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Development and validation of a liquid chromatographic-electrospray tandem mass spectrometric multiresidue method for
Hendrik De Ruyck1, Els Daeseleire, Herman De Ridder
1Ministry of the Flemish Community, Agricultural Research Centre Ghent (CLO), Department of Animal Product Quality and Transformation Technology (DVK), Brusselsesteenweg 370, B-9090 Melle, Belgium. h.deruyck@clo.fgov.be
Abstract:
A liquid chromatographic-tandem mass spectrometric multiresidue method for the simultaneous quantitative determination of the tetrahydroimidazole, levamisole and the benzimidazoles thiabendazole, oxfendazole, oxibendazole, albendazole, fenbendazole, febantel and triclabendazole in milk has been developed and validated. The anthelmintic residues were extracted with ethyl acetate. The liquid chromatographic separation was performed on a reversed-phase C18 column with gradient elution. The analytes were detected by tandem quadrupole mass spectrometry after positive electrospray ionisation by multiple reaction monitoring. The confirmatory method is very sensitive and each component can be detected at a residue level lower than 1 microgram/l. The method is validated according to the revised European Union requirements and all parameters were found conform the criteria. The evaluated parameters were linearity, specificity, stability, recovery, precision (repeatability and within-laboratory reproducibility) and analytical limits (detection limit, decision limit and detection capability). This analytical method is applied in the Belgian monitoring programme for classical anthelmintic veterinary drugs in raw farm cow's milk.