial para la salud, ser un agente potencial que mejora el rendimiento y, por último, constituirse en una práctica que promueve la violación del espíritu del deporte. 10 Algunos estudios especifican los métodos de detección de estas sustancias prohibidas, [96][97][98][99][100][101][102][103][104][105][106][107][108] al igual que los perfiles de los atletas que recurren al dopaje. [109][110][111] • La categoría 4.…”

Section: Resultados Y Análisisunclassified

El Dopaje Deportivo Como Cuestión Socialmente Viva: Una Revisión Bibliográfica

Contreras

Torres-Aranguren

2019

Quím. Nova

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This paper aims to present a review of the concept doping in scientific journals published in the period 2008 to 2018. The diversity of approaches that position doping as a socially acute question (SAQ) allow us to recognize the implications of this concept in educational contexts. The state of the art methodology seeks to reflexively recover production on the meaning that is attributed in the literature to the knowledge, practices and social, political and educational implications of a subject as complex as doping. Among the trends found, the Analytical Chemistry approach is highlighted, associated with the studies carried out in the laboratories on techniques and methods for the detection of prohibited substances; the consequences in terms of costs and benefits of doping from biochemical and physiological studies; the set of ideas, conceptions and representations that people have against doping; the educational programs and the pedagogical proposals that study the psychological, epistemological and methodological foundations for the prevention of doping; and the legal aspects, public policies and debates around doping and competition rules.

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“…The chemical structure of IBU is shown in Figure 1. [6]. According to a survey of the literature, no research have been done utilizing the UPLC-MS/MS technique to determine the quantity of IBU in pharmaceutical formulations.…”

Section: Introductionmentioning

confidence: 99%

Determination of Ibuprofen in Pharmaceutical Preparations by UPLC-MS/MS Method

Koçak

Atila

2022

Türk Doğa Ve Fen Dergisi

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Ibuprofen (IBU) is a non-steroidal anti-inflammatory drug that is extensively prescribed. For the determination of IBU in pharmaceutical formulations, a sensitive, simple, accurate, and rapid ultra-performance liquid chromatography method in combination with tandem triple quadruple mass spectrometry (UPLC-MS/MS) has been used and validated. The chromatographic separation was accomplished using a C18 UPLC column, 95 Å, 2.1 x 50 mm, 1.8 µm, and 0.1 percent formic acid in conjunction with acetonitrile (25:75 v/v. The flow rate was 0.15 ml min-1, with a run duration of 2.0 minutes. The injection volume was 5 μL and the column temperature was held constant at 40 °C.The mass transitions of İbuprofen and IS were m/z 205.1 → 159.0 and 249.9 → 229.1, respectivelty. According to ICH guidelines, the approach was thoroughly verified. The linear range 1-5000 ng mL-1 calibration curve has a strong correlation coefficient (0.9921). Within and between days precision were expressed as relative standard deviation and were lower than 6.24%. This method has been used to determine IBU in both pure form and pharmaceutical formulations with great success.

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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

Cited by 21 publications

References 27 publications

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

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

El Dopaje Deportivo Como Cuestión Socialmente Viva: Una Revisión Bibliográfica

Determination of Ibuprofen in Pharmaceutical Preparations by UPLC-MS/MS Method

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