The Analyst · 2001 · 28 citations · 5 references
PharmacyToxicologyVeterinary ToxicologyAnalytical ChemistryAnalytical ToxicologyMass Spectrometric AnalysisAnalytical ChromatographyAnalytical Method ValidationAssay ValidationBioanalytical Method ValidationToxicological Screening Of PharmaceuticalsVeterinary Drug ResiduesAnalytical Detection LimitsAnalytical Methods DevelopmentDrug Residue DetectionEgg ResiduesInternal Standard AnalysisLimitsMarker Residue AnalysisVeterinary Drug Residue Limits
A method is described for the quantitative confirmation of 4,4'-dinitrocarbanilide (DNC), the marker residue for nicarbazin in chicken liver and eggs. The method is based on LC coupled to negative ion electrospray MS-MS of tissue extracts prepared by liquid-liquid extraction. The [M-H]- ion at m/z 301 is monitored along with two transition ions at m/z 137 and 107 for DNC and the [M-H]- ion at m/z 309 for the internal standard, d8-DNC. The method has been validated according to the new EU criteria for the analysis of veterinary drug residues at 100, 200 and 300 microg kg(-1) in liver and at 10, 30 and 100 microg kg(-1) in eggs. Difficulties concerning the application of the new analytical limits, namely the decision limit (CCalpha) and the detection capability (CCbeta) to the determination of DNC in both liver and eggs are discussed.
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