Determination of residues of azaperone in the kidneys by liquid chromatography with fluorescence detection

An analytical method has been developed for the quantitative determination of residues of the tranquillizer azaperone (AZN) in the kidneys of slaughtered animals. Samples were extracted with acetonitrile, extracts were acidified and further purified with solid-phase extraction (SPE) on a polymeric m...

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Bibliographic Details
Published in:Analytica chimica acta 2007-03, Vol.586 (1-2), p.374-382
Main Author: Cerkvenik-Flajs, Vesna
Format: Article
Language:English
Subjects:
Acetonitriles - pharmacology
Analysis
Analytical chemistry
Animals
Azaperol
Azaperone
Azaperone - analysis
Cattle
Chemistry
Chromatographic methods and physical methods associated with chromatography
Chromatography, High Pressure Liquid - methods
Chromatography, Liquid - methods
Drug Residues - analysis
Exact sciences and technology
Food Analysis - methods
Horses
Kidney - drug effects
Kidney - metabolism
Kidneys
Liquid chromatography-fluorescence
Other chromatographic methods
Poultry
Residues
Sensitivity and Specificity
Spectrometric and optical methods
Spectrometry, Fluorescence - methods
Swine
Tranquilizing Agents - analysis
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Summary:An analytical method has been developed for the quantitative determination of residues of the tranquillizer azaperone (AZN) in the kidneys of slaughtered animals. Samples were extracted with acetonitrile, extracts were acidified and further purified with solid-phase extraction (SPE) on a polymeric mixed-mode cation-exchange sorbent, Oasis®. AZN and its main metabolite azaperol (AZL) were eluted by alkaline methanol (MeOH), the eluate was evaporated, re-dissolved and analysed by gradient high performance liquid chromatography (LC) on reversed and deactivated phase LiChrospher 60-RP select B at excitation and emission wavelengths of 245 and 345nm, respectively. The method was validated according to the requirements of European Commission Decision 2002/657/EC, using fortified porcine kidneys. The method proved to be selective, specific against carazolol (CAR) and linear over a concentration range 10–150μgkg−1 (r2>0.99). Over a concentration range 50–150μgkg−1, mean recovery of AZN and AZL was 88.2 and 91.2%, respectively, with intra-laboratory reproducibility of
ISSN:0003-2670
1873-4324
DOI:10.1016/j.aca.2006.11.010