Determination of nifursol metabolites in poultry muscle and liver tissue. Development and validation of a confirmatory method
article
A method is described for the identification and quantitative determination of 3,5-dinitrosalicylic acid hydrazide (DSH), the marker residue of nifursol metabolites in poultry (turkey, broiler) muscle and liver tissue. The method is based on the acid-catalysed hydrolysis of tissue-bound metabolites to free DSH and in situ derivatisation with 2-nitrobenzaldehyde to the corresponding nitrophenyl derivative NPDSH. A structural analogue of DSH, 4-hydroxy-3,5- dinitrobenzoic acid hydrazide (HBH) was synthesised to serve as an internal standard. The analytes were isolated from the matrix by liquid-liquid extraction with ethyl acetate. Determination was performed by LC-MS/MS with negative electrospray ionisation. The [M - H]+ ions of NPDSH and NPHBH at m/z 374 were fragmented by collision induced dissociation (CID) producing transition ions at m/z 182, 183 and 226. The transition ions at m/z 182 and 226 were selected for monitoring of NPDSH while the transition ion at m/z 183 was selected for NPHBH. The method has been validated according to the EU criteria of Commission Decision 2002/657/EC at 0.5, 1.0 and 1.5 μg kg-1 in muscle and liver tissue. A decision limit (CCα) was obtained of 0.04 and 0.025 μg kg-1 in muscle and liver, respectively. Similarly a detection capability (CCβ) was obtained of 0.10 and 0.05 μg kg-1 in muscle and liver, respectively. The introduction of HBH as an internal standard did not lead to a significant improvement of the quantitative performance of the method. In fact for liver better performance characteristics were obtained when the IS was not taken into account. Nevertheless, as a qualitative marker for recovery, HBH could still be very useful in the analysis of unknown samples. © The Royal Society of Chemistry 2005.
Topics
Food and Chemical Risk Analysis3,5 dinitro n' (5 nitrofurfurylidene)salicylhydrazide4 hydroxy 3,5 dinitrobenzoic acid hydrazideAcetic acid ethyl esterBenzaldehyde derivativeHydrazide derivativeNifursolNitrobenzoic acid derivativeUnclassified drugCatalysisChemical analysisChemical structureDerivatizationElectrosprayHydrolysisLiquid liquid extractionLiverMetaboliteMuscleNonhumanPoultryQuantitative analysisStandardSynthesisTurkey (bird)Validation processAnimalsAntiprotozoal AgentsChromatography, LiquidDrug ResiduesFood AnalysisFood ContaminationLiverMass SpectrometryMusclesNitrofuransPoultry
TNO Identifier
238492
ISSN
0003-2654
Source
Analyst, 130(5), pp. 763-771.
Pages
763-771
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