Reference : Pre-study and in-study validation of an ultra-high pressure LC method coupled to tandem ...
Scientific journals : Article
Life sciences : Veterinary medicine & animal health
Human health sciences : Pharmacy, pharmacology & toxicology
http://hdl.handle.net/2268/8566
Pre-study and in-study validation of an ultra-high pressure LC method coupled to tandem mass spectrometry for off-line determination of oxytetracycline in nasal secretions of healthy pigs.
English
Bimazubute, Marcel Aimé [Université de Liège - ULg > > > >]
Rozet, Eric mailto [Université de Liège - ULg > Département de pharmacie > Chimie analytique >]
Dizier, Isabelle [> > > >]
Van Heugen, Jean-Claude mailto [Centre Hospitalier Universitaire de Liège - CHU > > Chimie médicale >]
Arancio, Enza [> > > >]
Gustin, Pascal mailto [Université de Liège - ULg > Département de sciences fonctionnelles > Pharmacologie, pharmacothérapie et toxicologie >]
Crommen, Jessica [Centre Hospitalier Universitaire de Liège - CHU > > Ophtalmologie >]
Chiap, Patrice [Centre Hospitalier Universitaire de Liège - CHU > > Pharmacologie clinique >]
2009
Journal of Chromatography. B : Analytical Technologies in the Biomedical & Life Sciences
Elsevier Science
877
23
2349-57
Yes (verified by ORBi)
International
1570-0232
1873-376X
Amsterdam
Netherlands
[en] Oxytetracycline ; Nasal secretions ; Healthy pigs ; UPLC–MS/MS ; Validation
[en] In order to quantify oxytetracycline (OTC) in nasal secretions of healthy pigs after intramuscular injection of OTC at doses of 10, 20 and 40 mg/kg bodyweight, an original method based on ultra-high pressure liquid chromatography coupled to tandem mass spectrometry (UPLC-MS/MS) was developed and fully validated. Sample preparation consisted in protein precipitation preceded by the addition of a releasing protein reagent. Metacycline (MTC) was used as internal standard. Separation was carried out at 65 degrees C in the gradient elution mode on a short analytical column filled with Acquity BEH C(18) stationary phase. The mobile phase consisted in a mixture of water and acetonitrile containing 1 mM of oxalic acid and 0.1% (v/v) of formic acid. The triple quadrupole mass spectrometer operated in the positive electrospray ionization mode; OTC and MTC were detected using multiple reaction monitoring. The pre-study and in-study validation of this bioanalytical method was performed by applying a novel strategy based on total measurement error and accuracy profiles. The maximum risk of observing future measurements falling outside the acceptance limits during routine as well as the measurements uncertainty were also estimated.
Researchers ; Professionals ; Students
http://hdl.handle.net/2268/8566
also: http://hdl.handle.net/2268/18775
10.1016/j.jchromb.2009.01.033

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