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J Chromatogr Sci ; 53(6): 925-31, 2015 Jul.
Article de Anglais | MEDLINE | ID: mdl-25480455

RÉSUMÉ

A comprehensive ultra-high performance liquid chromatography/tandem mass spectrometry (UHPLC/MS/MS) procedure for detection of nine ß-agonists in animal-derived food is described. The method was based on enzymatic hydrolysis with ß-glucuronidase from Helix pomatia, followed by a liquid-liquid extraction procedure with perchloric acid and a solid-phase extraction scheme using two kinds of cartridges, HLB and MCX. The influence of sample solution pH in the extraction recovery was studied, and pH 4.0 was found to give the best recovery. The analytes were eluted with methanol containing 4% ammonia. A validation procedure for quantitative analysis of ß-agonists in animal-derived food was performed. The three kinds of internal standards, d3-salbutamol, d6-ractopamine and d9-clenpenterol, were applied in the sample preparation and detection of UHPLC/MS/MS. The recoveries from spiked samples ranged between 74.9 and 106.9%. The relative standard deviations of detection were at 0.7-9.6%. The limits of detection and quantification were 0.01-0.05 and 0.03-0.20 µg/kg, respectively. The effect of sample matrix in the detection was discussed in detail.


Sujet(s)
Agonistes bêta-adrénergiques/analyse , Chromatographie en phase liquide à haute performance/méthodes , Résidus de médicaments/analyse , Éthanolamines/analyse , Viande/analyse , Animaux , Chromatographie en phase liquide/méthodes , Rein/composition chimique , Limite de détection , Modèles linéaires , Foie/composition chimique , Reproductibilité des résultats , Suidae , Spectrométrie de masse en tandem/méthodes , Médicaments vétérinaires/analyse
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